United States Department of Agriculture Natural Resources Conservation Service

Soil Survey Laboratory Methods Manual
Soil Survey Investigations Report No. 42 Version 4.0 November 2004

SOIL SURVEY LABORATORY METHODS MANUAL
Rebecca Burt, Editor

Soil Survey Investigations Report No. 42 Version 4.0 November 2004

Cover Photo:The cover illustrates the continuum of data collected or produced for the soil survey of a geographic area. The soil survey map, landscape, and pedon are from northern Iredell County, North Carolina and are representative of the Banister pedon. This series is classified as a fine, mixed, active, mesic Aquic Hapludalf. This soil is a very deep, moderately to somewhat poorly drained soil on stream terrace positions in the Piedmont physiographic province of Virginia and North Carolina. Laboratory data sheet illustrates particle-size data produced by the Soil Survey Laboratory. The photomicrograph of soil fabric features a slightly altered, exfoliated biotite grain under cross-polarized light. Bar scale in photo is 0.25 mm. (Photo credit of Banister landscape and pedon: John Kelly and Michael A. Wilson, NRCS, Raleigh, NC and NRCS, Lincoln, NE.)

FOREWORD Laboratory data are critical to the understanding of the properties and genesis of a single pedon, as well as to the understanding of fundamental soil relationships based on many observations of a large number of soils. Development of both an analytical database and the soil relationships based on those data are the cumulative effort of generations of soil scientists at the Soil Survey Laboratory (SSL). The purpose of the Soil Survey Investigations Report (SSIR) No., Soil Survey Laboratory Methods Manual is to document methodology and to serve as a reference for the laboratory analyst. It is expected that this document will continue to evolve and change over time as new methods are developed and old methods are modified or retired based on new knowledge or technologies. This manual is an historical document in that it describes both current and obsolete methods at the SSL. This manual also provides historical perspective, documenting the contributions of many soil scientists who have gone before us. Many of these scientists are noted in the section on contributors. Dr. Rebecca Burt, author of the Soil Survey Information Manual (SSIR No. 45, 1995), served as technical editor for all versions of the SSIR No. 42 (1989, 1992, 1996, 2004). Her contribution is significant in scope; she wrote some of the methods; is responsible for the review process encompassing additions, corrections, and consistency of other methods; and provided leadership in the assemblage of this document.

PREFACE The standard methods described in the Soil Survey Investigations Report (SSIR) No. 42, Soil Survey Laboratory Methods Manual are those used by the Soil Survey Laboratory (SSL), National Soil Survey Center (NSSC). Included in the SSIR No. 42 are descriptions of current as well as obsolete methods, both of which are documented by method codes and linked with analytical results that are stored in the SSL database. This linkage between laboratory method codes and the respective analytical results is reported on the SSL data sheets. The methods in current use at this laboratory are described in enough detail that they can be performed in many laboratories without reference to other sources. An introduction to each group of related methods describes common characteristics. However, some repetition is included in order to make the method descriptions complete in themselves and to minimize reference to other parts of the manual. Some analytical results in the SSL national database were obtained using procedures that are no longer used at the SSL. Descriptions for these procedures are located in a section following the current methods. Information is not available to describe these procedures in the same detail as used to describe the current methods in the laboratory. Since the publication of the SSIR No. 42 (1996), there has been a significant increase in the number and kinds of methods performed at the SSL, resulting in a re-structuring of the method codes. As in past versions of the SSIR No. 42, the current method codes are hierarchical and alphanumerical. However, the obsolete method code structure had only a maximum of four characters, e.g., 6A2b, whereas the new structure has more characters, carrying more information about the method, e.g., particle-size and sample weight bases for reporting data. This version of the SSIR No. 42 carries not only the new method codes but also the older ones as well. The table for cross-referencing these older codes precede the method descriptions of the obsolete SSL methods. This linkage between the method code systems is important to maintain, as many older SSL data sheets and scientific publications report these older codes. The table of contents presents the ensemblage of this manual, beginning with the current methods and codes followed by obsolete methods with respective obsolete codes. The SSL data have been provided in reports, e.g., Primary and Supplementary Characterization Data Sheets, and in electronic forms, including tapes, disks, and CD-ROMs. More recently, other reports have been developed, e.g., Soil Taxonomy Characterization Data Sheets, and data are available via the NRCS Soils web site http://soils.usda.gov/. Historically, the SSIR No. 42 has described and assigned method codes only to those data reported on the Primary Characterization Data Sheets. This tradition is followed in this version of the SSIR No. 42. With the exception of some SSL primary analytical data included for user convenience, the data on the Supplementary and Taxonomy Characterization Data Sheets are derived data, using analytical data as a basis for calculation and do not carry method codes. Data on the Supplementary and Taxonomy Characterization Data Sheets are not described in this manual. For more detailed information about the calculation and application of these derived values, refer to the other important source documents provided by the United States Department of Agriculture, Natural Resources Conservation Service (USDA-NRCS) referenced in this maual. The methods described herein identify the specific type of analytical or calculated data. Most of these methods are analytical in nature, i.e., quantitative or semi-quantitative measurements, and include physical, chemical, mineralogical, and biological analyses. Sample collection and preparation in the field and the laboratory are also described. Historically, the SSIR No. 42 has described some derived values, e.g., coefficient of linear extensibility (COLE) and water retention difference (WRD) and reported these values along with the analytical data on the SSL Primary Characterization Data Sheets. This version of the SSIR No. 42 follows this tradition. Since the publication of the SSIR No. 42 (1996), several more derived values have been added to the Primary Characterization Data Sheets. While these data have been assigned method codes, detailed descriptions are not included in this version of the SSIR No. 42. For

more detailed information about the calculation and application of these derived values, refer to other important source documents provided by USDA-NRCS referenced in this manual. The purpose of this manual is to document methodology and to serve as a reference for the laboratory analyst. The standard methods described in this SSIR No. 42, Soil Survey Laboratory Methods Manual, Version 4.0 replaces as a methods reference all earlier versions of the SSIR No. 42 (1989, 1992, and 1996, respectively) and SSIR No. 1, Procedures for Collecting Soil Samples and Methods of Analysis for Soil Survey (1972, 1982, and 1984). All SSL methods are performed with methodologies appropriate for the specific purpose. The SSL SOP’s are standard methods, peer-recognized methods, SSL-developed methods, and/or specified methods in soil taxonomy (Soil Survey Staff, 1999). An earlier version of this manual (1996) also served as the primary document from which a companion manual, Soil Survey Laboratory Information Manual (SSIR No. 45, 1995), was developed. The SSIR No. 45 describes in greater detail the application of SSL data. Trade names are used in the manual solely for the purpose of providing specific information. Mention of a trade name does not constitute a guarantee of the product by USDA nor does it imply an endorsement by USDA. Rebecca Burt, Editor Reseach Soil Scientist Soil Survey Investigations USDA-NRCS Lincoln, Nebraska

USDA Nondiscrimination Statement The U.S. Department of Agriculture (USDA) prohibits discrimination in all its programs and activities on the basis of race, color, national origin, sex, religion, age, disability, political beliefs, sexual orientation, and marital or family status. (Not all prohibited bases apply to all programs.) Persons with disabilities who require alternative means for communication of program information (Braille, large print, audiotape, etc.) should contact USDA's TARGET Center at 202-720-2600 (voice and TDD). To file a complaint of discrimination write USDA, Director, Office of Civil Rights, Room 326W, Whitten Building, 14th and Independence Avenue, SW, Washington, DC 20250-9410 or call 202-720-5964 (voice or TDD). USDA is an equal opportunity provider and employer.

CONTRIBUTORS
Laboratory data are critical to the understanding of the properties and genesis of a single pedon, as well as to the understanding of fundamental soil relationships based on many observations of a large number of soils. The development of laboratory methods, the analytical database, and the soil relationships based on those data are the cumulative effort of several generations of scientists. These efforts may be defined as methods development, database design and development, and investigations of data relationships. Methods development in the Soil Survey Laboratory results from a broad knowledge of soils, encompassing topical areas of pedology, geomorphology, micromorphology, physics, chemistry, mineralogy, biology, and field and laboratory sample collection and preparation. The following lists many of these contributing scientists, some of whom have since retired from USDA-NRCS and/or are deceased. Some of these contributions are cited throughout this manual as scientific publications. The following list is not comprehensive for developmental work preceding the formation of the Soil Survey Laboratory in Lincoln, Nebraska. In addition to the scientists, the current Soil Survey Laboratory technicians are also listed. These analysts play a key role not only in performing the analyses but also in developing new or modifying old methods, and ensuring data quality. Scientists (past and current) and physical science technicians (current) are listed alphabetically as follows: Scientists: Lyle T. Alexander, Steven L. Baird, Otto W. Baumer, Ellis C. Benham, C. Reese Berdanier Jr., Wade A. Blankenship, Benny R. Brasher, Laurence E. Brown, Rebecca Burt, John G. Cady, Frank J. Carlisle, James H. DeMent, Joe D. Dixon, Moustafa A. Elrashidi, Richard R. Ferguson, Klaus W. Flach, Carol D. Franks, Donald P. Franzmeier, Erling E. Gamble, Don W. Goss, Robert B. Grossman, George C. Holmgren, C. Steven Holzhey, Robert H. Jordan, R. Leo Juve, Fredrick M. Kaisaki, John M. Kimble, Leo C. Klameth, Ellis G. Knox, Susan E. SamsonLiebig, Warren C. Lynn, Maurice J. Mausbach, M. Dewayne Mays, Dean C. McMurty, Milton M. Meyer, John L. Millet, Reuben E. Nelson, W. Dennis Nettleton, Carolyn G. Olson, Ronald F. Paetzold, Roger B. Parsons, Richard L. Pullman, Ivan W. Ratcliff Jr., Thomas G. Reinsch, Earnest D. Rivers, Sam J. Ross, Philip J. Schoeneberger, Leo G. Shields, Christopher W. Smith, Terrence M. Sobecki, John A. Thompson, Geroge W. Threlkeld, Michael A. Wilson, Douglas A. Wysocki, Ronald D. Yeck, and Keith K. Young. Physical Science Technicians: Larry V. Arnold, Michelle A. Etmund, Kristina Goings, Diane G. Hooper, Patricia E. Jones, Janis L. Lang, Christopher W. Lee, Valerie M. Murray, James F. Neal, Kathyrn L. Newman, Michael J. Pearson, Susan J. Reidel, Crystal A. Schaecher, Emily K. Rose Seifferlein, James E. Thomas, Pamela A. VanNeste, Lester E. Williams, and Thomas J. Zimmer.

ACKNOWLEDGEMENTS
We gratefully acknowledge those individuals who provided technical review of the Soil Survey Laboratory methods by topical area. Their thoughtful comments and suggestions are deeply appreciated. These reviewers of the Soil Survey Laboratory Methods Manual, Soil Survey Investigations Report No. 42, Version 4.0 are listed alphabetically as follows: Reviewers Jacob H. Dane, Department of Agronomy and Soils, 202 Funchess Hall, Auburn University, Auburn, Alabama 36849-5412 Richard P. Dick, Department of Crop and Soil Science, Agricultural and Life Sciences Building 3067, Oregon State University, Corvallis, Oregon 97331 Glendon W. Gee, 1637 Birch Avenue, Richland, Washington, 99352 Mark Flock, Vice-President, Soil and Plant Analysis Council, Brookside Laboratory, Inc., 308 S. Main Street, New Knoxsville, Ohio 45871 Willie G. Harris, Soil and Water Science Department University of Florida, 2169 McCarty Hall, Gainesville, Florida 32611-0000 Yash Kalra, Canadian Forest Service, 5320 – 122 Street, Edmonton, Alberta, Canada T6H 3S5 Robert Miller, Coordinator, North American Proficiency Testing Program, Soil and Crop Science Department, Colorado State University, Fort Collins, Colorado 80523

METHODS OF ANALYSIS FOR SOILS, WATER, AND BIOLOGICAL MATERIALS CONTENTS METHOD TITLE SAMPLE COLLECTION AND PREPARATION Field Sample Collection and Preparation
Site Selection Geomorphic Pedon Water Biological

METHOD CODE 1 1A
1A1 1A1a 1A1b 1A1c 1A1d

PAGE 1 1
1 1 1 1 1

Laboratory Sample Collection and Preparation
Soils Samples Bulk Natural Fabrics Clods Cores Preparation Field-Moist Preparation Whole Soil Histosol Analysis Biological Analysis <2-mm Fraction Chemical and Selected Physical Analysis 1500-kPa Water Content Field-Field-Moist/Air-dry Ratio <2-mm Fraction Sieved to < 0.425 mm Atterberg Limits Air-Dry Preparation Whole Soil Aggregate Stability Repository Samples <2-mm Fraction Standard Chemical, Physical, Mineralogical Analysis Salt Analysis 1500-kPa Water Content Air-Dry/Oven-Dry Ratio Presence of Carbonates <2-mm Fraction Sieved to <0.425 mm Atterberg Limits <2-mm Fraction Processed to ≈ 180 µm

1B

1B1 1B1a 1B1a1 1B1a2 1B1a3 1B1a4 1B1b 1B1b1 1B1b1a 1B1b1a1 1B1b1a2 1B1b1b 1B1b1b1 1B1b1b2 1B1b1b3 1B1b1c 1B1b1c1 1B1b2 1B1b2a 1B1b2a1 1B1b2a2 1B1b2b 1B1b2b1 1B1b2b2 1B1b2b3 1B1b2b4 1B1b2b5 1B1b2c 1B1b2c1 1B1b2d

16
16 16 16 17 17 17

17 19 20 20 20 20 20 20 21 21 21 21 21 21 22 22 22 22 23 23 23 23 23 24

i

CONTENTS METHOD TITLE
Total Carbon, Nitrogen, and Sulfur Carbonates and/or Gypsum Chemical Analysis of Organic Materials <2-mm Fraction Sieved to 75 µm Major and/or Trace Elements Particles >2 mm Particle-Size Analysis Particle-Size Analysis, Recorded 2- to 20-mm Fraction Processed to <2-mm Chemical, Physical, and Mineralogical Analysis 2- to 20-mm Fraction Processed to <2-mm and Recombined with <2-mm Fraction Chemical, Physical, and Mineralogical Analysis Proportion and Particle-Size of Air-Dry Rock Fragments that Resist Abrupt Immersion in Tap Water Particle-Size Analysis, Not Recorded Whole-Soil Processed to <2-mm Chemical, Physical, and Mineralogical Analysis Water Samples Preparation

METHOD CODE
1B1b2d1 1B1b2d2 1B1b2d3 1B1b2e 1B1b2e1 1B1b2f 1B1b2f1 1B1b2f1a 1B1b2f1a1 1B1b2f1a1a 1B1b2f1a2 1B1b2f1a2a 1B1b2f1a3 1B1b2f1b 1B1b2f1b1 1B1b2f1b1a 1B2 1B2a 1B2b

PAGE
24 24 24 24 24 24 25 25 25 25 26 26 27 25 26 26 29 29 29 30 30 30 30 30 30 30 30 30 30 30 30 30 31 31 31 31 31 31 31 31 31

Biological Materials 1B3 Samples 1B3a Biology Bulk Sample 1B3a1 Microbial Biomass Sample 1B3a2 Preparation 1B3b Field-Moist Preparation 1B3b1 <2-mm Fraction 1B3b1a Microbial Biomass 1B3b1a1 Air-Dry Preparation 1B3b2 <2-mm Fraction Sieved <53 µm, with <53 µm (C-Mineral) and 1B3b2a > 53 µm (Particulate Organic Matter) Processed to ≈ 180 µm Total Carbon, Nitrogen, and Sulfur Analysis 1B3b2a1 <2-mm Fraction 1B3b2b Other Biological Analyses 1B3b2b1 Dry (50 C) Preparation 1B3b3 Roots 1B3b3a Root Biomass 1B3B3a1 Roots Processed to ≈ 180 µm 1B3b3a1a Total Carbon, Nitrogen, and Sulfur Analysis 1B3b3a1a1 Plants 1B3b3b Plant Biomass 1B3b3b1 Plants Processed to ≈ 180 µm 1B3b3b1a Total Carbon, Nitrogen, and Sulfur Analysis 1B3b3b1a1

ii

CONTENTS METHOD TITLE CONVENTIONS Methods and Codes Data Types Particle-Size Fraction Base for Reporting Data
Particles <2 mm Particles >2mm

METHOD CODE 2 2A 2B 2C
2C1 2C2

PAGE 31 31 32 32
32 32

Sample Weight Base for Reporting Data
Air-Dry/Oven-Dry Field-Field-Moist/Oven-Dry Correction for Crystal Water

2D

2D1 2D2 2D3

33 33 33

33

Significant Figures and Rounding Data Sheet Symbols SOIL PHYSICAL AND FABRIC-RELATED ANALYSES Particle-Size Distribution Analysis

2E 2F 3 3A

33 33 34 34
34 34 41 41 50 46 46 51 46 46 52 47 47 53 47 47 53 48 48 55

Particles <2 mm 3A1 Pipet Analysis for routinely reported size fractions 3A1a (1, 0.5, 0.25, 0.1, 0.047 mm, <20 µm, and <2 µm), with or without <0.2-µm fraction, with or without <2-µm carbonate clay Pipet Analysis with Standard Pretreatments and Dispersion 3A1a1 Air-Dry 3A1a1a Field-Moist 3A1a1b Pipet Analysis with Carbonate Removal 3A1a2 Air-Dry 3A1a2a Field-Moist 3A1a2b Pipet Analysis with Iron Removal 3A1a3 Air-Dry 3A1a3a Field-Moist 3A1a3b Pipet Analysis with Silica Removal 3A1a4 Air-Dry 3A1a4a Field-Moist 3A1a4b Pipet Analysis with Ultrasonic Dispersion 3A1a5 Air-Dry 3A1a5a Field-Moist 3A1a5b Pipet Analysis with Water Dispersion 3A1a6 Air-Dry 3A1a6a Field-Moist 3A1a6b

iii

CONTENTS METHOD TITLE
Particles >2 mm Weight Estimates By Field and Laboratory Weighing From Volume and Weight Estimates Volume Estimates

METHOD CODE
3A2 3A2a 3A2a1 3A2a2 3A2b

PAGE
66 67 67 70 70

Bulk Density
Saran-Coated Natural Clods Field State 33 kPa Oven-dry Rewet Reconstituted 33 kPa Oven-Dry Compliant Cavity Field State Ring Excavation Field State Frame Excavation Field State Soil Cores Field State

3B
3B1 3B1a 3B1b 3B1c 3B1d 3B2 3B2a 3B2b 3B3 3B3a 3B4 3B4a 3B5 3B5a 3B6 3B6a

73
75 75 80 86 89 99 99 99 98 98 100 100 102 102 104 104

Water Retention
Pressure-Plate Extraction 6 10, 33, 100, or 200 kPa Water Retention <2 mm Sieved, Air-Dry Natural Clods Soil Cores Rewet Reconstituted Pressure-Membrane Extraction 1500 kPa Water Retention <2 mm Sieved, Air-Dry <2 mm Sieved, Field-Moist Water Retention at Field State

3C
3C1 3C1a-e 3C1a-e1a 3C1a-d2 3C1a-d3 3C1c4 3C1c5 3C2 3C2a 3C2a1a 3C2a1b 3C3

105
106 106 106 108 114 117 121 125 125 125 129 131

iv

CONTENTS METHOD TITLE METHOD CODE 3D
3D1 3D2 3D3 3D4 3D4a 3D5 3D5a 3D5b 3D5c 3D6 3D7 3D8 3D9 3D10 3D11 3D12 3D13

PAGE

Ratios and Estimates Related to Particle Size Analysis, Bulk Density, and Water Retention
Air-Dry/Oven-Dry Ratio Field-Moist/Oven-Dry Ratio Correction for Crystal Water Coefficient of Linear Extensibility Air-Dry or Oven-Dry to 33-kPa Tension Water Retention Difference, Whole Soil Between 33-kPa and 1500-kPa Tension Between 10-kPa and 1500-kPa Tension Between 33-kPa and 1500-kPa (Air-Dry) Tension 1500 kPa Water/Clay Ratio Total Silt Fraction Total Sand Fraction 2- to 5-mm Fraction 5- to 20-mm Fraction 20- to 75-mm Fraction 0.1- to 75-mm Fraction >2-mm Fraction

132
132 132 132 135 135 137 137 137 137 138 138 138 138 139 139 139 139

Micromorphology
Thin sections Preparation Interpretation

3E

3E1 3E1a 3E1b

140
140 140 143

Wet Aggregate Stability

Wet Sieving Air-dry 2 to 1 mm 2- to 0.5-mm Aggregates Retained Pycnometer Gas Displacement Oven-dry <2 mm >2 mm Liquid Limit Air-Dry, <0.4 mm Field-Moist, <0.4 mm Plasticity Index Air-Dry, <0.4 mm Field-Moist, <0.4 mm

3F

3F1 3F1a 3F1a1 3F1a1a 3G1 3G1a 3G1a1 3G1a2 3H1 3H1a1 3H1b1 3H2 3H2a1 3H2b1

163
163 163 163 163

Particle Density

3G

165
165 165 165 165

Atterberg Limits

3H

167
167 167 167 167 167 167

v

CONTENTS METHOD TITLE SOIL AND WATER CHEMICAL EXTRACTIONS AND ANALYSES Acid Standardization Ion Exchange and Extractable Cations
Displacement after Washing NH4OAc, pH 7 Automatic Extractor 2 M KCl Rinse Steam Distillation HCl Titration Cation Exchange Capacity (CEC-7) Air-Dry, <2 mm Field-Moist, <2 mm Atomic Absorption Spectrophotometer Calcium, Magnesium, Potassium, and Sodium Air-Dry, <2 mm Field-Moist, <2 mm NH4Cl, Neutral Unbuffered Automatic Extractor 2M KCl Rinse Steam Distillation HCl Titration Cation Exchange Capacity Air-Dry, <2 mm Field-Moist, <2 mm Atomic Absorption Spectrophotometer Calcium, Magnesium, Potassium, and Sodium Air-Dry, <2 mm Field-Moist, <2 mm BaCl2-Triethanolamine, pH 8.2 Extraction Automatic Extractor Automatic Titrator Back Titration with HCl Extractable Acidity Air-Dry, <2 mm Field-Moist, <2 mm Centrifuge Automatic Titrator Back Titration with HCl Extractable Acidity Air-Dry, <2 mm Field-Moist, <2 mm

METHOD CODE 4 4A 4B
4B1 4B1a 4B1a1 4B1a1a 4B1a1a1 4B1a1a1a 4B1a1a1a1 4B1a1a1a1a1 4B1a1a1a1b1 4B1a1b 4B1a1b1-4 4B1a1b1-4a1 4B1a1b1-4b1 4B1b 4B1b1 4B1b1a 4B1b1a1 4B1b1a1a 4B1b1a1a1 4B1b1a1a1a1 4B1b1a1a1b1 4B1a1b 4B1b1b1-4 4B1b1b1-4a1 4B1b1b1-4b1 4B2 4B2a 4B2a1 4B2a1a 4B2a1a1 4B2a1a1a1 4B2a1a1b1 4B2b 4B2b1 4B2b1a 4B2b1a1 4B2b1a1a1 4B2b1a1b1

PAGE 167 167 173
173 173 173 173 173 173 173 173 173 184 184 184 184 181 181 181 181 181 181 181 181 188 188 188 188 191 191 191 191 191 191 191 194 194 194 194 194 194

vi

2 (Sum of Cations) CEC-8. Calculated Base Saturation by Sum of NH4OAc Extractable Bases + 1 N KCl Extractable Aluminum. Set to 100% Base Saturation by CEC-8. Calculated Sum of NH4OAc Extractable Bases + 1 N KCl Extractable Aluminum .2. pH 7 Sum of Extractable Bases by NH4OAc. Calculated Base Saturation by CEC-7. Not Calculated vii METHOD CODE 4B3 4B3a 4B3a1 4B3a1a 4B3a1a1-2 4B3a1a1-2a1 4B3a1a1-2b1 4B4 4B4a 4B4a1 4B4a1a 4B4a2 4B4a2a 4B4b 4B4b1 4B4b1a 4B4b1b 4B4b2 4B4b2a 4B4b2b 4B4c 4B4c1 4B4c1a 4B4c1b 4B4c2 4B4c2a 4B4c2b 4B4c3 4B4c3a 4B4c3b 4B4c4 4B4c4a 4B4c4b 4B4d 4B4d1 4B4d1a 4B4d1b PAGE 197 197 197 197 197 197 197 201 201 201 201 201 201 202 202 202 202 202 202 202 202 202 202 202 203 203 203 203 203 203 203 203 203 204 204 204 204 204 .2. Calculated Aluminum Saturation by Sum of NH4OAc Extractable Bases + 1 N KCl Extractable Aluminum. Calculated CEC-8. pH 7 (CEC-7) Base Saturation by CEC-7. Set to 100% Base Saturation by NH4Cl Base Saturation by NH4Cl.2.2 Base Saturation by CEC-8. Not Calculated Aluminum Saturation Aluminum Saturation by ECEC Aluminum Saturation by Sum of NH4OAc Extractable Bases + 1 N KCl Extractable Aluminum. Calculated Cation Exchange Capacity (CEC) CEC-8. pH 7.2. Calculated Sum of Extractable Bases by NH4Cl Sum of Extractable Bases by NH4Cl. Calculated Base Saturation by NH4Cl. Calculated Base Saturation by CEC-8. Not Calculated Base Saturation Base Saturation by NH4OAc. Mn Air-Dry. Not Calculated Base Saturation by ECEC Base Saturation by Sum of NH4OAc Extractable Bases + 1 N KCl Extractable Aluminum.CONTENTS METHOD TITLE 1 N KCl Extraction Automatic Extractor Inductively Coupled Plasma Spectrophotometer Radial Mode Al. Not Calculated Effective Cation Exchange Capacity (ECEC) Sum of NH4OAc Extractable Bases + 1 N KCl Extractable Aluminum . <2 mm Field-Moist. <2 mm Ratios and Estimates Related to Ion Exchange and Extractable Cations Sum of Extractable Bases Sum of Extractable Bases by NH4OAc.

<2 mm Field-Moist. 24h. <2 mm 1 M KCl pH Air-Dry. Dual Beam 4D 4D1 4D1a 4D1a1a1 4D1a1a1a 4D1a1a1a1-2 4D1a1a1a1-2a-b1 4D1a1a1a1-2b1 4D2 4D2a 4D2a1 4D2a1a 217 219 219 219 219 219 219 219 223 223 223 223 viii .CONTENTS METHOD TITLE Activity 1500-kPa Water/CEC-7 METHOD CODE 4B4e 4B4e1 PAGE 204 204 Reaction Soil Suspensions Electrode Standard Glass Body Combination Digital pH/Ion Meter 1 N NaF. <2 mm Field-Moist. <2 mm 1:2 0.01 M CaCl2 pH Combination pH-reference electrode Automatic Titrator 1:1 water pH Air-Dry.5 – 7.01 M CaCl2 pH Air-Dry. Final Solution ≈ 0. pH 7.8 Air-Dry. 1 M KCl UV-Visible Spectrophotometer. <2 mm Field-Moist. <2 mm 4C 4C1 4C1a 4C1a1 4C1a1a 4C1a1a1 4C1a1a1a1 4C1a1a1b1 4C1a1a2 4C1a1a2a1 4C1a1a3 4C1a1a4 4C1a2 4C1a2a 4C1a2a1 4C1a2a1a1 4C1a2a1b1 4C1a2a2 4C1a2a2a1 4C1a2a2b1 4C1a2a3 4C1a2a3a1 4C1a2a3b1 204 204 204 204 204 205 205 205 207 207 209 211 213 213 213 213 213 213 213 213 215 215 215 Soil Test Analyses Anion Resin Extraction Two-Point Extraction 1 h. Dual-Beam Phosphorus (2 points) Air-Dry. <2 mm Field-Moist. <2 mm Field-Moist. <2 mm Saturated Paste pH Air-Dry. <2 mm Aqueous Extraction Single-Point Extraction 1:10. <2 mm Oxidized pH Organic Materials pH. 30 min UV-Visible Spectrophotometer.

<2 mm Bray P-2 Extraction UV-Visible Spectrophotometer. <2 mm Flow Injection. Potassium. <2 mm Field-Moist. <2 mm Field-Moist. <2 mm Olsen Sodium-Bicarbonate Extraction UV-Visible Spectrophotometer. Copper. <2 mm Field-Moist. <2 mm Bray P-1 Extraction UV-Visible Spectrophotometer. Nickel. Selenium. Dual Beam Phosphorus Air-Dry. <2 mm Field-Moist. Calcium. Phosphorus. Arsenic. Cadmium. Manganese. <2 mm Flow Injection. Barium. <2 mm 4D6b1a1-18a1 Field-Moist. 4D6b1a1-18 Chromium. Dual Beam Phosphorus Air-Dry.CONTENTS METHOD TITLE Phosphorus Air-Dry. Iron. 3 Extraction 4D6 UV-Visible Spectrophotometer. <2 mm Field-Moist. Automated Ion Analyzer Phosphorus Air-Dry. Dual Beam 4D6a Phosphorus 4D6a1 Inductively Coupled Plasma Atomic Emission 4D6b Spectrophotometer Axial Mode 4D6b1 Ultrasonic Nebulizer 4D6b1a Aluminum. <2 mm 4D6b1a1-18b1 Citric Acid Soluble UV-Visible Spectrophotometer. Dual Beam Phosphorus Air-Dry. Automated Ion Analyzer Phosphorus Air-Dry. Magnesium. and Zinc Air-Dry. Sodium. <2 mm Field-Moist. Dual-Beam Phosphorus Air-Dry. <2 mm METHOD CODE 4D2a1a1 4D2a1a1a1 4D2a1a1b1 4D2a1b 4D2a1b1 4D2a1b1a1 4D2a1b1b1 4D3 4D3a 4D3a1 4D3a1a1 4D3a1b1 4D3b 4D3b1 4D3b1a1 4D3b1b1 4D4 4D4a 4D4a1 4D4a1a1 4D4a1b1 4D5 4D5a 4D5a1 4D5a1a1 4D5a1b1 PAGE 223 223 223 226 226 226 226 231 231 231 231 231 234 234 234 234 239 239 239 239 239 242 242 242 242 242 246 246 246 249 249 249 249 249 249 253 253 253 253 253 Mehlich No. Cobalt. Lead. <2 mm Field-Moist. < 2 mm 4D7 4D7a 4D7a1 4D7a1a1 4D7a1b1 ix .

<2 mm. <2 mm Field-Moist. Electronic Carbonates Calcium Carbonate Air-Dry. <2 mm Air-Dry. <2 mm METHOD CODE 4D8 4D8a 4D8a1 4D8a1a1 4D8a1b1 4D9 4D9a 4D9a1 4D9a1a 4D9a1a1-2 4D9a1a1-2a1 4D9a1a1-2b1 4D9a1a1-2b2-3 4D10 4D10a 4D10a1 4D10a1a 4D10a1a1 4D10a1a1a1 4D10a1a1b1 PAGE 257 257 257 257 257 260 260 260 260 260 260 260 260 265 265 265 265 265 265 265 Carbonate and Gypsum 3 N HCl Treatment CO2 Analysis Manometer. <2 mm 1 M KCl Extraction Cadmium-Copper Reduction Sulfanilamide N-1-Naphthylethylenediamine Dihydrochloride Flow-Injection. Automated Ion Analyzer Nitrate-Nitrite Air-Dry.CONTENTS METHOD TITLE New Zealand P Retention UV-Visible Spectrophotometer. qualitative and quantitative Air-Dry. Fumigated and Non-fumigated Anaerobic Incubation 2 M KCl Extraction Ammonia – Salicylate Flow Injection. <2 mm Air-Dry. Automated Ion Analyzer N as NH3 – Mineralizable N Air-Dry. 2 to 20 mm 4E 4E1 4E1a 4E1a1 4E1a1a 4E1a1a1 4E1a1a1a1 4E1a1a1a2 4E2 4E2a 4E2a1 4E2a1a 4E2a1a 4E2a1a1a1 4E2a1a1a2 269 269 269 269 269 269 269 269 273 273 273 273 273 273 273 Electrical Conductivity and Soluble Salts Aqueous Extraction 1:2 Aqueous Extraction Conductivity Bridge Electrical Conductivity 4F 4F1 4F1a 4F1a1 4F1a1a 277 277 277 277 277 x . <2 mm Field-Moist. Dual Beam Phosphorus Air-Dry. <2 mm Field-Moist. 2 to 20 mm Aqueous Extraction Precipitation in Acetone Conductivity Bridge Electrical Conductivity Gypsum. <2 mm Field-Moist.

<2 mm Saturated Paste Extraction Automatic Extractor Atomic Absorption Spectrophotometer Calcium. <2 mm Field-Moist. Iron. Bromide. Chloride. Nitrate. <2 mm Resistivity Air-Dry. <2 mm Saturated Paste Gravimetric Water Percentage Air-Dry. and Sodium Air-Dry. Phosphate. <2 mm Ion Chromatograph Conductivity Detector Self-Regeneration Suppressor. Calculated with Saturated Paste Extraction Sodium Adsorption Ratio (SAR) Estimated Total Salt METHOD CODE 4F1a1a1 4F1a1a1a1 4F2 4F2a 4F2a1 4F2a1a1 4F2b 4F2b1 4F2b1a1 4F2b2 4F2b2a1 4F2c 4F2c1 4F2c1a 4F2c1a1-4 4F2c1a1-4a1 4F2c1b 4F2c1b1 4F2c1b1a 4F2c1b1a1-8 4F2c1b1a1-8a1 4F2c1c 4F2c1c1 4F2c1c1a 4F2c1c1a1-2 4F2c1c1a1-2a1 4F3 4F3a 4F3a1 4F3a2 4F3b 4F3c PAGE 277 277 278 282 282 282 284 284 284 286 286 289 289 290 290 290 294 294 294 294 294 299 299 299 299 299 301 301 301 302 303 303 Selective Dissolutions Dithionite-Citrate Extraction Atomic Absorption Spectrophotometer Aluminum. Potassium. and Manganese Air-Dry. <2 mm Ratios and Estimates Related to Soluble Salts Exchangeable Sodium Percentage (ESP) ESP. Fluoride. Nitrite. and Sulfate Air-Dry. Calculated without Saturated Paste Extraction ESP. <2 mm 4G 4G1 4G1a 4G1a1-3 4G1a1-3a1 4G1a1-3b1 303 307 307 307 307 307 xi . H2SO4 Carbonate and Bicarbonate Air-Dry. <2 mm Conductivity Bridge Electrical Conductivity Air-Dry. Magnesium.CONTENTS METHOD TITLE Salt Prediction Air-Dry. Acetate. <2 mm Automatic Titrator Combination pH-Reference Electrode Acid Titration.

Arsenic. Vanadium. Dual Beam Transmittance Optical Density Air-Dry. <2 mm Ratios and Estimates Related to Ammonium Oxalate Extraction Al + 1⁄2 Fe Sodium Pyrophosphate Extraction Atomic Absorption Spectrophotometer Aluminum. Thallium. Copper. Chromium. Iron. Beryllium. <2 mm Acid Digestion K2Cr2O7 + (H2SO4 + H3PO4 Digestion) Nesbitt Bulb CO2 Evolution. <2 mm Field-Moist. Barium. <2 mm 4H 4H1 4H1a 4H1a1 4H1a1a 4H1a1a1 4H1a1a1a 4H1a1a1a1-20 324 324 324 324 324 324 324 324 4H1a1a1-20a1 324 xii . Molybdenum. Lead. Iron. <2 mm Field-Moist. <2 mm Field-Moist. Tungsten.CONTENTS METHOD TITLE METHOD CODE 4G2 4G2a 4G2a1 4G2a1a 4G2a1a1-5 4G2a1a1-5a1 4G2a1a1-5b1 4G2a2 4G2a2a 4G2a2a1 4G2a2a1a1 4G2a2a1b1 4G2b 4G2b1 4G3 4G3a 4G3a1-3 4G3a1-3a1 4G3a1-3b1 4G3b 4G3b1 4G3b1 4G3b1a 4G3b1a1 4G3b1a1a1 4G3b1a1b1 PAGE Ammonium Oxalate Extraction Automatic Extractor Inductively Coupled Plasma Atomic Emission Spectrophotometer Radial Mode Aluminum. Manganese. Antimony. <2 mm UV-Visible Spectrophotometer. Strontium. Phosphorus. and Silicon Air-Dry. Tin. and Manganese Air-Dry. Gravimetric Organic Carbon Air-Dry. <2 mm Field-Moist. Cadmium. Nickel. Manganese. <2 mm 312 312 312 312 312 312 312 312 312 312 312 312 317 317 317 317 317 317 317 317 317 317 317 317 317 317 Total Analysis Acid Digestion HNO3 + HCl Digestion Microwave Inductively Coupled Plasma Atomic Emission Spectrophotometer Axial Mode Ultrasonic Nebulizer Silver. Cobalt. Phosphorus. Zinc Air-Dry.

Phosphate. Magnesium. Acetate. Iron.CONTENTS METHOD TITLE HCl Digestion Water Bath Flow through Hydride-Generation and Atomic Absorption Spectrophotometer Arsenic and Selenium Air-Dry. Nitrate. <2 mm Oven-Dry. Titanium Air-Dry. and Sulfur Air-Dry. <2 mm Cold Vapor Atomic Absorption Spectrophotometer Mercury Air-Dry. Fluoride. Magnesium. and Sulfate Automatic Titrator Combination pH-reference Electrode Acid Titration. <2 mm HF + HNO3 + HCl Digestion Microwave Boric Acid Inductively Coupled Plasma Atomic Emission Spectrophotometer Radial Mode Aluminum. H2SO4 Carbonate and Bicarbonate 4I 4I1 4I1a 4I1a1 4I1a1a 4I1a1a1 4I2 4I2a 4I2a1 4I2b 4I2b1-4 4I2c 4I2c1 4I2c1a 4I2c1a1-8 4I2d 4I2d1 4I2d1a 4I2d1a1-2 352 352 352 352 352 352 353 353 353 355 355 358 358 358 358 363 363 363 363 xiii . <2 µm Dry Combustion Thermal Conductivity Detector Carbon. and Sodium Ion Chromatograph Conductivity Detector Self-Regeneration Suppressor Bromide. Silicon. Manganese. Calcium. Zirconium. Potassium. Nitrogen. Nitrite. Chloride. Sodium. Potassium. Phosphorus. <2 mm METHOD CODE 4H1a1b 4H1a1b1 4H1a1b1 4H1a1b1a1-2 4H1a1b1a1-2a1 4H1a1c 4H1a1c1 4H1a1c1a1 4H1b 4H1b1 4H1b1a 4H1b1a1 4H1b1a1a 4H1b1a1a1-11 4H1b1a1a1-11a1 4H1b1a1a1-11b2 4H2 4H2a 4H2a1-3 4H2a1-3a1 PAGE 331 331 331 331 331 336 336 336 341 341 341 341 341 341 341 341 347 347 347 347 Ground and Surface Water Analyses Reaction Electrode Standard Glass Body Combination Digital pH/Ion Meter pH Electrical Conductivity and Salts Conductivity Bridge and Cup Electrical Conductivity Atomic Absorption Spectrophotometer Calcium.

>53 µm (POM) Air-Dry. <53 µm (C-Min) 368 368 369 371 374 375 375 375 376 376 376 376 379 379 379 379 381 381 381 381 381 381 385 385 385 385 385 385 385 5A 5B 5C 5D 5E 6 6A 6A1 6A1a 6A1a1 6A1a1a1 6A2 6A2a 6A2a1 6A2a1a1 6A3 6A3a 6A3a1 6A3a1a 6A3a1a1 6A3a1a1a1 6A4 6A4a 6A4a1 6A4a1a 6A4a1a1-3 6A4a1a1-3a1 6A4a1a1-3a2 xiv . Phosphorus.02 M KMnO4 Extraction UV-Visible Spectrophotometer. Iron. Dual Beam Hot Water Extractable Organic Carbon Air-Dry.CONTENTS METHOD TITLE Total Analysis Inductively Coupled Plasma Atomic Emission Spectrophotometer Radial Mode Ultrasonic Nebulizer Aluminum. and Sulfur Air-Dry. Manganese. <2 mm Acid Dissolution 1 N HCl Dissolution + FeCl2 Gas Chromatography CO2 Analysis Carbonates Air-Dry. <2 mm 0. Dual Beam Active Carbon Air-Dry. and Silicon METHOD CODE 4I3 4I3a 4I3a1 4I3a1a 4I3a1a1-5 PAGE 365 365 365 365 365 ANALYSIS OF ORGANIC SOILS OR MATERIALS 5 Mineral Content Pyrophosphate Color Fiber Volume Melanic Index Ratios and Estimates Related to Organic Matter SOIL BIOLOGICAL AND PLANT ANALYSES Soil Analyses 0. <2 mm Particulate Organic Matter and Carbon-Mineral Total Analysis Dry Combustion Thermal Conductivity Detector Carbon. Nitrogen.5 M K2SO4 Extraction + Heating with Disodium Bicinchoninic Reagent UV-Visible Spectrophotometer.

K 300°C. Whole-Soil Fumigated. Mg Glycerol Solvated. Nitrogen. Plants (above-ground) 6C 6C1 6C2 6C3 6C3a 6C3a1 6C3a1a 6C3a1a1-3 6C3a1a1-3a1 6C3a1a1-3a2 394 394 394 394 394 394 394 394 394 394 Ratios and Estimates Related to Biological Analyses 6E MINERALOGY Instrumental Analyses X-Ray Diffraction Thin Film on Glass. and Sulfur Dry (50°C). Whole-Soil Non-Fumigated METHOD CODE 6B 6B1 6B1a 6B1a1 6B1a1a1 6B2 6B2a 6B2a1 6B2a1a 6B2a1a1 6B2a1a1a1-2 PAGE 388 388 388 388 388 388 388 388 388 388 388 Plant Analyses Root Biomass Plant (above-ground) Biomass Plant Nutrition Total Analysis Dry Combustion Thermal Conductivity Detector Carbon.CONTENTS METHOD TITLE Fumigation Incubation Gas Chromatography CO2 Analysis Soil Microbial Biomass Field-Moist. Automated Ion Analyzer N as NH3 – Mineralizable N Field-Moist. Roots Dry (50°C). K 500°C Thermogravimetric Analysis Thermal Analyzer Differential Scanning Colorimetry Thermal Analyzer Differential Thermal Analysis Thermal Analyzer 398 398 398 399 399 399 410 410 410 410 415 415 7 7A 7A1 7A1a 7A1a1 7A2 7A2a 7A3 7A3a 7A4 7A4a xv . Resin Pretreatment II Mg Room Temperature. Whole-Soil 2 M KCl Extraction Automatic Extractor Ammonia – Salicylate Flow Injection.

CONTENTS METHOD TITLE Surface Area N2 Adsorption Brunauer. Emmett and Teller Theory Vacuum Degassing Multi-Point Air-Dry. Epoxy Platy Grains Magnetic Separation Static Tube Separation Froth Flotation 7B 7B1 7B1a 7B1a1 7B1a2 7B2 7B2a 7B2b 7B2c 422 422 422 428 428 434 434 437 439 Ratios and Estimates Related to Optical Analysis Total Resistant Minerals 7C 7C1 442 442 Mineralogy Codes 443 xvi . <2 mm METHOD CODE 7A5 7A5a 7A5a1 7A5a1a 7A5a1a1 7A5a1a1a1 7A5a1a2 7A5a1a2a1 PAGE 418 418 418 418 418 418 418 418 Optical Analyses Grain Studies Analysis and Interpretation Separation by Heavy Liquids Grain Mounts. <2 mm Single Point Air-Dry.

0. Buchner Funnel (CEC-7) Direct Distillation Displacement Distillation 5 5A 5A1 5A1a 5A1b 619 619 620 xvii . pH 7.SOIL SURVEY LABORATORY METHODS (Obsolete Methods with Old Method Codes) METHOD TITLE SAMPLE COLLECTION AND PREPARATION Laboratory Preparation of Soil Samples Carbonate-Containing Material Carbonate-Indurated Material METHOD CODE 1 1B 1B3 1B4 PAGE 609 609 609 609 PARTICLE-SIZE ANALYSIS Particles <2 mm (pipet method) Air-Dry Samples Carbonate and Noncarbonate I Moist Samples Carbonate and Noncarbonate I 3 3A 3A1 3A1a 3A2 3A2a 610 610 610 612 613 613 FABRIC-RELATED ANALYSES Bulk Density Saran-Coated Clods Air-Dry 30-cm Absorption 1/3-Bar Desorption II 1/3-Bar Desorption III 1/10-Bar Desorption Paraffin Coated Clods Oven-Dry Nonpolar-Liquid-Saturated Clods 4 4A 4A1 4A1b 4A1c 4A1e 4A1f 4A1g 4A2 4A2a 4A4 4B1 4B1b 4B3 613 613 613 616 616 616 616 616 616 616 617 Water Retention Pressure-Plate Extraction Soil Pieces Sand-Table Absorption Thin Sections Moved-Clay Percentage Scanning Electron Microscope 4B 617 617 617 617 618 618 618 Micromorphology 4E 4E1 4E1c 4E2 618 ION EXCHANGE ANALYSES Cation Exchange Capacity (CEC) NH4OAc.

0. Automatic Titrator 5F1 626 626 6A1 6A1a 6A1b 6A1c 626 627 469 xviii . pH 8.2 5B 5B1 5B1a 5B1b 5B2 5B3 5B3a 5B3b 5B4 5B4a 5B4b 5B5 5B5b 624 624 624 624 624 624 625 625 625 625 625 625 625 Base Saturation 5C 5C2 625 625 625 Exchangeable Sodium Percentage (ESP) NH4OAc. Automatic Extractor Direct Distillation Steam Distillation I Steam Distillation II METHOD CODE 5A2 5A2a 5A4 5A5 5A5a 5A6 5A6a 5A7 5A7a 5A8 5A8a 5A8b 5A8c 5A9 5A9a 5A9b 5A9c PAGE 621 621 621 622 622 622 623 623 623 623 561 463 624 564 466 Extractable Bases NH4OAc.2 NH4OAc. pH 7. pH 7. pH 8.2 Barium by Flame Photometry NH4OAc. Leaching Tube Uncorrected (extractable) Corrected (exchangeable) NH4OAc.0). Automatic Extractor Corrected (exchangeable) NH4OAc. pH 7.0 (CEC-7. pH 8. Buchner Funnel Uncorrected (extractable) Corrected (exchangeable) KCl-TEA Extraction.0 (CEC-7.0. Mechanical Extraction Direct Distillation NH4OAc. pH 7. pH 7.0. pH 7.CONTENTS METHOD TITLE NaOAc.0 BaCl2. pH 8.0.2 Centrifuge Method KOAc.2 (revised) Uncorrected (extractable) Corrected (exchangeable) NH4OAc. Leaching Tube Direct Distillation NH4Cl. pH 8. pH 7.0 5D 5F 6 6A 5D1 625 Calcium-Saturation CHEMICAL ANALYSES Organic Carbon Acid-Dichromate Digestion FeSO4 Titration CO2 Evolution.0). Automatic Extractor Direct Distillation Steam Distillation I Steam Distillation II NH4Cl.2 KCl-TEA Extraction. pH 7. Gravimetric FeSO4 Titration.0. pH 7. pH 8.

Automatic Titrator Dry Combustion N2 Evolution Kjeldahl Digestion III Ammonia Steam Distillation 6B 6B1 6B1a 6B1b 6B2 6B2a 6B3 6B3a 6B4 6B4a 6B5 6B5a Iron Dithionite Extraction Dichromate Titration EDTA Titration Dithionite-Citrate Extraction Orthophenanthroline Colorimetry Atomic Absorption I Atomic Absorption II Dithionite-Citrate-Bicarbonate Extraction Potassium Thiocyanate Colorimetry Pyrophosphate-Dithionite Extraction Sodium Pyrophosphate Extraction I Atomic Absorption Ammonium Oxalate Extraction Atomic Absorption HF Dissolution Atomic Absorption HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry Sodium Pyrophosphate Extraction II Atomic Absorption Ammonium Oxalate Extraction Inductively Coupled Plasma Spectrometry I Inductively Coupled Plasma Spectrometry II xix 6C 6C1 6C1a 6C1b 6C2 6C2a 6C2b 6C2c 6C3 6C3a 6C4 6C5 6C5a 6C6 6C6a 6C7 6C7a 6C7b 6C8 6C8a 6C9 6C9a 6C9b . Automatic Titrator Semimicro Kjeldahl Ammonia Distillation Kjeldahl Digestion II Ammonia Steam Distillation.CONTENTS METHOD TITLE Dry Combustion CO2 Evolution I CO2 Evolution II CO2 Evolution III CO2 Evolution IV CO2 Evolution V Peroxide Digestion Weight Loss Sodium Pyrophosphate Extraction II Atomic Absorption METHOD CODE 6A2 6A2a 6A2b 6A2c 6A2d 6A2e 6A3 6A3a 6A4 6A4a PAGE 628 629 630 567 473 631 631 631 631 631 631 632 633 633 569 569 475 475 477 477 634 634 635 636 479 483 637 637 638 638 639 639 639 572 487 490 490 575 495 Nitrogen Kjeldahl Digestion I Ammonia Distillation Ammonia Distillation.

30 min. Overnight Aluminon I NH4OAc Extraction Aluminon III 6F 645 Aluminum 6G1 6G1a 6G1b 6G1c 6G1d 6G1e 6G2 6G2a 6G3 6G3a 6G 647 648 649 649 649 650 650 650 650 650 xx .CONTENTS METHOD TITLE Manganese METHOD CODE 6D 6D1 6D1a 6D2 6D2a 6D2b 6D3 6D3 6D3b 6D3c 6D4 6D4a 6D5 6D5b 6D6 6D6a PAGE Dithionite Extraction Permanganate Extraction Dithionite-Citrate Extraction Atomic Absorption I Atomic Absorption II 1 N KCl Extractable. Automatic Extractor Inductively Coupled Plasma Spectrometry I Inductively Coupled Plasma Spectrometry II Atomic Absorption II Sodium Pyrophosphate Extraction II Atomic Absorption Ammonium Oxalate Extraction Inductively Coupled Plasma Spectrometry HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry HCl Treatment Gas Volumetric Manometric Weight Loss Weight Gain Titrimetric Warburg Method Sensitive Qualitative Method Visual. Aluminon I Aluminon II Aluminon III Fluoride Titration Atomic Absorption KCl Extraction II. Gas Bubbles H2SO4 Treatment Gravimetric Weight Gain 640 640 479 479 483 580 500 504 490 490 495 495 487 487 Calcium Carbonate 6E 6E1 6E1a 6E1b 6E1c 6E1d 6E1e 6E1f 6E2 6E2a 6E3 6E3a 6F1 6F1b 6F1c 6F2 6F5 641 641 641 641 641 643 643 643 644 644 644 644 645 645 645 646 647 Gypsum Water Extract Indirect Estimate Ion Chromatograph Weight Loss Gypsum Requirement KCl Extraction I.

CONTENTS METHOD TITLE NaOAc Extraction Aluminon III Sodium Pyrophosphate Extraction I Atomic Absorption Ammonium Oxalate Extraction Atomic Absorption Dithionite-Citrate Extraction Atomic Absorption I Atomic Absorption II NH4Cl. Automatic Extractor Atomic Absorption 1 N KCl Extractable. Automatic Extractor Atomic Absorption I Inductively Coupled Plasma Spectrometry I Inductively Coupled Plasma Spectrometery II Atomic Absorption II Sodium Pyrophosphate Extraction II Atomic Absorption HF Dissolution Atomic Absorption HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry Ammonium Oxalate Extraction Inductively Coupled Plasma Spectrometry I Inductively Coupled Plasma Spectrometry II METHOD CODE 6G4 6G4a 6G5 6G5a 6G6 6G6a 6G7 6G7a 6G7b 6G8 6G8a 6G9 6G9a 6G9b 6G9c 6G9d 6G10 6G10a 6G11 6G11a 6G11b 6G12 6G12a 6G12b PAGE 650 650 650 651 651 651 479 479 483 651 651 584 580 500 504 490 490 572 487 575 495 Extractable Acidity BaCl2-Triethanolamine I Back-Titration with HCl BaCl2-Triethanolamine II Back-Titration with HCl KCl-Triethanolamine II Back-Titration with NaOH BaCl2-Triethanolamine III Back-Titration with HCl Automatic Extractor Saturation Extraction Acid Titration Saturation Extraction Acid Titration 6H 6H1 6H1a 6H2 6H2a 6H3 6H3a 6H4 6H4a 652 652 652 653 653 653 653 654 654 Carbonate 6I 6I1 6I1a 655 655 655 Bicarbonate 6J 6J1 6J1a 655 655 655 xxi .

CONTENTS METHOD TITLE Chloride METHOD CODE 6K1 6K1a 6K1b 6K1c 6K1d PAGE Saturation Extraction Mohr Titration Potentiometric Titration Anion Chromatograph Anion Chromatograph. Ionic Suppressor 6K 656 657 588 508 Sulfate Saturation Extraction Gravimetric. Ionic Suppressor 6L 6L1 6L1a 6L1b 6L1c 6L1d 6L2 6L2a 657 658 588 508 659 659 Nitrate 6M 6M1 6M1a 6M1b 6M1c 6M1d 659 660 588 508 Calcium Saturation Extraction EDTA Titration Atomic Absorption I Atomic Absorption II NH4OAc Extraction EDTA-Alcohol Separation Oxalate-Permanganate I Oxalate-Permanganate II Oxalate-Cerate Atomic Absorption I Atomic Absorption II NH4Cl-EtOH Extraction EDTA Titration KCl-TEA Titration Oxalate-Permanganate EDTA Titration Atomic Absorption HF Dissolution Atomic Absorption HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry 6N 6N1 6N1a 6N1b 6N1c 6N2 6N2a 6N2b 6N2c 6N2d 6N2e 6N2f 6N3 6N3a 660 514 517 661 662 663 663 521 524 664 666 666 666 666 667 667 667 487 6N4 6N4a 6N4b 6N4c 6N5 6N5a 6N5b xxii . BaSO4 Precipitation Saturation Extraction Phenyldisulfonic (PDS) Acid Colorimetry Diphenylamine Anion Chromatograph Anion Chromatograph. Ionic Suppressor NH4OAc Extraction Gravimetric. BaSO4 EDTA Titration Anion Chromatograph Anion Chromatograph.

CONTENTS METHOD TITLE Magnesium METHOD CODE 6O1 6O1a 6O1b 6O1c 6O2 6O2a 6O2b 6O2c 6O2d 6O2e 6O3 6O3a 6O4 6O4a 6O4b 6O4c 6O5 6O5a 6O5b PAGE Saturation Extraction EDTA Titration Atomic Absorption I Atomic Absorption II NH4OAc Extraction EDTA-Alcohol Separation Phosphate Titration Gravimetric Atomic Absorption I Atomic Absorption II NH4Cl-EtOH Extraction EDTA Titration KCl-TEA Extraction Phosphate Titration EDTA Titration Atomic Absorption HF Dissolution Atomic Absorption HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry Saturation Extraction Flame Photometry Atomic Absorption I Atomic Absorption II NH4OAc Extraction Flame Photometry Atomic Absorption I Atomic Absorption II HF Dissolution Atomic Absorption HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry Saturation Extraction Flame Photometry Atomic Absorption I Atomic Absorption II NH4OAc Extraction Flame Photometry Atomic Absorption I Atomic Absorption II HF Dissolution Atomic Absorption HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry xxiii 6O 667 514 517 668 669 670 521 524 671 671 671 671 671 672 672 487 Sodium 6P 6P1 6P1a 6P1b 6P1c 6P2 6P2a 6P2b 6P2c 6P3 6P3a 6P3b 6Q1 6Q1a 6Q1b 6Q1c 6Q2 6Q2a 6Q2b 6Q2c 6Q3 6Q3a 6Q3b 672 514 517 673 521 524 673 487 Potassium 6Q 674 514 517 674 521 524 572 487 .

Ionic Suppressor HF Dissolution Atomic Absorption HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry Ammonium Oxalate Extraction Inductively Coupled Plasma Spectrometry I Inductively Coupled Plasma Spectrometry II Saturation Extraction Anion Chromatograph Anion Chromatograph. pH 8.5 Methylene Blue Colorimetry HCl Release (sulfide) Iodine Titration SO2 Evolution KIO3 Infrared I Infrared II Perchloric Acid Digestion Molybdovanadophosphoric Acid Colorimetry Adsorption Coefficient Bray P-1 Absorbed Phosphorus Spectrophotometer New Zealand P Retention Spectrophotometer I Spectrophotometer II Citric Acid Extractable Spectrophotometer HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry Saturation Extract Carmine Colorimetry Saturation Extraction Anion Chromatograph Anion Chromatograph.CONTENTS METHOD TITLE Sulfur METHOD CODE 6R 6R1 6R1a 6R2 6R2a 6R3 6R3a 6R3b 6R3c PAGE NaHCO3 Extract. Ionic Suppressor 675 675 675 675 676 594 528 677 677 678 530 530 596 534 536 536 487 487 Phosphorus 6S 6S1 6S1a 6S2 6S3 6S3 6S4 6S4 6S4b 6S5 6S5 6S6 6S6a 6T1 6T1a Boron 6T 681 681 681 Fluoride 6U 6U1 6U1a 6U1b 588 508 Silicon 6V 6V1 6V1a 6V1b 6V2 6V2a 6V2b 681 487 575 495 Nitrite 6W 6W1 6W1a 6W1b 588 508 xxiv .

CONTENTS METHOD TITLE MINERALOGY Instrumental Analyses Preparation Carbonate Removal Organic-Matter Removal Iron Removal Disaggregation and Particle-Size Fractionation Particle-Size Distribution Analysis Pretreatment X-Ray Diffraction Thin Film on Glass Solution Pretreatment Resin Pretreatment I NaPO3 Pretreatment I Thin Film on Tile Solution Pretreatent Resin Pretreatment Sodium Metaphosphate Pretreatment Powder Mount Diffractometer Recording Camera Recording Thin Film on Glass Resin Pretreatment II NaPO3 Pretreatment Powder Mounts Differential Thermal Analysis DTA I Thermal Gravimetric Analysis TGA I TGA II Infrared Analyses Differential Scanning Calorimetry DSC I METHOD CODE 7 7A 7A1 7A1a 7A1b 7A1c 7A1d 7A1e 7A2 7A2a 7A2b 7A2c 7A2d 7A2e 7A2f 7A2g 7A2h 7A2i 7A2j 7A2k 7A3 7A3 7A4 7A4a 7A4b 7A5 7A6 7A6 PAGE 682 682 682 682 683 683 684 685 685 685 685 685 686 686 540 686 686 687 687 688 598 688 602 602 Optical Analysis Grain Studies Grain Mounts. Canada Balsam Electron Microscopy Na2CO3 Fusion X-Ray Emission Spectrography HF Dissolution HF + HNO3 + HCl Dissolution 7B 7B1b 7B2 689 689 689 689 689 606 550 690 555 Total Analysis 7C 7C1 7C2 7C3 7C4a 7D1 7D2 Surface Area Glycerol Retention EGME Retention xxv 7D .

Quick Test Saturated Paste. Mixed Saturation Extract Conductivity Conductivity. Conductivity Saturation Extract Conductivity Soil Suspensions Water Dilution KCl CaCl2 METHOD CODE 8 8A 8A1 8A1a 8A1b 8A2 PAGE 690 690 690 691 692 Saturated Paste. Capillary Rise 8B 8B1 8B1a 692 692 693 Reaction (pH) 8C 8C1 8C1a 8C1c 8C1e 8D2 8D3 8D4 8D5 693 693 693 693 693 Ratios and Estimates To Noncarbonate Clay Ca to Mg (Extractable) Estimated Clay Percentage Estimated Total Salt Iron Plus Aluminum. Pyrophosphate Extractable to Dithionite Citrate Extractable Index of Accumulation 8D 557 557 557 557 557 558 558 8D6 8D7 Optical Density (Ammonium Oxalate Extract) Zircon HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry xxvi 8J 8K 8K1 8K1a 575 487 487 487 Copper 8L 8L1 8L1a 8Ml 8M1a 487 487 487 Zinc 8M 487 487 487 Arsenic 8N 8Nl 8N1a 8O1 8O1a 487 487 487 487 487 Titanium 8O 487 .CONTENTS METHOD TITLE MISCELLANEOUS Saturated Paste. Mixed Bureau of Soils Cup.

CONTENTS METHOD TITLE Selenium METHOD CODE 8P 8Pl487 8P1a 8Q1 8Q1a 8Rl 8R1a PAGE 487 487 HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry HF + HNO3 + HCl Dissolution Inductively Coupled Plasma Spectrometry Cadmium 8Q 487 487 487 Lead 8R 487 487 487 xxvii .

A complete description of the sampling site not only provides a context for the various soil properties determined but it is also a useful tool in the evaluation and interpretation of the soil analytical results (Patterson. and sampling and sub-sampling procedures to be followed. 1993). and many types of samples. Coordination of mapping. In the laboratory. The soils mapped by the NCSS are identified by names that serve as references to a national system of soil taxonomy (Soil Survey Staff. The plan needs to address the site selection. and present information about the universe of concern.e. wherein general knowledge of similar materials. The objectives of a project or study form the basis for designing the sampling strategy. the SSL has more routinely used intuitive sampling plans to obtain representative samples. Both field and laboratory data are used to design map units and provide supporting information for scientific documentation and predictions of soil behavior. pedon.. landscape..SAMPLE COLLECTION AND PREPARATION (1) Field Sample Collection and Preparation (1A) Site Selection (1A1) Geomorphology (1A1a) Pedon (1A1b) Water (1A1c) Biological (1A1d) 1. and pedon documentation of the sampling site serves as a link in a continuum of analytical data. ranging from knowledge to guesses. systematic. sampled horizon. 1993). representative. Landscape. descriptions of site and soil pedon. and composite. e.g. e. landform. and careful sample collection. 1984. Application General: The United States National Cooperative Soil Survey (NCSS) Program has prepared soil maps for much of the country. In the field. Forest Service. Concerted effort is made to keep analytical variability small. The Soil Survey Laboratory (SSL) primarily serves the NCSS. 1988). A representative sample is one that is considered to be typical of the universe of concern and whose composition can be used to characterize the universe with respect to the parameter measured (Taylor. 1999). intuitive and statistical. The intuitive sampling plan is one based on the judgment of the sampler. random. 1996). Soil Survey Staff. which is conducted jointly by USDA Natural Resources Conservation Service (NRCS). and its history (Soil Survey Division Staff.. are used (Taylor. its environment. and overall soil survey area. Requisites to successful laboratory analysis of soils occur long before the sample is analyzed (Soil Conservation Service. Precise laboratory work means that the principal variability in characterization data resides in sample variability. the primary objectives of sample collection and preparation are to homogenize and obtain a representative soil sample to be used in chemical. 1996). past experience. This continuum is illustrated on the cover of this manual. and representatives of U.g. A soil map delineates areas occupied by different kinds of soil. A carefully designed sampling plan is required to provide reliable samples for the purpose of sampling. In the field. the Bureau of Land Management (BLM). 1988). each of which has a unique set of interrelated properties characteristic of the material from which it is formed. Universities and Agricultural Experiment Stations. There are various kinds of sampling plans. The analyst and the reviewer of data assume that the sample is representative of the soil horizon being characterized. depth of sampling. the primary objective of SSL sampling programs has been to select sites and pedons that are representative of a soil series and to collect samples that are representative of horizons within the pedon. sampling is the precision-limiting 1 . sampling site selection. these requisites include site selection. details of collection. i. type and number of samples. and sample collection in this program contributes to the quality assurance process for laboratory characterization (Burt. and mineralogical analyses (method 1B).S. In this context. physical.

sediment bodies. description. 2003b). and geomorphic processes. Wyosocki and Philip J. Pedon descriptions and classifications along with measured lab data. Hunt. 1970. Soils occurrence can be accurately predicted and mapped using observable landscape features (e. 1938. The first function listed above involves planned. 2. Gile et al. soil geomorphology serves several key functions in Soil Survey. Such studies quantify and explain the links between soil patterns and stratigraphy. NE. Soils can not be fully understood or studied using a single observation scale. slope inflections. A number of earth science sources (Fenneman 1931. Schoeneberger. Further. 2003a. Provides a conceptual basis for understanding and reliably predicting soil occurrence at the landscape scale.. soil scientists extend knowledge from point observations and descriptions to larger land areas. NRCS. Soil survey updates by MLRA can and should involve similar studies.variable. Parsons et al. Columbia Plateau. which are an important component of the Soil Survey.) identify and name geomorphic regions. Thus. Piedmont. Lincoln. vegetation. and Atlantic Coastal Plain provide both a geologic and geographic context for communicating regional soil and landform knowledge. landforms. 1957. Ruhe et al. Douglas A. complex continuum across the Earth’s landscape.. bedrock outcrops. 1965. but justified by the quantitative information and scientific understanding acquired. 1967. 4. 2001. Geomorphic functions are best explained by citing examples. The prime goal of the Soil Survey is to segregate the soil continuum into individual areas that have similar properties. Soil map-unit delineations are the individual landscape areas defined during and depicted in a soil survey. parent materials. parent materials. Research Soil Scientists. Provides a scientific basis for quantitatively understanding soil landscape relationships. accurately apply to a named soil map unit or landscape areas (soil component) within the map unit. however. 1970. Gamble et al. and classification occur at the pedon scale (1 to ≈ 7 m). Studies of this nature provide the most rigorous. 1970. As a result. During a Soil Survey soil scientists achieve these functions both tacitly and by deliberate effort. surface age. and represent a small portion of any map unit (10’s to 1000’s hectares). and hydrology. Terms such as Basin and Range. 3. Soil observation. landforms. Provides a geologic and geographic context or framework that explains regional soil patterns. stratigraphy. pedons selected. Instead.. which can be summarized as: 1. similar use and management. 1946. To accomplish the task of Soil Survey at reasonable cost and time. described. landforms. and complete information about soil patterns and landscapes. The three remaining geomorphic functions are tacit and to a degree inherent in a soil survey. Soil scientists can reliably project (“scale up”) pedon information to soil map units based on experience and the strong linkages among soils. Warhaftig. Communicates effectively and succinctly soil location within a landscape. The value of relating soil patterns to these regions is self-evident. wrote the geomorphic component of this procedure..g. quantitative. parent material. and sampled for laboratory analysis represent only a small subset of the observation points. soil scientists use multiple scales to study and segregate soils and to transfer knowledge to soil users. Geomorphic Considerations1: Soils form a vital. site-selection and sample collection and preparation are critical to successful soil analysis.. Lee et al. detailed soil landscape studies (e. which are grouped by geologic and landform similarity. NSSC. 1 2 . landscape position. 1981. The required time and effort are significant. and therefore.g. and site history. Daniels et al.

or pedon sampling must also consider and address the geomorphology. Recent publications (Soil Survey Staff. In another geomorphic setting soil distribution and hydrology may be controlled by stratigraphic relationships rather than by elevation or landscape patterns.g. backslope etc. multiple samples across the same hillslope). Such studies are applicable and necessary to the Major Land Resource Area (MLRA) soil survey approach. Water. i. and drainage pattern. slope shape and gradient. Keep in mind that the sampled pedon represents both a taxonomic unit and landscape unit. A well-designed geomorphic study can test this hypothesis.. Crucial problems can be addressed by appropriately designed geomorphic. The existence of other soils or taxa can and should be included in the soil description and also the map unit description. soil horizon. 1999) as a unit of sampling within a soil. and Soil Biology Sampling: The pedon is presented in soil taxonomy (Soil Survey Staff. Among these are landform type. soil geomorphic relationships deserve and sometimes demand specific study during a soil survey. Wysocki et al. stream terrace. Soil patterns on landscapes follow catenary relationships. Map unit design includes landform recognition and naming. Both the landscape and taxonomic unit should be considered in site selection... Every sample pedon should include both a complete soil and geomorphic description. which should convey soil property.g. stream terrace. In turn a clear. Moreover. it provides an understanding of the entire soil landscape. For characterization project select the dominant taxonomic unit within a given landscape unit. 2002. 3 . and landscape and soil hydrology.g. Wysocki et al.. but serves multiple purposes. parent materials. The unit could be a landform (e.stratigraphy. a hillslope position (e. This appears intensive.. laboratory resources. It is important to characterize both individual pedon properties and the soil relationships both above and below on the landscape. a geomorphic component (e. a silty or sandy mantle over adjacent soils and/or landforms may be of eolian origin. Note that a single landscape unit (e. footslope). the smallest body of one kind of soil large enough to represent the nature and arrangement of horizons and variability in the other properties that are preserved in samples (Soil Survey Division Staff. and observations on landscape position. This tacit soil landscape knowledge model is partially encapsulated in block diagrams and map unit and pedon descriptions. For example. 2000) provide a comprehensive and consistent system for describing geomorphic and landscape attributes for soil survey. Study or sampling objectives can vary. A landscape unit is a more easily field recognizable and mappable feature than a soil taxonomic unit.g. 2000.. This is an efficient use of both sampling time and effort.) it occurs upon. or sometimes compel and create new models. landscape position. 1998. Preliminary or initial soil pattern knowledge is commonly based on landscape or geomorphic relationships. and perhaps most importantly.. stratigraphic. site selection. as well as. These studies need not be elaborate.g. and parent material properties. Schoeneberger et al. parent material distribution. nose slope). 1993). or parent material study.S. Pedon. or all of these. 1998. Observations during a soil survey refine existing landscape models.. A drill core or backhoe pit sequence can address this hypothesis. 2002 for more detailed information. Note that the landscape unit that is sampled can be multi-scale. photo tonal patterns).e. Geomorphology is an integral part of all soil survey processes and stages. The Geomorphic Description Systems (GDS) is not discussed here. During a soil survey soil scientists develop a tacit knowledge of soil occurrence generally based on landscape relationships..e. Lastly. backslope) may contain one or more taxonomic units. or drumlin). Refer to Soil Survey Staff.. Soil occurrence is consistently linked to a number of geomorphic attributes. drainage. Any study plan. landscape and geomorphic relationships. concise geomorphic description effectively conveys soil location within a landscape to other soil scientists and soil users. Soil scientists capture this observational and expert knowledge through soil map unit and pedon descriptions. but they require fore thought and planning. A sample pedon or set of pedons provides vital characterization data and also can quantify the catenary pattern and processes. In the U. In a characterization project. This goal requires that soils be sampled as a catenary sequence (i. dune. the sample pedons should be representative of the landscape unit (e. and Schoeneberger et al.

A representative sample is collected using the boundaries of the horizon to define the vertical limits and the observed short-range variability to define the lateral limits. impact analysis for erosion effects. Histosols. 1995).. to estimate saturated hydraulic conductivity. Pankhurst et al. weighed. skeleton grains. either in conjunction with pedon sampling or independently. As with pedon sampling. color. The USDA NRCS has utilized soil biology and carbon data in macro-nutrient cycling. and designating and sampling a sub-horizon if root mass and morphology change. In the laboratory. Pankhurst et al.. to determine the coefficient of linear extensibility (COLE). The same bulk sample collected for soil mineralogical. For example. These descriptions include observations of specific soil properties such as texture. Descriptions may also include inferences of soil quality (soil erodibility and productivity) as well as soil-forming factors (climate. Biological samples are also be collected for analysis at the laboratory.soil Survey Program. conservation management practices.g. These projects are typically in conjunction with soil investigations and have involved monitoring seasonal nutrient flux to evaluate movement of N and P via subsurface and overland flow from agricultural lands into waterways and wetlands. and to investigate genesis of soil or pedological features. the <20-mm fraction is sieved and weighed..to 75-mm fraction is generally sieved. 2). and discarded. laboratory pedon data combined with field data (e. 3) but before the vertical section by the sampling process (Fig. pedon. sampling by horizon. transects and pedon descriptions) are used to define map unit components. either in conjunction with pedon sampling or independently. Bulk density clods are used for water retention data. establish or modify property ranges for soil series. soil quality determinations. weathering intensity. Summary of Method A site is selected that meets the objectives of the laboratory sampling. Microscope slides of soil prepared for micromorphology are used to identify fabric types. In the field. and soil horizon for the sample. 1994. Biological samples are also collected for analysis at the SSL. global climate change predictions.. resource assessments. The tag on the sample bag is labeled to identify the site. Measurable biological indices have been considered as a component to assess soil quality (Gregorich et al. Undisturbed clods are collected for bulk density and micromorphological analysis. 1994). 1). Vertisols. Clods are obtained in the same part of the pit as the mixed. or permafrost-affected soils. The variable nature or special problems of the soil itself. A large number of soil biological properties have been evaluated for their potential use as indicators of soil quality/health (Doran and Parkin. and chemical analyses during pedon sampling can also be used 4 . Photographs are typically taken of soil profile after the layers have been identified (Fig. A soil pit is often excavated with a back-hoe (Fig. long-term soil fertility assessments. may require the use of specific excavation and sampling techniques. 1997.g. The SSL estimates weight percentages of the >2-mm fractions from volume estimates of the >20-mm fractions and weight determinations of the <20-mm fractions by method 3A2. representative sample. the 20. sampling for root biomass includes selecting a representative site. Representative samples are collected and mixed for chemical. 2. physical. 4). e.. illuviation of argillans. establish ranges of component properties. 2001). topography. and carbon sequestration (Franks et al.. and to identify compacted horizons.. to convert from a weight to volume basis. and answer taxonomic and interpretive questions (Wilson et al. and geologic material). Depth and breadth of pit depend on the soil material and objectives of sampling. slope. vegetation. and mineralogical analyses. physical. Soil horizons or zones of uniform morphological characteristics are identified for sampling (Fig. 1997). the shear failure that forms slickensides in Vertisols also disrupts the soil to the point that conventional soil horizons do not adequately describe the morphology. and depth. Water samples are analyzed by the SSL on a limited basis in the support of specific research projects. The site and soil pedon are described and georeferenced.

Fig.Fig. 2. 1. Soil horizons or zones of uniform morphological characteristics are identified for sampling. 5 . Excavated pit for pedon sampling.

4. Fig. Pedon sampling activities.Fig. Photographs are typically taken of soil profile after the layers have been identified but before the vertical section by the sampling process. 3. 6 .

. Gloves (powderless) may be used. as the details of collection can vary with local conditions. and the frequency of sampling (Velthorst. High temperatures can also alter microbial populations and activity (Wollum.. a number of obstacles may arise from external sources. Sometimes pits have to be hand-excavated. phosphate. small sample volume has more contact with larger bottles compared to small bottles (Velthorst. 1994). and releasing aluminum and silica (Velhorst. i. 1993). insects.for some soil biological analyses. Sampling for trace element analysis requires the use of clean. 1972. aerobic samples will remain aerobic during transport to the laboratory (Wollum.g. as some soils irreversibly harden upon drying. resulting in a change in the concentration of some elements (e. Specific recommendations are not applicable. Surface litter and O horizons are sampled separately. 1996). as they are generally permeable to CO2 and O2. 1996). sorbing dissolved organic carbon. Water samples are affected by microbial activity. e.g. which can influence pH and the separation of dissolved organic matter from the water phase.. are requested. steep terrain. Nevertheless. and large rock fragments. 1975. plastic bags will suffice for most biological samples.. errors increase with the permeability of bottle wall. these samples require expedited transport under ice or gel packs and are refrigerated (4°C) immediately upon arrival at the laboratory.. desorption) as well as the bottle volume can affect the analytical results... Avoid long periods between collection and laboratory analysis of water and some types of biological (e. To prevent significant changes (e. and Nanzyo. as these cups have a small cation exchange capacity. Water samples can also be collected for laboratory analyses at the same time as pedon sampling. Water samples require expedited transport under ice or gel packs and are refrigerated (4°C) immediately upon arrival at the laboratory. If certain biological analyses. Preservation of sample integrity. volatilization. glass bottles release sodium and silicon with time. for the appropriate treatment of these cups before use. microbial biomass) and soil samples (e. polyethylene bottles increase the chlorine content with time or adsorb organic material. these samples require expedited transport under ice or gel packs and are refrigerated (4°C) immediately upon arrival at the laboratory to avoid changes in the microbial communities.. or sample water. e. and the loss of iron through precipitation or oxidation (Velthorst. Water sample containers should be acid washed and capped in the laboratory prior to collection in the field. microbial biomass. degradation. Espinoza et al. Ceramic cups for collection of soil water may require an acid pretreatment prior to installation in the field.e.g. e. Alternatively. In general.g. depth. nitrate. as with pedon sampling. Do not allow soils to dry. The SSL recommends double-bagging zip locked plastic bags to prevent loss of sample water content.. nonmetallic equipment. screw cap. The drying of these containers should also be considered with regards to interferences or contaminants. Interferences In the process of sampling. affecting some laboratory analyses such as particle size (Kubota. 1996).e. and ammonium). the primary objective of water sampling is the same as with soil and biological sampling. Choice of water sampling site depends not only on the purpose of the investigation but also on local conditions.g. Avoid contamination of water samples by not touching the inner part of the sample container.. the reduction of sulfate to sulfide and chlorine to chloride. 1996). i.. Extreme care and precision are required for samples with low natural elemental concentrations. Refer to the respective manufacturer’s manual.g. sulfidic materials). The kind of water sample container (adsorption. 7 .g. accessibility. e. Soil Moisture Corporation. alteration in microbial community). to obtain a representative sample in laboratory analyses. preventing sample drying. a separate bio-bulk sample can be collected in the field. 3. The addition of microbial inhibitors may be necessary. Common sense and the guidelines for obtaining representative samples are applied to the extent possible. wet terrain.g. Avoid freezing water samples. 1994). weather. avoiding changes or contamination during sampling and transport is important.

for bulk density and thin section clods 5.26 Garden clippers 5.3 Dow Saran F-310 Resin. drill rig.6 Shipping bags (canvas. plastic. leather.24 Camera 5. 5.22 Plastic sheets 5. backhoe.13 Felt markers.14 Sampling pans 5. Take precautions when operating or in the proximity of machinery. for biological samples 5.17 Rock hammer 5.g. Equipment 5.29 Scale.12 Clothes pins 5. ± 0. for bagged samples 5.4. e. 8 . with screw caps.34 Bulk density equipment. for biological samples 5. cardboard with dividers 5.3 Tags. e. Department of Labor Occupational Safety and Health Administration (OSHA) standards. Available from Dow Chemical Company. with ice or gel packs. with staples 5. Safety Sampling pits deeper than 125 cm (5 feet) need to be shored to meet U.2 Water. bulk density frame or ring excavations. permanent 5. compliant cavity (procedure 3B5.19 Measuring tape 5. or one side has to be opened and sloped upward to prevent entrapment. and when lifting sample bags.11 Rope 5.25 Frame.23 Canvas tarp 5. powderless 5..5 Aluminum case.21 Sieves (3-inch and 20-mm) 5. 100-lb capacity. to transport cores from drill rig or hydraulic probe 5.27 Pruning shears 5.01 g sensitivity. Reagents 6.28 Bucket 5. for weighing roots and plant residue 5.9 Stapler.30 Analytical balance. or burlap) for mixed samples 5. in spray bottle 6. 3B3.8 Core boxes.32 Containers. 50 cm x 50 cm 5. if natural clods are not appropriate technique. acid-washed. for rock fragments 5. for mixed soil samples 5.20 Photo tape 5. Acetone used in the saran mix is flammable and should be used down wind from a site to keep fumes from collecting in the bottom of the pit.16 Chisel 5.1 Acetone 6.15 Sampling knives 5. for water samples 5.4 Plastic bags.1 Plastic bags.10 Hair nets 5. 3B4.31 Cooler.g. respectively) 6.. or hydraulic probe.2 Zip locked plastic freezer bags.18 Nails 5.33 Gloves. for shipping clod boxes 5.S.7 Clod boxes.

The sampling procedure is the same for hand-dug and backhoe pits.. The sampling may be extended deeper by bucket auger or hydraulic probe as appropriate to meet the objectives of the project. samples may be collected as standards for the survey project for texture. or to a maximum depth of 2 meters. Often. horizon (zone). Also.g. their morphological properties. and depth (as a minimum). Samples are typically collected from specific horizons in 3 to 5 locations that relate to the question or are representative of the map unit. a specific project may be designed to study the relationships between a catena of soils. Another study may be designed to determine the lateral extent of stratigraphic breaks. Geomorphology and Stratigraphy Projects: These projects are designed to study relationships between soils. A limited number of analyses. A standard suite of laboratory analyses are performed on each horizon.7. Mark horizons or zones to be sampled. and the hydrology of the area. Collect 3 bulk density clods from each horizon. Two clods are used in the primary analysis. In addition. specific analyses. and place a representative sub-sample. redoximorphic features. the soil and coarse fragments need to be sieved and weighed as described below. Sampling and analytical requests may be similar to the scheme used in a characterization or reference project. may be requested to provide more complete information on the specific pedon sampled. Pedons are generally excavated through the solum and into the parent material. provide data for transect of a mapping unit. Hand-digging may be necessary depending on site location. are performed on these samples. if needed. e. in a plastic sample bag. Example sampling schemes presented as general project categories based on project needs are as follows: Reference Projects: These projects are designed to answer specific questions on mapping or soil classification. and/or the stratigraphy of their parent materials. If the soil has rock fragments in one or more horizons. the best procedure is to place 4 to 5 kg soil on the plastic sheet or canvas tarp. When using a backhoe. shoring is required to meet OSHA standards if the pit is deeper than 125 cm (5 ft). Slope the pit upward toward the backhoe for an escape route. Characterization Projects: These projects are designed to obtain comprehensive soil characterization data for a representative pedon of a map unit or a pedon which is included in a research study. minimum of 3 kg (3 qt). core samples may be collected to several meters in depth through the use of a hydraulic probe. Label a tag with soil name. type of soil material. soil survey number. dig the pit in the form of an arc with a minimum working face deeper than about 150 cm (5 ft). If a transect is used to test map unit composition. Clods should be roughly fist-sized 9 . specific to the questions asked. Pedon Sampling Techniques Excavated Pits: A pit may be excavated by hand or with a backhoe. Double fold the top of the plastic bag (forward and reverse) and staple the top of the tag under the folds. as well as clods of natural fabric for bulk density and micromorphology. an appropriate sample from each transect point may be collected for analyses that are critical to distinguishing between map unit components. landforms. or for collection of calibration standards. Unless the soil exhibits little short range variability. If this is not practical. The pit can also be modified from the back side to form a T with the back of the trench opened and widened for an escape route. Take a representative sample from boundary to boundary of a horizon and for a lateral extent to include the observed short-range variability. such as mineralogy or andic properties. The third clod is reserved for a rerun. Procedures Project and Sampling Objectives The number and types of samples collected from a site are governed in part by the objectives of the information needed. Site or pedon selection is governed by the objectives of the study but often is selected to represent typical segments of the landform. or availability of a backhoe. mix thoroughly by rolling action. organic carbon. For example. Samples collected from each horizon include bulk samples of approximately 3 kg. or for calibration of field office analyses such as base saturation.

Label the top of the box to identify type of sample (bulk density or thin section) and appropriate soil survey numbers and horizons (zones) for the samples. Smooth a planar area in the pit face. Place in a plastic bag 10 . Clods can be dipped and then hung. Fill empty cells with a wadded paper. and put into a cell of a clod box. Mark horizon breaks on the plastic. smooth off the sample flush with the top of the can. Clods should be roughly fist size. Tape down the top of a filled clod box with nylon filament tape (one short piece on each end and two short pieces in front). describe and then sample. and depth for the core. If the clod is dry. Hand Probe: Remove surface if it is not suitable for coring. Therefore. the clod can be placed in a hairnet and dipped briefly in saran as described above.and should fit into the cell (8 x 6 x 6 cm) of a clod box fairly snugly. in saran mix to coat the clod. Hydraulic probe: Remove surface if it is not suitable for coring. In either case. Single clod boxes also ship well. one density is representative for all water contents of coarsetextured soils. With a sharp knife trim the exterior to remove any oil and contaminating soil material. but kept unmodified otherwise. or can be hung and then dipped by raising the container up to immerse the clod. It is assumed that there is no volume change with water content in sandy soils. Place sample in a plastic bag and label with soil survey number. This prevents clods from shifting in transit. If the material is too sandy and/or too dry to hold together in a clod. and hang from a rope with a clothes pin to dry. In this case. Place a staple in the top of each clod for orientation. Keep the saran container covered except when dipping clods to prevent acetone evaporation. Additional coats are applied in the laboratory. Remove core sections and lay in order on plastic sheet. Dip once. Place the clod in a hair net. With the palm of the hand. Place six clod boxes in an aluminum case for shipment. If the soil fabric is fragile. with a knife blade. and are generally suitable for a limited number of analyses only. Take the clods in the same vicinity of the pit as the mixed sample. Break the block into fist-sized pieces and pare into a ovoid (eggshaped) clod. Mix the horizon or zone to be sampled. Collect 2 clods from each horizon for preparation of thin sections and micromorphological examination. The sampler should make special note of any features to be studied by thin section. Measure core length against depth in hole to determine if the core has been compressed. When the clod is dry (bottom is not sticky to the touch). mist the clod with water just until the surface glistens to inhibit saran penetration of the clod. Clod boxes are designed to identify sequences of 3 clods per horizon. Samples need to be a minimum of 500 g (1 pt). or. lay a board across the bottom of the can and tap lightly with a hammer or geology pick until the bottom of the can is flush with the pit wall. Mark horizon breaks on the plastic. Label the appropriate cell on the inside of the lid of the box to identify the soil survey number and horizon (zone) for the sample. Collect two samples per horizon. Mix the horizon or zone to be sampled. smooth a planar horizontal area. Sampling is easier if the can has a small hole in the bottom to allow air to escape as the can is inserted. tie the top of the bag in a single knot and put into a cell in a clod box. Then dig out the sampling can plus extra sample and. Label the appropriate cell on the inside of the lid of the box to identify the soil survey number and horizon (zone) for the clod. bulk density samples can be collected with an aluminum can or other small can of known volume. if sampling from the top down. Label the appropriate cell on the inside of the lid of the box to identify the soil survey number and horizon (zone) for the clod. Empty the contents of the can into a plastic bag. horizon (zone). Remove core sections and lay in order on plastic sheet. Indicate the volume of the sampling can in the sampling notes. Place the clod in a plastic bag and put into a cell of a clod box. place the clod in a plastic bag. Coat only once in the field. briefly. Avoid leaving empty cells in a clod box. gently push the can into the smoothed area until the bottom of the can is flush with the wall or until resistance stops you. Split one core open to mark horizons. choose an area that appears representative of the horizon. Measure core length against depth in hole to determine if the core has been compressed. Carve out a working section in the pit wall to remove an undisturbed block. briefly.

A core segment can be taken for thin section. If undisturbed blocks can be removed for bulk density. double fold the bag. and depth for the sample. and horizon. place the core in a plastic bag and put the bag into a cell in a clod box. and the core diameter is 3 inches or more. Mark a segment 8-cm long on an undisturbed section and slice a cylindrical segment. If the hydraulic conductivity is slow enough. and depth for the core. Place in a plastic bag and label with soil survey number. and horizon. If the samples appear undisturbed. tie the top in a knot. Sampling depth in a pit can be extended by the use of an auger in the pit bottom. Label the appropriate cell number on the inside of the box lid to identify the site. Core segments can be placed in a hair net. When horizon breaks are detected. placed in a plastic bag and then put into a cell of a clod box. Bucket Auger: Remove surface if it is not suitable for auguring. Place in a plastic bag and label with soil survey number. mark 10-cm segments. place excavated sample in a bucket of known weight (tare) and weigh. Place a minimum of 4 kg (1 gal) in a plastic bag. and depth for the core. dipped once briefly in saran mix to coat the clod. 5 cm on a side). horizon (zone). Place a staple in the top of the core. pedon. samples for bulk density can be taken from a second core. Put the double bagged sample in a clod box and label the appropriate cell on the inside of the lid to identify the soil survey number and horizon (zone) for the sample. hung from a rope with a clothes pin to dry. Place the core segment in a plastic bag and place bag into a bulk density (clod) box for shipment. Remove auger loads and lay in order on plastic sheet. horizon (zone). placed in a plastic bag and then put into a cell of a clod box. Note the sample dimensions in the sampling notes. Sieve the sample through both a 75-mm and 20-mm sieve (3/4 in) onto a canvas tarp which can be suspended from a scale. Obtain a minimum of 500 g (1 pt) for a reference sample or 3 kg (3 qt) for a characterization sample. carve out cubes of known dimension (e. dipped once.. Note the core diameter and length in the soil description. place the block in a plastic bag and tie the top in a knot. obtain samples of upper layers from a pit. Measurements of core diameter and length can be used to calculate volume and density at the field-state water content. Mix the horizon or zone to be sampled.g. If the 20 to 75-mm fraction is not weighed in the field. Mix the horizon or zone to be sampled. and place a single 11 . briefly in saran mix to coat the clod. Measurements of core diameter and length can be used to calculate volume and density at the field-state water content. Mark horizon breaks on the plastic.and label with soil survey number. hung from a rope with a clothes pin to dry. and staple. slice with a knife. measure depth in hole and mark it on the plastic. and record these values in the description or sampling notes. estimate the volume percent and record in the sampling notes or description. Core segments can be placed in a hair net. The water content is determined on the sample in the laboratory. Rotary drill (hollow stem): Remove drill core sections and lay in order on plastic sheet. If the core has not been compressed. dig and remove samples below the water table as far as practical with due haste and place on a plastic sheet in an orderly fashion for describing and processing. Obtain a minimum of 500 g (1 pt) for a reference sample or 3 kg (3 qt) for a characterization sample. Weigh the 20 to 75 mm and the <20 mm fractions in pounds or kilograms. Measure core length against depth in hole to determine if the core has been compressed. Weights are calculated to an oven-dry base in the laboratory. Label the appropriate cell number on the inside of the box lid to identify the site. Organic Soils: If the soils are drained or the natural water table is below the surface. Specific Pedon Sampling Techniques Soils with Rock Fragments: If coarse fragments up to 75 mm (3 in) in diameter are to be weighed in the field. and record these weights. Place in a second plastic bag if soil is saturated. Obtain a minimum of 500 g (1 pt) for a reference sample or 3 kg (3 qt) for a characterization sample. Estimate the coarse fragment volume percent of both the 75 to 250 mm (10 in) fraction and > 250-mm fraction. and the core diameter is 3 inches or more. horizon (zone). Collect samples from below the water table with a Macaulay peat sampler. pedon. samples for bulk density can be taken from the core. If the core has not been compressed. Mark a segment 8 cm long on an undisturbed section and slice a cylindrical segment.

A gilgai surface topography is reflected in the subsurface by bowl-shaped lows and highs.7 by 1. Frozen earth can be removed in successive steps with a gasoline-powered jackhammer. Save the large chunks. Test the depth to the frost table with a small (1 to 2 mm) diameter steel rod. and put in a clod box. As an alternative. Glass containers must be adequately packed for shipment to prevent breakage. Examine the surface and designate horizons. nitrogen gas can be bubbled through the sample for a few minutes to displace air. The sample shape is a halfcylinder. Note thickness of segregated ice lenses and make a visual estimate of relative volume of segregated ice. and tag. tie the top. Larger samples can be taken below the water table by removing the surface mat with a spade and sampling lower layers with a post-hole digger. Once in the lab. Take replicate samples for the mixed sample. Tie the top in a knot and place in a second plastic bag and tie the top of that bag in a knot. fold top. Excavate to a depth of 30 to 50 cm below the frost table. if it appears air remained in the container. Note on graph paper if necessary and photograph. From the bottom of the pit remove soil from the non-work face so it 12 . if practical. 1999) commonly occur in intra-tidal zones adjacent to oceans.3 m) to leave about 10 cm of unfrozen material over the permafrost. Vertisols: The shear failure that forms slickensides in Vertisols also disrupts the soil to the point that conventional horizons do not adequately describe the morphology. if possible. as necessary. the following procedure is suggested: Dig a trench long enough to cover two or three cycles of morphological expression. Sulfidic Soil Materials: These materials as defined by soil taxonomy (Soil Survey Staff. extend the pit through at least one cycle. The intent is to keep the material at the field pH prior to running the oxidized pH test. remove all unfrozen material to examine the conformation of the frost table. If a cyclic pattern (up to a few meters) is evident in the surface topography. Sample each horizon or zone for mixed sample. carve a block to fit snugly in a tared water can. Place lid on can. bulk density. then replace the lid. The following sampling approach is suggested. Keep containers in the dark and cool. In order to examine morphology and associated soil properties in more spatial detail. knead to remove air. Sulfidic soil samples require expedited transport in a cooler and are refrigerated (4 °C) immediately upon arrival at the laboratory. and thin section as is practical. Put two small bags of sample into one large plastic bag. Clean off the pit face and be ready to photograph immediately. depth in sampling notes along with the tare weight. Fill the container nearly full of sample and add ambient soil water so that all air is eliminated when the lid is secured. impose a grid over the pit face and sketch the morphology on graph paper. Place representative pieces into a water-tight container so that the sample can be weighed. When the description of the unfrozen material is complete. Place pieces from each step on a separate plastic sheet. In many cases the surface layers are organic materials. staple. The objective is to record the morphology of the unfrozen soil before the permafrost is disturbed. If the soil is disrupted to the extent that lateral horizons do not represent the morphology. and weighed again to calculate the amount of water and volume of ice. put can in a plastic bag. The organic layers can be carved out with a sharp knife or shovel in many cases and removed. Place samples of each layer on plastic for examination. One convention is to sample pedons out of the low and the high areas which represent extremes in the cyclic morphology. Mason jars and plastic containers with a positive sealing mechanism work well. dried. Examine pieces and describe the morphology as they are removed. Transfer samples to small plastic bags. Put the double bagged sample in a clod box and label the appropriate cell on the inside of the lid to identify the soil survey number and horizon (zone) for the sample. Describe the soil down to the frost table. Note the sampler diameter and length of core in sampling notes. and are saturated most or all of the time.segment in a plastic bag. Identify can number. Excavate a small pit (about 0. The permafrost is very resistant to excavation and the cryoturbation disrupts horizon morphology. Permafrost Affected Soils: Soils with permafrost present two special sampling problems. Use containers with an airtight cover.

surface litter and O horizons are sampled separately by cutting out a 50 x 50-cm area in a square to a measured depth for bulk density determinations. If certain biological analyses. place the loop over the spike.. The USDA-NRCS projects requiring collection of water samples have typically been in conjunction with special soil investigations. as the details of collection can vary with local conditions.water. Geological Survey field manual. Assign a number and a horizon designation to each cell. Place a line level on the string. and S. C. and chemical analyses during pedon sampling can also be used for some soil biological analyses. pull the string taut. Specific recommendations are not applicable. the plants should be identified either in the field or later using a plant identification key so as to determine which plants are associated with the soil microbial communities. Alternatively. Include replicate samples in the sampling plan. Properly label samples to show important information. Hammer a spike into the wall at one end of the pit. either in conjunction with pedon sampling or independently.. Transfer the morphology outlined by the string to graph paper by measuring the x-coordinate along the string and the y-coordinate above or below the string. e.. available online at http://pubs.. refer to the U. and run the string to the far end of the pit. Construct a level line about one meter below the highest point on the surface. e.g. These samples are weighed.S. 1996). separated by genus or species and by live and dead fractions. As with pedon sampling. sampling for root biomass includes selecting a representative site. i. soil. to obtain a representative sample for use in laboratory analyses. microbial biomass. depth.e. Sample each cell for characterization analysis as described above. Each plant fraction is weighed. The sampling area is approximately 1 m2. Tie a loop in string. Place a marker at each meter along the string from one end to the other.gov/. physical. either in conjunction with pedon sampling or independently. the primary purpose of which is to identify and/or quantify the variability in all or part of the sampling and analysis system. the primary objective of water sampling is the same as with soil sampling. these samples require expedited transport under ice or gel packs and are refrigerated (4°C) immediately upon arrival at the laboratory to avoid changes in the microbial communities. and the frequency of sampling (Velthorst. are requested. place a second spike through the loop. The amount and composition of water samples vary strongly with small changes in location.slopes up and away. and intermediate positions along the cycle. Refer to http://soils. All vegetation is clipped to the soil surface. e. dried. total N. particulate organic matter (POM). raise or lower the spike until the string is level.g.g.usgs. and designating and sampling a sub-horizon if root mass and morphology change. dried. Choice of water sampling site depends not only on the purpose of the investigation but also on local conditions. Detailed information about the elements of a water quality 13 .usda. Soil Biology Sampling Biological samples are also be collected for laboratory analysis. Other USDA-NRCS field procedures and sampling protocols for samples that do not require analysis at the SSL are not covered in this manual. The sampling scheme can include traditional pedon sequences by sampling vertical sequences of cells at low. The same bulk sample collected for soil mineralogical. high. Typically a 50 x 50-cm area is sampled. tie another loop in the string. For more detailed discussion of sampling protocols and investigations of water quality. Use a level or a plumb bob to make the y measurement vertical. depth. both in centimeters. As with pedon sampling. Water Sampling Water samples can also be collected for laboratory analyses. etc. Use nails and string to outline boundaries of morphological cells.gov for more detailed discussion of these topics. Typically the roots are separated by hand sieving at the laboratory. and re-weighed to determine root biomass. and hammer the spike into the pit face. sampling by horizon. Nevertheless. a separate bio-bulk sample can be collected in the field. and re-weighed to determine above-ground biomass. horizon. At the time of sampling for above-ground biomass.

Am. Fenneman. Sample collection procedures for laboratory analysis in the United States Soil Survey Program. equipment.R. and R. Gregorich and M. and T. 534 pp. J. and W. D. and B. D.000. sample filtration (0. 1970. p. Stewart (eds. Plant Anal.M.M. R.. Include blank samples in the sampling plan.G.M. etc. R. (1999) for more detailed descriptions of the purpose and processing procedures for blanks and replicate samples. electrical conductivity. (Reprinted 1957) Physical division of the Unites States. 1:7. Al. inner part of the container or screw cap. Stewart (eds. Soil Sci.g. root biomass. 8. 1946. (1 sheet). and T. The sample is then split into two sub-samples. Fe. C. CRC Press LLC. trip.. Soil Sci. N. 1997.g.C.E. Parkin.) Assessment methods for soil carbon. Refer to Wilde et al. Fenneman.B. Gloves (powderless) may be used. 34: 276-281. NY.monitoring and assessment program may be found at the U. Before water sampling in the field. Some water analyses. ambient. Gamble. NY. Coleman. and R. Geomorphic surfaces and soils in the Black Creek Valley. Am..F. Mn) and the other for anion analyses. Doran.. Avoid touching the sample water.B.. microbial biomass. Kimble. with one acidified to pH 2 for cation analyses (e.H. as optimal preservation is not possible (Velthorst.D.. J. Upon completion of these analyses. and split. N.E. and B. Doran. Proc.epa. J.B. Adams. C. p. 39.R. need to be performed promptly.F. Kimble. New York. R. Nettleton. Carter (eds. Elsevier. R. and L. R.S. McGraw-Hill Co. Jr. Commun.34: 648-653.. R. Cady. Madison. Espinoza.. Environmental Protection Agency’s website http://www.D. Soc.B. 14 . 27:1293-1298. p. 81-113. Some relationships among Coastal Plains soils and geomorphic surfaces in North Carolina. Gamble.g. Grossman. Lal.g.G.M. Resour.105-113. Soil. e. J. depth. M. Bezdicek. time. References Burt. Carter. Doran.. Pankhurst. Gregorich. the primary purpose of which is to identify and/or quantify the variability in all or part of the sampling and analysis system. New York..B.A. sequential. Water samples require expedited transport under ice or gel packs and are refrigerated (4 °C) immediately upon arrival at the laboratory. Characterization of mineral forms in Andepts from Chile. Bur. Daniels. E. Sci.G. Mines and Miner. US GPO. McGraw-Hill Co. These other water analyses also need to be performed as promptly as possible.M. without the introduction of change or contamination. Soils and geomorphology in the basin and range area of southern New Mexico—Guidebook to the desert project . Am. Follett. 1994.000.E.. Johnston County North Carolina. Hawley. 1975.) Soil quality for crop production and ecosystem health. Common types of replicate samples include concurrent. Boca Raton. Dwyer.W. E.. NY. Physiography of the western United States. Biological attributes of soil quality. and field blanks). WI. Soil.M. Proc. Include replicate samples in the sampling plan. 2001. Proc.S. In J.A. Preserve samples in the field-state until analysis at the laboratory. 1938.W. Sci.. Rust. E. Physiography of the eastern United States. S. US Geological Survey. In R.M. rinse the containers several times with the sample water and completely fill the container and screw cap with the sample water. Properly label sample containers to show important information. e. Gile. 39:556-561. Washington DC.M. Mem.) Defining soil quality for a sustainable environment. Soc. SSSA. and J.gov/. N. Franks. Fl. W. and sampling design under development by NRCS. Samson-Liebig. total and inorganic C..W. Daniels. M. J. 1931.W. Defining and assessing soil quality. In E. 3-21. Soc.H.45-µm membrane) is used to separate dissolved from suspended material. E. There are many possible types of blanks (e. Sobecki.R. L. Fenneman. source-solution. 714 pp. 1996). N.. location. 1981. 222 p. 1996. Organic carbon methods. 1970. the primary purpose of which is to identify potential sources of sample contamination and assess the magnitude of contamination with respect to concentration of target analytes.

. McDonald.A. J. C. 2002. Quality assurance of chemical measurements. H. P. Exp. Soil Sci. Am. B. Soil survey manual. DC. Soc.E. 1965. Am.M.V. Water analysis. Boca Raton. Agric. 42. London.. No. Lincoln. A4. Proc. Soc. 1995. In Martin R. Elsevier Sci. Lincoln. M.J. C. 67:1309-1317. book 9. Pankhurst. Buckerfield. NE. England. Version No. C. Washington. Ruhe. Laurent. MI.J. W. Wysocki. C. E. Benham.0. Nanzyo. B.. Taylor.). and R.E.M.. p. Dahlgren.S. p. D.S.B. B. Handb. Nanzyo. Physical characteristics of volcanic ash soils. 2nd ed. In P. Michelsen. and V. P. R. and H. Iwatsubo. Inc. Soil Sci.A.B. Chelsea. FL. Soil Survey Staff. Print. Print. O’Brien. 1997. Cady. Lee. J. Washington. Schoeneberger.. D. Lewis Publ. Developments in soil science 21.K. M.. 1993. and E.0. and A. Soil Survey Staff. Secondary mineral genesis from chlorite and serpentine in an ultramafic soil toposequence. genesis.T. Vali. 436. Gupta (eds. 437 p. DC. 1970. Soil Sci..J. R. Ness. Collection of water samples: U. and B.E.. Shoji. and R. Lee. Wilde. Soil Conservation Service. Amrhein. No. U. Washington. Landscape evolution and soil formation in southwestern Iowa. Agric. J. 1988. J.. and C.A. F. T. Soil Sci. 18:79-87. 118:303-320. Biological indicators of soil health. Can. C. Office. J. Oregon. Office. Willamette Valley. J.E. 1967. B. van Lagen.B. Physiography of the United States. Part 629. Physiographic divisions of Alaska.S. and W. Washington. Carter (ed. Govt. Evaluation of soil biological properties as potential bioindicators of soil health. DC.A. 18. accessed May 2004 at http://pubs. chap. Freeman & Co.C.D. S. Broderson (eds. Pedogenesis in a wetland meadow and surrounding serpentinitic landslide terrain. Parsons. 15 . Soil Sci. 35:1015-1028. Hawke. Nutr. Kubota. 1-4. 2003a.C. In P.R. J. USDANRCS.J.J. Soil Survey Division Staff. 34: 485-491.). Soil Survey Investigations Report No. DC. U.. UK. 1967.D. 52 p. The Netherlands. Radtke.H. USDA-NRCS. V. R.water. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. Govt. T. Am. Patterson.D. Version 2. Creasy. Print. 1999.. Amrhein. 2001.) Volcanic ash soils. Handb. 3. Amrhein.D.Hunt. Print. Spatial distributions of soil chemical conditions in a serpentinitic wetland and surrounding landscape.) Soil sampling and methods of analysis. and Plant. 121-242. NE.V. G. E. USA. 65:1183-1196. CAB International Wallingford. Lewis Publ.D. C. Doube.G. Pankhurst. B. National Soil Survey Center. USDA. Soil development and geomorphic surfaces. Office. Dahlgren (eds. Office. Geoderma. 1996. B. Field book for describing and sampling soils. Shoji. Backhuys Publ. US Geological Survey Professional paper 482.S. K. Daniels. Sears.usgs. Graham. and R. Velthorst (eds. Soil survey laboratory methods manual.S. Amsterdam. Laurent.M. Geological survey techniques of water resources investigations. and D. R. 1999.S.O. Govt. Aust. and R. Aggregate formation of allophanic soils: Effects of drying on the dispersion of soils. 1996. Soil Survey Staff. 1972. Leiden. 1993. Schoeneberger. Buurman. 1998.C. Balster. 1. Govt. Wahrhaftig. 2003b.A. USDA-NRCS. Soc. Lee.gov/.T. Doube. USDA Tech. Kirkby. Soc. National Soil Survey Center. 1349. properties and utilization. northern California.C.G.K. 1993. In S. 480 p. Collection and preparation of soil samples: Site description. Wysocki. R.. Gupta. National soil survey handbook USDA-NRCS. Gibs. S. pp 189-207.. U. Glossary of landforms and geologic materials. T. 1984. C.B. Bull. U. Geomorphology. Procedures for collecting soil samples and methods of analysis for soil survey.V.R.) Manual for soil and water analysis. Velthorst. C. R. USDA-SCS Soil Survey Investigations Report No. Graham.S. Graham.C. Publ..

. Sub-sampling reduces the cost of the investigation.L. Schoeneberger.L. In M. p. 1986). Microbiological and biochemical properties.S. Soil material needs to be adequate in amount and thoroughly mixed in order to obtain a representative sample. Wollum. The SSL receives bulk soil samples from across the U. ASA and SSSA.. Madison. Undisturbed clods are used to investigate micromorphology and determine some physical properties.Wilson.. 1994.e. i. and mineralogical analyses. as it permits the estimation of some characteristics of the larger sampling unit without the necessity of measurement of the entire unit.. field-moist) and the original and final particle-size fraction (e. 1986). Baird. LaGarry. P..and laboratory-assigned numbers that carry important information about the soil sample (e. Boca Raton. D'Agostino. Efficient use of sub-sampling depends on a balance between cost and precision (Petersen and Calvin. Anderson. Soil variability and sample size are interferences to sample collection and preparation. These identification numbers are unique client. pedon. Sumner (ed.g. Wysocki. No. and H. A. 1-14. e. 45 (1995) for a detailed explanation of sample identification numbers. bulk density. S.g. Identification numbers and preparation codes are reported on the SSL Primary Characterization Data Sheets. Southard. K.S. ISBN: 0-8493-3136. All soils from quarantined areas are strictly controlled under APHIS quarantine regulations 7 CFR 330. and P.W. CRC Press LLC. and cores.A. an additional component of variability.D. but usually decreases the precision with which the soil characteristics are estimated. Refer to the Soil Survey Investigations Report (SSIR) No. and mineralogical analyses. physical.J. and year sampled).B. location.G. Sub-sampling also may be used.) Handbook of soil science. Angle. FL. M.g. These codes carry generalized information about the characteristics of the analyzed fraction. National Soil Survey Center Soil Technical Note Handbook 430-VI Amendment 5. For preparation procedures for soil bulk samples.P.. there has been a significant revision of these preparation codes. November 15. soil horizon.. 6 publication of laboratory data in soil surveys. sieved <2-mm fraction processed to 75 µm) and by inference. D. Weaver. Detailed information on the current preparation codes as they appear on the Primary Characterization Data Sheets may be obtained from the SSL upon request. S. and S. Laboratory preparation codes depend on the properties of the sample and on the requested analyses. 1986). 42 (1996).. At each stage of sampling. Arroues. physical. the water content (e. WI. Bottomley (eds. This version of the SSIR No.A.E. Geomorphology of soil landscapes.) Methods of soil analysis. 1994. the variability within the larger units. the type of analyses performed. Part 2.E.S. The objective of laboratory preparation is to homogenize the soil samples used in chemical. is added to the sampling error (Petersen and Calvin. In R.g. and internationally for a wide variety of chemical. J. Since the publication of the SSIR No. 2000. 16 . clods. Bulk Samples (1B1a1) Laboratory identification numbers and preparation codes are assigned to bulk soil samples. Sampling provides a means to estimate the parameters of these soil characteristics with an acceptable accuracy at the lowest possible cost (Petersen and Calvin. R. proceed to 1B1b. Laboratory Sample Collection and Preparation (1B) Soil (1B1) Samples (1B1a) The purpose of any soil sample is to obtain information about a particular soil and its characteristics. air-dry. Soil sampling for microbiological analysis. 42 (2004) does not describe in detail the revised preparation codes. The SSL also typically receives natural fabrics.

N. and mineralogical analysis. to meet the sample preparation requirements of the analytical instrument. some standard air-dry analyses by definition may require non-sieved material. depending on the type of soil material. and plasticity index for Andisols and Spodosols (1B1b1c1). These identification numbers typically relate to a corresponding bulk sample.. available water capacity and linear extensibility. 1999) to define sapric.Natural Fabrics. Air-dry is generally the optimum water content to handle and to process soil. and Cores (1B1a2-4) Laboratory identification number and preparation codes are assigned to natural fabrics (NF).. and/or when moist chemical analyses (1B1b1b1) are appropriate..g.. For some standard air-dry analyses. Knowing the amount of rock fragments is necessary for several applications. e. samples can be tested for the proportion and particle-size of air-dry rock fragments that resist abrupt immersion in tap water (1B1b2f1a3). Generally. laboratory preparation procedures were described as standalone methods based on various procedures summarized by specific preparation codes that are reported on the SSL Primary Characterization Data Sheets. and discarded (1B1b2f1a) and are excluded from most chemical. the weight of air-dry soil remains relatively constant. and fibric organic materials. The intent herein is not to detail all possibilities of the universe but to describe some of the master preparation procedures that are typically requested for laboratory analyses. In this version of the SSIR No. whole-soil samples for aggregate stability (1B1b2a1) A field-moist. and soil quarantine regulations. e. physical.g.or gypsum-indurated material or material from Cr and R soil horizons.. Additionally.g. Some exceptions include but are not limited to samples containing coarse fragments with carbonate.g. or the coarse fragments and fine-earth material are homogenized and crushed to < 2 mm with laboratory analyses made on the wholesoil (1B1b2f1b1a). and biological activity is low during storage. e. and S (1B1b2d1). e. Additionally. For routine soil analyses. Clods. hemic. Atterberg Limits (1B1b2c1). and as such the evaluation of these materials (Histosol analysis) require a field-moist. 42. weighed. Application In the SSIR No.. e. fine-earth (<2-mm) fraction (method 1B1b2b1). the coarse fragments may be crushed to <2 mm and analytical results reported on that fraction. total C.g. 42 (1996). Some biological analyses require field-moist samples (1B1b1a2). This approach is the logic base whereby laboratory procedures are described in this version of the SSIR No. The decomposition state of organic materials is used in soil taxonomy (Soil Survey Staff. the <2-mm fraction is further processed so as to be in accordance with a standard method.g. Laboratory analyses of soil samples are generally determined on the air-dry. preparation codes. e. e. In addition.. 17 . water retention (1B1b1b2). and Canadian laboratories homogenize and process samples to pass a 2-mm sieve (Bates. whole-soil sample (1B1b1a1). most U. 42 (2004). total elemental analysis (1B1b2e1) and carbonates and/or gypsum (1B1b2d2). In these cases. as air-drying may cause significant changes in the microbial community. 1993). clods. A process approach is appropriate in that any one sample received from the field may result in a number of laboratory sub-samples being collected and prepared based on analytical requests and type of materials. and cores. Refer to 1B1a1 for information on these identification numbers.S. 2 to 20 mm (1B1b2f1a2a).g. <2-mm sample is prepared when the physical properties of a soil are irreversibly altered by air-drying. Soil Sample Preparation (1B1b) 1. these procedures are described more as a procedural process. the >2-mm fractions are sieved. particle-size analysis. or to achieve greater homogeneity of sample material.

<0. This process is repeated four times. crushed. 3. e. and 2.1 Electronic Balance. Whenever possible. square-hole. rubber stopper and placed in a refrigerator for future analysis. 2004). the fine-earth fraction and the >2-mm fractions are homogenized and passed through a laboratory jaw crusher to reduce all material to pass a 2-mm sieve.2. physical. 4. and mineralogical analysis.g. weight measurements are made and recorded on the 20. Safety Dust from sample processing is a nuisance. The HCl used to check carbonates can destroy clothing and irritate skin. tared 5. "moist" samples or materials should have weights two to four times larger than for "dry" specimens (American Society for Testing and Materials.to 5-mm fractions. some or all of these >2-mm fractions may be processed to a finer fraction and saved for chemical.2 Cardboard trays for sample storage 5.to 20-mm and 2.1 80 mesh. Air-dry.to 20mm. plastic.0 kg. stainless steel 5. an additional component of variability. 1986). For most standard chemical.425 mm for Atterberg Limits and ≈ 180 µm for chemical analysis of organic materials. if needed. Equipment 5. Field-moist. Use a face-shield and goggles when operating the jaw crusher. In other cases. fine-earth fraction samples are processed by forcing the material through a 2-mm screen by hand or with a large. Generally.4. ±1-g sensitivity and 15-kg capacity 5. after the respective weights of the 5. the minimum specimen size ("dry" weight) that needs to be sieved and weighed is 1. air-dry and/or field-moist samples may also be prepared as whole-soil samples or processed further to finer fractions than <2 mm. Keep clothing and hands away from the crusher and pulverizer when these machines are in use. Interferences Soil variability and sample size are interferences to sample collection and preparation. with the recombined material saved for laboratory analysis. 5. and mineralogical analysis.4 Sieves. Enough soil material needs to be sieved and weighed to obtain statistically accurate rock fragment content. 180 µm 18 . Additionally.to 5-mm fractions are recorded. Refer to ASTM Standard Practice D 2488 (American Society for Testing and Materials. At each stage of sampling. In order to accurately measure rock fragments with a maximum particle diameter of 20 mm. Soil material needs to be in adequate amount and thoroughly mixed to obtain a representative sample. 2004). with these fractions then discarded. <75 µm sub-samples for major and trace elements are processed metal-free. Immediately rinse acid with water from clothing or skin and seek professional medical help. 2004). A mask should be worn in order to avoid breathing dust. with the processed material saved for laboratory analysis. A homogenized soil sample is more readily obtained from air-dry material than from field-moist material. For example. the variability among smaller elements within the larger units. 5. In some cases. Use goggles when operating the air compressor.. Depending on the nature of the soil material and requested analyses. Soil is mixed by moving it from the corners to the middle of processing area and then by redistributing the material. Summary of Method Any one soil sample received from the field may result in a number of laboratory subsamples being collected and prepared based on the properties of the sample and on the requested analyses. is added to the sampling error (Petersen and Calvin.3 Trays. these fractions may be recombined and crushed to <2 mm in a laboratory jaw crusher. Refer to ASTM Standard Practice D 2488 (American Society for Testing and Materials. these weight measurements may not be recorded. and sieved to <2 mm. the field sample is air-dried.to 75-mm. physical.

nylon cloth sieve 5.4 19 mm.6 Wooden rolling pin 5.5.16 Planetary ball mill.to 15-mm.4. Harrison. 7.9 Metal plate. 2-oz 5. 1.12 Scintillation glass vials. Model P-5.4.5 If only air-dry sub-samples are requested. Fritsch. 7.94 g of sodium carbonate (Na2CO3) in 1 L of RO water. Brinkmann Instruments Inc.7 Rubber roller 5. 5.4 If field-moist sub-samples are requested. Model BB2/A. and/or 8 oz with tops 5. IL.17 Syalon balls. 75 µm. proceed to procedure 1B1b2.. Thoroughly mix soil material.18 Metal weighing cans. Dissolve 35.5 76 mm. Brinkmann Instruments Inc. SpeedAire. IL. 1-pint. Cast-iron Series. 3/4 in 5.4. 20-mL 5.2 1 N HCl 6. 2 mm 5.4. <2-mm sub-samples are requested.7 40-mesh. 19 . Soil Bulk Sample Preparation (1B1b) Field-Moist Preparation (1B1b1) 7. proceed to procedure 1B1b1b. proceed to procedure 1B1b1.5 Pulverizer 5.75 mm 5. 7.425 mm 5.15 Air compressor. OH.4.10 Containers. 0. 80-mL 5. Co.. 2-oz 5. 3 in 5.1 Reverse osmosis (RO) water 6.6 If field-moist. whole-soil sub-samples are requested. proceed to procedure 1B1b1a. Lewis Center.3 Sodium hexametaphosphate solution.2 Weigh sample in sample bag to nearest g before air-drying and record weight. plastic. and bowls. Retsch. 7.5 cm 5.6 200-mesh. paper.3 4 mesh.11 Containers.14 Brown Kraft paper 5. Reagents 6.7 If only field-moist. 4. Des Plaines.13 Metal weighing cans. 7. 76 x 76 x 0.19 Cross beater mill. 4. 7.7 g of sodium hexametaphosphate (NaPO3)6 and 7. OH 5. Procedures Soil Bulk Sample Preparation (1B1b) 7. 6. with lids 5. Campbell Hausfeld Mfg.8 Laboratory jaw crusher.1 Weigh soil sample in sample bag to nearest g when logged-in and record weight.4. 12. 12-oz.3 Remove soil sample from sample bag and distribute on a plastic tray. 5. Gilson. Des Plaines.2 10 mesh. Retsch..

<2-mm sub-samples include but are not limited to 1B1b1b1. select material for representative sub-samples from at least five different areas on the plastic tray.10 For biological analyses. Store the biology bulk sample in the refrigerator for future analysis. Process a sub-sample of field-moist material by forcing the material through a 2-mm screen by hand or with a large. Process a subsample of field-moist material by forcing the material through a 2-mm screen by hand or with a 20 . Soil Bulk Sample Preparation (1B1b) Field-Moist Preparation (1B1b1) <2-mm Fraction (1B1b1b) 7. This sub-sample is termed a biology bulk sample.11 Procedures for field-moist.Soil Bulk Sample Preparation (1B1b) Field-Moist Preparation (1B1b1) Whole-soil (1B1b1a) 7. 1B1b1b2. select material for representative sub-samples from at least five different areas on the plastic tray. Soil Bulk Sample Preparation (1B1b) Field-Moist Preparation (1B1b1) Whole-soil (1B1b1a) Biological Analysis (1B1b1a2) 7. whole-soil prepared in an 8-oz container. whole-soil sub-samples include but are not limited to 1B1b1a1 and 1B1b1a2 as follows: Soil Bulk Sample Preparation (1B1b) Field-Moist Preparation (1B1b1) Whole-soil (1B1b1a) Histosol Analysis (1B1b1a1) 7. rubber stopper and place in a 1pint plastic container.8 Procedures for field-moist. Prepare a sub-sample of the field-moist. select material for representative sub-samples from at least five different areas on the plastic tray.9 For Histosol analysis. Store in the refrigerator for future analysis. Prepare a sub-sample of field-moist. Store in the refrigerator for future analysis. 1B1b1b3. which may be obtained from the bulk soil sample upon arrival at the laboratory.13 For moist 1500-kPa water content of mineral and organic material.12 For moist chemical analysis. proceed to 1B3. Soil Bulk Sample Preparation (1B1b) Field-Moist Preparation (1B1b1) <2-mm Fraction (1B1b1b) 1500-kPa Water Content (1B1b1b2) 7. select material for representative sub-samples from at least five different areas on the plastic tray. and 1B1b1c1 as follows: Soil Bulk Sample Preparation (1B1b) Field-Moist Preparation (1B1b1) <2-mm Fraction (1B1b1b) Chemical and Selected Physical Analysis (1B1b1b1) 7. For additional information on biology collection and preparation procedures. whole-soil prepared in a plastic container.

22 For aggregate stability analysis.19 If air-dry. proceed to procedure 1B1b2a. Prepare an air-dry. whole-soil sub-samples are requested. Process a sub-sample of field-moist material by forcing the material through a 2-mm screen by hand or with a large. rubber stopper and place in a 4-oz plastic container. Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) 7.18 Weigh sample to nearest g after air-drying and record weight.14 For field-moist/oven-dry (FMOD) ratio (required if any moist analyses are determined).16 Before air-drying.425 mm (1B1b1c) Atterberg Limits (1B1b1c1) 7. Soil Bulk Sample Preparation (1B1b) Field-Moist Preparation (1B1b1) <2-mm Fraction (1B1b1b) Field-Moist/Oven-Dry Ratio (1B1b1b3) 7. 7. select material for representative sub-samples from at least five different areas on the plastic tray. 7.425 mm). <2-mm sub-samples are requested. weigh sample on a tared tray (tray weight) to nearest g and record weight. Place sub-sample in a 12-oz plastic container and store in the refrigerator for future analysis. rubber stopper and then sieved to 40-mesh (0.20 If only air-dry.large. 7. whole-soil sample in a 12-oz paper container. Process a sub-sample of field-moist material by forcing the material through a 2-mm screen by hand or with a large. Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) Whole-Soil (1B1b2a) 7. select material for representative sub-samples from at least five different areas on the plastic tray. 21 . rubber stopper and place in a 2-oz metal weighing can. proceed to procedure 1B1b2b.17 Air-dry the sample in an oven at 30 to 35° C for 3 to 7 days.15 For moist Atterberg Limits. whole-soil sub-samples include but are not limited to 1B1b2a1 and 1B1b2a2 as follows: Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) Whole-Soil (1B1b2a) Aggregate Stability Analysis (1B1b2a1) 7. Store in the refrigerator for future analysis.21 Procedures for air-dry. 7. Soil Bulk Sample Preparation (1B1b) Field-Moist Preparation (1B1b1) <2-mm Fraction Sieved to <0. select material for representative sub-samples from at least five different areas on the plastic tray.

substitute a rubber roller for a wooden rolling pin. Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) <2-mm Fraction (1B1b2b) Salt Analysis (1B1b2b2) 7. 7. 1B2b2b3. 7. physical. 1B2b2b2. select material for representative sub-samples from at least five different areas on the plastic tray. <2-mm fractions include but are not limited to 1B1b2b1. prepare a 12-oz paper container of fine-earth material. proceed to procedure 1B1b2f . 1B2b2d1. Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) <2-mm Fraction (1B1b2b) 7. 1B2b2b5.29 For a saturation paste when salt analyses are requested. Crush clayey soils that contain no coarse fragments in a laboratory jaw crusher. If a NF sample was not selected in the field. 1b2b2c1.25 Roll soil material on a flat. 22 . sieved <2-mm fraction in a 1-pint plastic container. 7. metal plate that is covered with brown Kraft paper with wooden rolling pin and/or rubber roller to crush clods to pass a 2-mm sieve. Physical and Mineralogical Analysis (1B1b2b1) 7.27 Procedures for air-dry. and 1B2b2e1 as follows: Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) <2-mm Fraction (1B1b2b) Standard Chemical. This weight includes the >2-mm fractions.23 For comprehensive sampling projects. Roll and sieve until only the coarse fragments that do not slake in sodium hexametaphosphate solution remain on sieve. 1B2b2b4.24 Weigh sample to nearest g and record weight.28 For standard chemical. Also prepare a 12-oz container for natural fabric (NF) sample. do not select NF samples for reference projects. sieved <2-mm fraction in a 12-oz paper container. 1b2b2d2. Prepare one sub-sample of the air-dry. select one from air-dried bulk sample. Generally. 1B2b2d3.26 Process air-dry soil by sieving to <2-mm. Thoroughly mix material by moving the soil from the corners to the middle of the processing area and then by redistributing the material. Repeat process four times. Store soil samples in repository. For preparation of the >2-mm fractions. For samples with easily crushed coarse fragments. Prepare one sub-sample of the air-dry.Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) Whole-Soil (1B1b2a) Repository Samples (1B1b2a2) 7. and mineralogical analysis. select material for representative sub-samples from at least five different areas on the plastic tray.

Prepare a subsample of air-dry. and possibly a few larger bubbles.The sample effervesces violently. Strong . these air bubbles appear immediately after the addition of 1 N HCl. add reverse osmosis water. and stir to remove entrapped air. sieved <2-mm fraction in a 2-oz metal weighing can.Bubbles rise at a few points in the sample and consistently appear at the same point in either a steady stream of tiny bubbles or in a slower stream of larger bubbles.More large bubbles are evident than with a slight reaction.33 For Atterberg Limits.31 For air-dry/oven-dry (ADOD) ratio (required if any air-dry analysis are determined). 23 .425 mm) in a 12-oz paper container. Very Slight . Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) <2-mm Fraction Sieved to 0. Many large bubbles appear to burst from the spot plate. sieved <2-mm material sieved to 40-mesh (0. Do not mistake trapped air bubbles for a positive test. Violent . Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) <2-mm Fraction (1B1b2b) Presence of Carbonates (1B1b2b5) 7. Prepare a sub-sample of the air-dry. select material for representative sub-samples from at least five different areas on the plastic tray. Often the reaction is violent at first and then quickly decreases to a reaction that produces many small bubbles. Generally.More small bubbles. appear throughout the sample than with a very slight reaction. Prepare one sub-sample of the air-dry. Place 1 g of the airdry fine-earth fraction in porcelain spot plate. Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) <2-mm Fraction (1B1b2b) Air-Dry/Oven-Dry Ratio (1B1b2b4) 7. Reference samples (knowns) are available for comparisons. and record as follows: None – No visual efferevescence. observe amount of effervescence. Add 1 N HCl to soil.425 mm (1B1b2c) Atterberg Limits (1B1b2c1) 7. select material for representative sub-samples from at least five different areas on the plastic tray.30 For air-dry 1500-kPa water content of mineral and organic materials. select material for representative sub-samples from at least five different areas on the plastic tray.32 Use a sub-sample of the ADOD sample (procedure 1B1b2b4) and check for the presence of carbonates. Slight . sieved <2-mm fraction in a 1-oz plastic cup.Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) <2-mm Fraction (1B1b2b) 1500-kPa Water Content (1B1b2b3) 7.

These fractions include mineral coarse fragments as well wood fragments that are >20 mm in cross section and cannot be crushed and shredded with the fingers. Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) <2-mm Fraction Sieved to 75 µm (1B1b2e) Total Major and/or Trace Elements (1B1b2e1) 7. proceed to procedure 1B1b2f1a3.35 Use the prepared sub-sample (procedure 1B1b2d1) for the determination of the amount of carbonates and/or gypsum. sieved <2-mm fraction processed in a planetary ball mill for 2 min and sieved to <75 µm (200 mesh) in a 20-mL scintillation glass vial.36 For chemical analysis of organic materials. If testing is requested for the proportion and particle-size of the air-dry. Prepare one sub-sample of the air-dry. and Sulfur Analysis (1B1b2d1) 7. Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) >2-mm Fractions (1B1b2f) 7. If the >2mm fractions contain carbonate. sieved <2-mm fraction processed in a cross beater to a fine grind (≈ 80 mesh.or gypsum-indurated material. proceed to procedure 1B1b2f1b1a. proceed to procedure 1B1b2f1a1a. Prepare one sub-sample of the airdry. If the >2-mm fractions are to be weighed. sieved <2-mm fraction processed in a cross beater mill to (≈ 80 mesh. select material for representative sub-samples from at least five different areas on the plastic tray. metal free. select material for representative subsamples from at least five different areas on the plastic tray. and S analyses.38 The following procedures are used for samples with >2 mm fractions. Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) <2-mm Fraction Processed to ≈ 180 µm (1B1b2b) Calcium Carbonate and Gypsum (1B1b2d2) 7.37 For total major and/or trace element analyses. >2-mm fraction that resist abrupt immersion in tap water. with no further laboratory analysis. If the >2-mm fractions are Cr or R material (Soil Survey Staff. 24 . and laboratory analysis is requested.Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) <2-mm Fraction Processed to ≈ 180 µm (1B1b2d) Total Carbon. and laboratory analysis is requested. When the data for >2-mm fractions are not recorded. Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) <2-mm Fraction Processed to ≈ 180 µm (1B1b2b) Chemical Analysis of Organic Materials (1B1b2d3) 7. 180 µm) in a 12-oz paper container. 180 µm) in a 20-mL scintillation glass vial. Nitrogen. Prepare a sub-sample of the air-dry. proceed to procedure 1B1b2f1a. 1999). recorded. N. select material for representative sub-samples from at least five different areas on the plastic tray.34 For total C. and discarded. proceed to procedure 1B1b2f1b.

to 20-mm. 2. Recorded (1B1b2f1a) 7. Weigh. Not Recorded (1B1b2f1b) 7.Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) >2-mm Fractions (1B1b2f) Particle-Size Analysis (1B1b2f1) Particle-Size Analysis. In this procedure (1B1b2f1a).to 75-mm.to 20-mm and 2. and mineralogical analysis as described in procedure 1B1b2b. soak (100 g of 2. and 2. and discard particles with diameters of 20 to 75 mm and 5 to 20 mm.to 75-mm. and discard. The <2-mm fraction is saved for chemical.40 This procedure (1B1b2f1b) is the same as described in procedure 1B1b2f1a except the weight of the >2-mm fractions are not recorded and all analytical results are reported on a <2mm basis.to 5-mm fractions are then recombined after their respective weights are recorded. physical. and Mineralogical Analysis (1B1b2f1a1a) 7. record weight.to 5-mm fraction) in sodium hexametaphosphate solution for 12 h. This material is saved for laboratory analysis and analytical results reported on the 2. Air-dry. record weight. 5 to 20-mm. physical. the standard procedure (1B1b2b) is usually requested. Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) >2-mm Fractions (1B1b2f) Particle-Size Analysis (1B1b2f1) Particle-Size Analysis. Physical.39 Process the air-dry soil by sieving to <2 mm as described in procedure 1B1b2b.to 20-mm Fraction Processed to <2-mm (1B1b2f1a1) Chemical. Process the air-dry soil by sieving to <2 mm as described in procedure 1B1b2b. If difficult to separate the <2-mm fraction from fragments. The <2-mm material is also saved for chemical.to 20-mm basis. Weigh soil material with diameters of 20.to 20-mm. 5. material is crushed to <2 mm in a laboratory jaw crusher. Recorded (1B1b2f1a) 2. and mineralogical analysis (1B1b2b) Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) >2-mm Fractions (1B1b2f) Particle-Size Analysis (1B1b2f1) Particle-Size Analysis.41 This procedure (1B1b2f1a1a) is commonly used for samples with carbonate.or gypsumindurated material. The recombined. If carbonate or gypsum accumulations are soft and easily pass a 2-mm sieve. and 2 to 5-mm and record weights as described in procedure 1B1b2f1a. The 5. weigh the material that does not slake. 25 . weight measurements are made on the 20. Weigh soil material with diameters of 2 to 5 mm.to 5-mm fractions.

9.6 9. This material is then recombined with the <2-mm fraction.42 This procedure (1B1b2f1a2a) is rarely requested. 11.to 20-mm and 2. The recombined. Section 4.Weigh soil material with diameters of 20. This material is saved for laboratory analysis and analytical results reported on the whole-soil basis.3 9. material is crushed to <2 mm in a laboratory jaw crusher.to 75-mm fraction Weight (g) of 5.to 5-mm fractions are then recombined after their respective weights are recorded. Report Reported data include but are not limited to the following: 9. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. geosynthesis.8 9. Very Slight.2 9. These analytical results are reported on the <20-mm basis or are calculated to the <2-mm basis.to 20-mm fraction Weight (g) of 2. Standard practice for description and identification of soils (visual-manual procedure). Calculations Calculations for coarse fragments are reported in 3A2. and Mineralogical Analysis (1B1b2f1b1a) 7. Annual book of ASTM standards.9 Weight (g) of field-moist soil sample Weight (g) of air-dry soil sample Weights (g) of processed air-dry soil Weight (g) of 20.to 20-mm. Not Recorded (1B1b2f1b) Whole-Soil Processed to <2-mm (1B1b2f1b1) Chemical. Physical..to 75-mm. Construction.7 9.4 9. Homogenize particles with diameters >2 mm and the fineearth material (<2-mm) and crushed to <2-mm in a laboratory jaw crusher. Strong.to 20-mm Fraction Processed to <2-mm and Recombined with <2-mm Fraction (1B1b2f1a2) Chemical.to 5-mm fraction before slaking Weight (g) of sub-sample of 2.1 9. 2004. PA.Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) >2-mm Fractions (1B1b2f) Particle-Size Analysis (1B1b2f1) Particle-Size Analysis. Process the air-dry soil by sieving to <2 mm as described in procedure 1B1b2b. Mineralogical Analysis (1B1b2f1a2a) 7. Recorded (1B1b2f1a) 2. The 5. 8.08.5 9. Physical. 5 to 20-mm. Soil and rock. 1999). 26 . ASTM. Violent) 10. Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) >2-mm Fractions (1B1b2f) Particle-Size Analysis (1B1b2f1) Particle-Size Analysis.to 5-mm fraction after slaking Effervescence with HCl (None. 04. D 2488. Slight. Philadelphia. 2. dimension stone. Vol.43 This procedure (1B1b2f1b1a) is mainly used to prepare samples from Cr or R soil horizons (Soil Survey Staff. References American Society for Testing and Materials. and 2 to 5-mm and record weights as described in procedure 1B1b2f1a.to 5-mm fraction Weight (g) of sub-sample of 2.

Monogr 9. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys.5-mm (nominally 10 mm). 19-24. Print. Part 1.) Soil sampling and methods of analysis. 1. DC. Summary of Method A representative sub-sample of the air-dry field sample is weighed and passed through a No. In M. 1996. U. Soil Survey Staff. Agric. Office.10 sieve. Washington. 10 sieve. 4. p. Soc. p. Klute (ed. Recorded (1B1b2f1a) Proportion and Particle-Size of Air-Dry Rock Fragments that Resist Abrupt Immersion in Tap Water (1B1b2f1a3) 1. USDANRCS. Soil handling and preparation. The >2-mm fraction is placed abruptly in tap water. Lewis Publ.0. 2004). There is a need for a procedure that is both reproducible and subjects the >2-mm fraction to an intermediate stress less than standard mechanical preparation.S.. 1993.Bates. 9. Can.S. Certain analyses can be run on the >2-mm fraction after separation by the water-immersion method. Calvin. Version No. FL. U. Soil Sci. Madison. 33-51. Version No. No. The resulting values can be subtracted from analyses on the whole ground sample to obtain estimates for the <2-mm fraction as removed by the water immersion treatment. T. For some situations. 4. Office. 1999. U. No. comparison of the results to use a dispersing agent may be valuable. DC. 3. 2nd ed. Physical and mineralogical methods. Handb. In A.R. 2004). Soil Survey Staff.0. left overnight. 42. and the wet >2-mm passed through a nest of No. and L. 27 . 2nd ed. Soil Survey Investigations Report No. 10. 1995. Carter (ed. Soil survey laboratory information manual. Print. 436. 2. Govt. 42. passed through a No. Govt. Soil Survey Staff. Interferences There are no known interferences. DC. R. Boca Raton. and 20-mm sieves. gently agitated. CRC Press. Print. Sampling. USDA-NRCS.D. ASA and SSSA. USDA-NRCS.E.) Methods of soil analysis. 3. Office. Soil Bulk Sample Preparation (1B1b) Air-Dry Preparation (1B1b2) >2-mm Fractions (1B1b2f) Particle-Size Analysis (1B1b2f1) Particle-Size Analysis. Petersen. for this another procedure would need establishment. WI. Safety Dust from sample processing is a nuisance.G. A mask should be worn in order to avoid breathing dust. Agron. Application It is widely accepted that the mechanical preparation of soil for laboratory analysis is difficult to standardize for samples that contain >2-mm particles with rupture resistance intermediate between earthy bodies and fragments of highly resistant rock (Grossman. Soil survey laboratory methods manual. Govt.S.. Soil Survey Investigations Report No. This method (1B1b2f1a3) provides a comparison to mechanical preparation methods and should aid in the development of more precise mechanical preparation dependent on sample properties (Grossman. Abrupt immersion in tap water of the initially air-dry >2-mm fraction has been chosen as the manner in which stress is applied. Washington. 1986. Washington.

Weigh the >2-mm particles and discard the<2-mm fraction. 7.11 Teaspoon. 5 to 20. Pour off into the sink as much of the water as possible without transfer of solids to the sink.8 Pan.7 Top loading balance. Procedure 7.000-g capacity.10 sieve and wash with a water stream to remove the material not resistant to the immersion treatment.2 Tap water of acceptable dispersability (taken as Zone A in Flanagan and Holmgren. plastic. in which 20-cm diameter sieve fits snugly 5. 60 x 40 x 15 cm 5.5 Cake pans. Air-dry the sample on the tray at 30 to 35°C.2 E = [F/(C – D)] x 100 8. 4 and No.4 5. straight-sided. 10.5 Follows 7. segregated by different colors 5.10 Plastic beads. Quantitatively transfer the >2-mm particles into the No.1 Remove roughly a one-fourth representative sub-sample inclusive of the >20-mm fraction from the field sample and weigh. with pan large enough to mount the trays listed under Section 5. Allow to stand until settled out. tablespoon 6.2 Bucket. fiberglass. large enough to line plastic container 5.1 Buckets. 8. Reagents 6. 1-g sensitivity and >10. 10 sieves. 20 x 20 x 4cm 5. plastic. 35 x 48 cm 5. Equipment 5. No.and 20-mm plus bottom pan 5. aluminum foil. 20-mm diameter No. plastic. Dry the sediment in the bucket by evaporation.to 20-mm particles as a percent of the <20-mm fraction. followed by disposal as a solid.1 A = [B/(C – D)] x 100 8.1 CaCl2·2H2O 6.4 After the 19-L bucket is full. 9. Obtain the 2 to 5.5.3 G = A + E 28 . 9 x 6 mm. 10 sieve. 1977). 7. 19-L (5-gal). place the 30-cm diameter No. 7.9 Plastic sheet.3 directly if no strength measurements. with 30-cm diameter 5. 10 sieve over the top of a 19-L diameter bucket. In the sink.6 Weigh each separate to the nearest g and report.2 Pass through a No.6 Sieves: 30-cm diameter No. 4. 7.3 Insert the hand to the bottom of the bucket and rotate the mass at one rotation per second 20 times. 7. Use a minimum amount of water. Pass through a nest of 20-mm. Leave the sample overnight. Quantitatively transfer from the 30-cm diameter sieve to a tray. Immerse the >2-mm fraction abruptly in tap water in a 10-L bucket in which there is approximately 1-L of water for roughly every 500 g of >2-mm particles. 7.3 Bucket. 10-L with 1-L marks 5. Subtract the >20-mm weight from the initial >2-mm weight. and 2. 8-mm.5. add about 30 g of CaCl2.4 Drying trays. Calculations 8.

e. 121-134. Report Report the 2 to 5. Some water analyses. as optimal preservation is not possible (Velthorst.to 20-mm fraction on <20-mm basis (%) 9. volatilization). related piping. References Flanagan. Fe.P.g. 2004. Water (1B2) Water Sample Preparation (1B2b) Avoid long periods between collection and laboratory analysis of water. electrical conductivity. These other water analyses also need to be performed as promptly as possible. 1996). PA. Avoid freezing water samples. The sample is then split into two sub-samples. total and inorganic C.to 5-mm fraction on <20-mm basis (%) B = Air-dry weight of 2. p. 5 to 20. Proportion and particle-size of air-dry rock fragments that resist abrupt immersion in tap water.g. R. Laboratory Sample Collection and Preparation (1B) Water (1B2) Samples (1B2a) As with soil samples.S. Lincoln. 11. 29 ..to 20-mm fractions as weight percentages of the <20mm fraction. Sherard and R. water samples require expedited transport under ice or gel packs and are refrigerated (4°C) immediately upon arrival at the laboratory. Mn) and the other for anion analyses. and erosion in geotechnical projects. Decker (eds. and G. Al. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.L.to 5-mm fraction after water immersion (g) C = Air-dry total weight of whole soil sub-sample (g) D = Air-dry weight of >20-mm fraction after water immersion (g) E = Weight percentage of 5.to 20-mm fraction after water immersion (g) G = Weight percentage 2.S. Grossman.where: A = Weight percentage 2.45-µm membrane) is used to separate dissolved from suspended material.B. American Society of Testing Materials. In J. and 2. Holmgren. Upon completion of these analyses. 1977.to 20-mm fraction on <20-mm basis (%) F = Air-dry weight of 5. which can influence pH and the separation of dissolved organic matter from the water phase.) Dispersive clays. USDA-NRCS. sample filtration (0.. need to be performed promptly.. Refer to 1B1a1 for information on these identification numbers and preparation codes. NE. with one acidified to pH 2 for cation analyses (e. degradation. To prevent significant changes (e. West Conshohocken. laboratory identification numbers and preparation codes are assigned to water samples..g. 10.G. Field methods for determination of soluble salts and percent sodium from extract for identifying dispersive clay soils. C. ASTM STP 623.

Additionally. If this is the case.. Biological Materials (1B3) Biological Material Preparation (1B3b) Air-Dry Preparation (1B3b2) <2-mm Fraction Sieved to <53 µm. are separate units from the soil bulk or other biology samples. Biological Materials (1B3) Biological Material Preparation (1B3b) Avoid long periods between collection and laboratory analysis of biological samples to prevent significant changes (e. and Sulfur (1B3b2a1) Refer to the section on soil biological and plant analyses (6) for additional information on the further processing and preparation of these biological samples for laboratory analysis. microbial biomass (1B3a2). requiring expedited transport under ice or gel packs and are refrigerated (4°C) immediately upon arrival at the laboratory. Biological preparation includes but is not limited to the following: Biological Materials (1B3) Biological Material Preparation (1B3b) Field-Moist Preparation (1B3b1) <2 mm (1B3b1a) Microbial Biomass (1B3b1a1) Refer to the section on soil biological and plant analyses (6) for additional information on the further processing and preparation of these biological samples for laboratory analysis. some biological samples. 30 . In other cases.. Refer to 1B1a1 for information on these identification numbers and preparation codes. biology bulk samples may be split in the field (1B3a1) and are separate sampling units from the soil bulk sample (1B1a1).g.Biological Materials (1B3) Samples (1B3a) Biology Bulk Sample (1B3a1) Microbial Biomass Sample (1B3a2) As with soil and water samples. Nitrogen. Store biology samples in the refrigerator (4°C) for future analysis. Biological Materials (1B3) Biological Material Preparation (1B3b) Air-Dry Preparation (1B3b2) <2-mm Fraction (1B3b2b) Other Biological Analyses (1B3b2b1) Refer to the section on soil biological and plant analyses (6) for additional information on the further processing and preparation of biological samples for laboratory analysis. laboratory identification numbers and preparation codes are assigned to biology samples. with > 53 µm (Particulate Organic Matter) and <53 µm Processed to ≈ 180 µm (1B3b2a) Total Carbon. Some biology samples arrive at the laboratory as part of the soil bulk sample.g. e. biological sub-samples are collected and prepared as described in 1B1b1a2. microbial community).

E. This manual also serves as the primary document from which a companion manual. A standard method is defined herein as a method or procedure developed by an organization. and E. 1988). 1992. Reporting the method by which the analytical result is determined helps to ensure user understanding of SSL data. A SOP is a procedure written in a standard format and adopted for repetitive use when performing a specific measurement or sampling operation. Procedures for Collecting Soil Samples and Methods of Analysis for Soil Survey (1972. 42 in enough detail that they can be performed in many laboratories without reference to other sources. a SOP may be a standard or one developed by a user (Taylor. 1995).Biological Materials (1B3) Biological Material Preparation (1B3b) Dry (50˚C) Preparation (1B3b3) Roots (1B3b3a) Root Biomass (1B3b3a1) Roots Processed to ≈ 180 µm (1B3b3a1a) Total Carbon. References Velthorst. B. Nitrogen. 1996. i. van Lagen. 1982.0 replaces as a methods reference all earlier versions of the SSIR No. and Sulfur (1B3b3a1a1) Plants (1B3b3b) Plant Biomass (1B3b3b1) Plants Processed to ≈ 180 µm (1B3b3b1a) Total Carbon.) Manual for soil and water analysis. p. Water analysis. This linkage between laboratory method codes and the respective analytical results is reported on the SSL data sheets.J. and 1984). both of which are documented by method codes and linked with analytical results that are stored in the SSL database. All SSL methods are performed with methodologies appropriate for the specific purpose. 31 . CONVENTIONS (2) Methods and Codes (2A) The SSL ensures continuity in its analytical measurement process with the use of standard operating procedures (SOP’s). 1.e. Included in the SSIR No. 45. SSL-developed methods. Buurman. and 1996. and Sulfur (1B3b3b1a1) Refer to the section on soil biological and plant analyses (6) for additional information on the further processing and preparation of these biological samples for laboratory analysis. 1988). The SSL SOP’s are standard methods. Version 4. respectively) and SSIR No. has been developed. 45 describes in greater detail the application of SSL data. The standard methods described in the SSIR No. Soil Survey Laboratory Information Manual (SSIR No.. In addition. 42 (1989. peer-recognized methods. this linkage provides a means of technical criticism and traceability if data are questioned in the future. 1999). The methods in current use at the SSL are described in the SSIR No. based on consensus opinion or other criteria and often evaluated for its reliability by a collaborative testing procedure (Taylor. Soil Survey Laboratory Methods Manual. Velthorst (eds. Nitrogen. The use of SOP’s provides consistency and reproducibility in soil preparations and analyses and helps to ensure that these preparations and analyses provide results of known quality. 42 are descriptions of current as well as obsolete methods. Leiden. and/or specified methods in soil taxonomy (Soil Survey Staff.J. 121-242. The SSIR No. 42. Backhuys Publ. In P. Descriptions of the obsolete methods are located at the back of this methods manual.

e. refer to the SSIR No. coefficient of linear extensibility (COLE) and water retention difference (WRD) and reported these values along with the analytical data on the SSL Primary Characterization Data Sheets. <20. As in past versions of the SSIR No. While these data have been assigned method codes. and in electronic forms. Since the publication of the SSIR No. Historically. This version of the SSIR No. 42. Primary and Supplementary Characterization Data Sheets.g. the SSIR No. With the exception of some SSL primary analytical data included for user convenience. Soil Survey Information Manual (1995) and Soil Taxonomy (Soil Survey Staff.. 1999). 42 carries not only the new method codes but also the older ones as well. However. refer to the SSIR No. This tradition is followed in this version of the SSIR No. Additional information may also be obtained from the SSL upon request. 1999). quantitative or semi-quantitative measurements. all data are reported on the basis of the <2-mm material. 42 has described and assigned method codes to only those data reported on the Primary Characterization Data Sheets. <75 mm. Weighted Average Clay. 42 (1996). Data on the Supplementary and Taxonomy Characterization Data Sheets are not described in this manual.. e. 42 follows this tradition. as many older SSL data sheets and scientific publications report these older codes. the older method code structure had only a maximum of four characters. Size-Fraction Base for Reporting Data (2C) Particles <2 mm (2C1) Particles <Specified Size>2mm (2C2) The reporting conventions for particle-size fractions for the < 2 mm and > 2mm fractions are herein designated as 2C1 and 2C2. e. there are other calculated data on the Primary Characterization Data Sheets that appear as “Pedon Calculations”.usda. Since the publication of the SSIR No. Soil Taxonomy Characterization Data Sheets.. Most of these methods are analytical in nature. Additionally. These calculated data are not assigned method codes nor described in this manual. and CD-ROMs.g.gov/. whereas the new structure has more characters.g. resulting in a re-structuring of the method codes. e. These older codes are cross-referenced in a table preceding the method descriptions of the obsolete SSL methods This linkage between the two method code systems is important to maintain. i. mineralogical.4. 45 (1995) and Soil Taxonomy (Soil Survey Staff. and 32 . and include physical. and biological analyses.. 42. For more detailed information about the calculation and application of these derived values. More recently. chemical.g... 42 (1996). particle-size and sample weight bases for reporting data. 42 has described some derived values. carrying more information about the method. Sample collection and preparation in the field and the laboratory are also described. there has been a significant increase in the number and kind of methods performed at the SSL. The SSL data have been provided in reports. using analytical data as a basis for calculation and do not carry method codes. respectively. e. Data Types (2B) The methods described herein identify the specific type of analytical or calculated data. there have been a few more derived values added to the Primary Characterization Data Sheets.e.g.g. including tapes. 42. For more detailed information about the calculation and application of these derived values. 45. Other size fractions reported on the Primary Characterization Data Sheets include but are not limited to the <0. e. the current method codes are hierarchical and alphanumerical. Unless otherwise specified. the SSIR No.. 6A1b. disks. and data are available via the NRCS Soils web site http://soils. the data on the Supplementary and Taxonomy Characterization Data Sheets are derived data. detailed descriptions are not included in this version of the SSIR No.Information is not available to describe some of these obsolete procedures in the same detail as used to describe the current methods in the laboratory. This version of the SSIR No. Historically. other reports have been developed.

tr(s) Trace.4 is not certain. Historically. -. respectively. As a rule of thumb. if present in the soil. the SSL uses the procedure of significant figures to report analytical data. If a value is reported as 19.. to calculate the sample weight that is equivalent to the required OD soil weight. Tr. 33 . and if required in a procedure. all data are reported on an oven-dry weight or volume basis for the designated particle-size faction. The maximum particle-size set is recorded in the parentheses in the column heading. Data Sheet Symbols (2F) The analytical result of “zero” is not reported by the SSL. The base with which to calculate the reported >2mm percentages includes all material in the sample smaller than the particle size recorded in the column heading. The calculation of the air-dry/oven-dry (AD/OD) ratio is used to adjust AD results to an OD weight basis and. if required in a procedure. these weights are reflective of the water content at the time of sample collection.. the 0. 1978). significant figures are said to be all digits that are certain plus one. either is not measurable by quantitative procedure used or is less than reported amount.4 units. . The calculation of the fieldmoist/oven-dry (FM/OD) ratio is used to adjust FM results to an OD weight basis. includes boulders with maximum horizontal dimensions less than those of the pedon. The FM/OD ratio is calculated by procedure 3D2. -(s) None detected by sensitive qualitative test. The AD/OD ratio is calculated by procedure 3D1. The AD/OD ratio is converted to a crystal water basis by procedure 3D3 for gypsiferous soils (Nelson et al. The maximum coarse-fragment size for the >2-mm base varies. Significant Figures and Rounding (2E) Unless otherwise specified. commonly termed whole soil. i. FM weight is defined herein as the sample weight obtained without drying prior to laboratory analysis. The maximum size for fragments >75 mm. Sample Weight Base for Reporting Data (2D) Air-Dry/Oven-Dry (2D1) Field-Moist/Oven-Dry (2D2) Correction for Crystal Water (2D3) Unless otherwise specified. to calculate the sample weight that is equivalent to the required OD soil weight. The base usually includes those fragments as large as 75 mm (3 in). The following symbols are used or have been used for trace or zero quantities and for samples not tested.Analysis run but none detected. In general. which contains some uncertainty.Analysis run but none detected. air-dry soils contain about 1 to 2 percent water and are drier than soils at 1500-kPa water content.the whole-soil base. repeated analyses of the same sample would vary more than one-tenth but generally less than a whole unit.e. TR Trace. detected only by qualitative procedure more sensitive than quantitative procedure used. tr. AD and OD weights are defined herein as constant sample weights obtained after drying at 30±5°C (≈ 3 to 7 days) and at 110±5°C (≈ 12 to 16 h).

DC. Govt. USDA-SCS. USDA-SCS. 1. Soil Survey Staff. USDANRCS. Soil Survey Investigations Report No. 1999. Print. Office.blank Analysis not run. Soil Survey Staff. Print. In the USDA classification system (Soil Survey Staff.. 1989. Soil survey laboratory methods manual.0. Print.S. Govt. USDANRCS. Soil survey laboratory information manual. DC. These distribution curves are used in many kinds of investigations and evaluations. 42. International Union of Soil Science (IUSS). No. Soil Survey Staff. Soil Survey Investigations Report No. References Soil Conservation Service. The behavior of most soil physical and many chemical properties are sharply influenced by the particle-size distribution classes present and their relative abundance. Particle-size distribution analysis is a measurement of the size distribution of individual particles in a soil sample. 42. silt. Print. 1. and soil science (Gee and Bauder. Soil Survey Staff. USDANRCS. Washington. DC. Office.S. Washington. Soil Conservation Service. Handb. In 34 .g. 1992. Soil survey laboratory methods manual. Version No. Office. Precise meaning is given to the term soil texture only through the concept of particle-size distribution (Skopp. 1984. 1996. 1992).0. particle-size is used as a tool to explain soil genesis. Agric. Soil Survey Investigations Report No. Application General: One of the most requested SSL characterization analysis is particle-size distribution analysis (PSDA). In addition to the USDA soil classification scheme. Govt. Soil Conservation Service. DC.S. hydrologic.S. e. Soil survey laboratory methods and procedures for collecting soil samples. SOIL PHYSICAL AND FABRIC-RELATED ANALYSES (3) Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) 1.05 since 0. Version No. Soil Survey Staff. U. These data may be presented on a cumulative PSDA curve. 1953. the Canadian Soil Survey Committee (CSSC). Govt. Version No. 1. Print. Govt. U. Office.1 is in fact <0. DC.S. DC. 436. U. Print. DC. Govt. Govt.0. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. Govt.S. Office. 1982.1. Soil Survey Investigations Report No. 1. Soil Survey Investigations Report No. Office. Soil survey laboratory methods manual.g.0. 1999). and American Society for Testing and Materials (ASTM). Washington. Version No. U. Print. It also recognizes proportions of five subclasses of sand. Office. 42. <0. Soil Survey Investigations Report No. U. 1995. 2nd ed. 1972. Washington. Soil survey laboratory methods and procedures for collecting soil samples.g. < Either none is present or amount is less than reported amount. USDA-NRCS. and define soil texture.1 is reported as 0. 1.S.. 1986). 2. Washington. U. quantify soil classification. e. 3. geomorphic. DC. Soil survey laboratory methods and procedures for collecting soil samples. Washington. engineering. Washington. USDA-SCS. the particle-size classes for differentiation of families in soil taxonomy (Soil Survey Staff. Washington. geologic. U. In soil science.05 to 0. Soil Survey Investigations Report No. USDANRCS. Print. there are other classification systems. and sand on a <2-mm basis. soil texture refers to the relative proportions of clay. 42..S. Office. U. analysis not run. e. 1993). nd Not determined.

2 µm. In particle-size classes of soil taxonomy (Soil Survey Staff.05 mm). with five subclasses of sand (very coarse. mechanical.. Upon completion of the chemical treatments. 1986). The break between sand and silt is 0. Standard SSL PSDA (3A1a1): The procedure described herein covers the destruction or dispersion of <2-mm diameter soil aggregates into discrete units by chemical. 1999). soils are pretreated to remove organic matter and soluble salts. special pretreatment and dispersion procedures (3A1a2-5) may be performed upon request by the project coordinator on the sample as follows: 35 . Fe. sandy loam.. re-hydration of clays. silt. Particle-size classes are a compromise between engineering and pedologic classes (Soil Survey Staff. The Kilmer and Alexander (1949) pipet method was chosen by the USDA Soil Conservation Service because it is reproducible in a wide range of soils.074-mm diameter. as this class limit represents the optical limits of the polarizing light microscope. respectively. The percentage fine clay is determined for soils that are suspected of having illuviated clay. or a coarser class and is treated as silt if the texture is very fine sand. and very fine) and two subclasses of silt (coarse and fine). the very fine sand (VFS) separate is split. the SSL determines the fine-clay and/or carbonate clay fractions.g. Fine-clay data can be used to determine the presence of argillic horizons or as a tool to help explain soil genesis. the VFS is treated as sand if the texture is fine sand.05 and 0. medium.05 to 2. The SSL routinely determines the soil separates of total sand (0. it is important to recognize that these other classification systems are frequently cited in the literature. have a major bearing on the physical properties which soils exhibit (Sumner. 1999). or ultrasonic means. the amount of each size-fraction is then gravimetrically measured as a percent of the total sample weight on an oven-dry basis. especially engineering systems.reporting and interpreting data. it is often subtracted from the total clay in order to make inferences about soil genesis and clay activities. The cation exchange capacity of carbonate clay is very low compared to non-carbonate clay. The sodium hexametaphosphate complexes any calcium in solution and replaces it with sodium on the exchange complex. The 0. The coarse silt is a soil separate with 0. loamy very fine sand.02 to 0.e. The carbonate-clay fraction is considered important in PSDA because clay-size carbonate particles have properties that are different from non-carbonate clay. silt (0. 1992). The primary objectives of dispersion are the removal of cementing agents. and the physical separation of individual soil particles (Skopp. i. mechanical agitation through shaking is used to enhance separation of particles and facilitates fractionation. Fine-Clay and Carbonate Clay: In addition to the routine soil separates of sand. American Association of State Highway and Transportation Officials (AASHTO) and the ASTM Unified Soil Classification System (USCS) (Gee and Bauder. In the standard SSL procedure (3A1a1).02-mm (20 µm) is the break between sand and silt in the International Classification system. In engineering classifications. 1999). the VFS is allowed to float. followed by the separation or fractionation of these particles according to size limits through sieving and sedimentation (Gee and Bauder. 1992). or a finer class (Soil Survey Staff. In engineering classes. The particle-size separation at 20 µm also has significance in optical microscopy. Since carbonate clay is a diluent. Pretreatment and Dispersion Techniques: The phenomena of flocculation and dispersion (deflocculation) are very important in determining the physical behavior of the colloidal fraction of soils and thus indirectly. silt loam. e.002 to 0. The fine-clay fraction consists of mineral soil particles with an effective diameter of <0. Upon isolation of these particle-sizes or size increments. fine. The hydrogen peroxide oxidizes the organic matter.02 mm in the USDA and International classification systems. Water holding capacity of carbonate clay is ≈ two thirds that of non-carbonate clay.0 mm). depending on analytical requests and properties of the sample. loamy fine sand. 1986). coarse. and Si. the limit between sand and silt is a 0. and clay (< 2 µm). In these instances. and clay. Complete dispersion by procedure 3A1a1 may be prevented in the presence of cementing agents such calcium carbonate.05-mm particle diameter. Samples are chemically treated with hydrogen peroxide and sodium hexametaphosphate to effect dispersion. Refer to the Soil Survey Staff (1999) for additional discussion on particle-size classes.

and clay form aggregates. The aliquots are dried at 110°C and weighed. omitted. dispersed with a sodium hexametaphosphate solution. Drying such soils decreases the measured clay content. Pretreatment of these soils with acid removes the carbonates (Grossman and Millet. The determination of particle-size distribution after the removal of carbonates is used primarily for studies of soil genesis and parent material. 1986.g. The clay and fine silt fractions are determined using the suspension remaining from the wet sieving process. Gee and Or.. 1961. whereby a 10-g sample is pretreated to remove organic matter and soluble salts.g. and 36 . The determination is used for soil parent material and genesis studies. 1949). Gee and Bauder. e. poured into a centrifuge bottle. Fine-Clay Determination: The soil suspension from procedure 3A1a1a is used to determine the fine-clay fraction. This approach is appropriate in that certain procedural steps may be modified. Ultrasonic Dispersion (3A1a5): Soils that do not completely disperse with standard PSDA can be dispersed using ultrasonic dispersion (Gee and Bauder. or enhanced by the investigator. stirred. and 25-mL aliquots removed with a pipet at calculated. The process by which specific procedural steps are selected for sample analysis is based upon knowledge or intuition of certain soil properties or related to specific questions. Gee and Or. 1978). The magnitude of the effect varies with the particular soil (Maeda et al. Summary of Method Standard SSL PSDA: The standard SSL procedure for analysis of particles with <2mm diameters is the air-dry method (procedure 3A1a1a). 1986. Pretreatments coupled with ultrasonic dispersion yield maximum clay concentrations (Mikhail and Briner. This can be attributed to the cementation upon drying (Maeda et al. 1977). stand-alone methods were described for the non-routine pretreatment and dispersion techniques as well as for the analysis of particles not routinely reported. or the addition of a chemical dispersant may be compared with results from chemical dispersion (Bouyoucos. 2. 1969. some soils irreversibly harden when dried and as such moist PSDA (3A1a1b) may be used. depending on the properties of the sample and on the requested analyses. 42 (2004). The phenomenon of aggregation through oven or air-drying is an important example of irreversibility of colloidal behavior in the soil-water system (Kubota. predetermined intervals based on Stokes' law (Kilmer and Alexander. sodium dithionite-citrate solution (Mehra and Jackson. these procedures are described more as a procedural process. In this version of the SSIR No. This suspension is diluted to 1 L in a sedimentation cylinder. A pretreatment with a weak base dissolves the Si bridges and coats and increases the soil dispersion. The iron oxides are removed using bicarbonate-buffered. special studies of soil genesis and parent material. Soils with iron cementation do not readily disperse. This is a developmental procedure as no standard method has been adopted using ultrasonic dispersion. 42 (1996). Iron Removal (3A1a3): Iron and other oxides coat and bind particles of sand.. 1986.. Gee and Bauder. clay. e. The sand fraction is removed from the suspension by wet sieving and then fractionated by dry sieving. SSL PSDA Process: In the SSIR No. 1977). 1972. While a homogenized sample is more easily obtained from air-dry material than from moist material. 1960. 2002).. and mechanically shaken. 2002). Water Dispersible PSDA (3A1a6): This method provides a means of evaluating the susceptibility of a soil to water erosion. Field-Moist PSDA (3A1a1b): The standard SSL procedure for particles with <2-mm diameter is the air-dry method (3A1a1a). The degree to which a soil disperses without the oxidation of organic matter or the removal of soluble salts. This suspension is stirred. 2002). and fine silt percentages. 1975). Silica Removal (3A1a4): Soils that are cemented by Si do not completely disperse with hydrogen peroxide pretreatment and sodium hexametaphosphate. Coarse silt is the difference between 100% and the sum of the sand.Carbonate Removal (3A1a2): Soils high in carbonate content do not readily disperse. Espinoza et al. silt. Jackson. The sample is dried in the oven to obtain the initial weight. fine and/or carbonate-clay fractions. Gee and Or. 1929).

weighed. Nm as rpm. The sample is dried in the oven and weighed to obtain the initial weight. and particle diameter in microns. the remainder of procedure 3A1a1 is followed. SSL Field-moist PSDA: For soils that irreversibly harden when dried. After removal of siliceous cementing agents. the remainder of procedure 3A1a1 is followed. the remainder of procedure 3A1a1 is followed. The pressure of the evolved gas is measured.0x108η log (rs-1)) (Nm2 Dµ2 ∆ρ)-1 where: tm = Time in minutes η = Viscosity in poises r = Radius in cm from center of rotation to sampling depth (3 cm + s) s = Radius in cm from center of rotation to surface of suspension Nm = rpm (1500) Dµ = Particle diameter in microns (0. a field-moist soil may also be subjected to special pretreatment and dispersion techniques 37 . The NaOAc solution is added to sample until carbonate bubbles no longer evolve. The NaOAc solution is then washed from the sample. an air-dry soil sample is pretreated to remove organic matter and soluble salts (3A1a1a). Carbonate-Clay Determination: The residue from procedure 3A1a1a is used to determine the carbonate-clay fraction. Similar to an air-dry sample. There are additional non-routine chemical pretreatments for the removal of cementing agents that often prevent complete dispersion. the remainder of procedure 3A1a1 is followed. Ultrasonic Dispersion (3A1a5a): A soil sample is pretreated to remove organic matter and soluble salts. procedure 3A1a1 is followed. and the other sample is further processed as outlined in procedure 3A1a1a. tmin. One sample is dried in the oven to obtain the oven-dry weight. The sample is subjected to ultrasonic vibration for 5 min. sodium dithionite-citrate solution and heated until the sample color changes to a grayish color.centrifuged at 1500 rpm. tm = (63. Silica Removal (3A1a4a): Soils are pretreated with H2O2 to remove organic matter. Sodium hexametaphosphate solution is added to the sample and then made to 100-mL volume with RO water.0x108 = Combination of conversion factors for convenient units of time in minutes. Upon omitting these procedural steps. A 25-mL aliquot is withdrawn with a pipet. Water Dispersible PSDA (3A1a6a): Water dispersible particle-size distribution analysis may also be determined from a soil suspension without the removal of organic matter or soluble salts. The time of centrifugation is determined from the following equation modified from Stokes' law (Jackson. moist soil to be pretreated to remove organic matter and soluble salts. Pretreatment and Dispersion Techniques: In the standard PSDA. and the percentage of fine clay is calculated based on the total sample weight. After removal of iron oxides. 1969). The pressure is related linearly to the CO2 content in the carbonates. or without the use of a chemical dispersant. These pretreatments may be requested by the project coordinator as follows: Carbonate Removal (3A1a2a): Carbonates are destroyed with a 1 N NaOAc solution buffered to pH 5. This residue is treated with acid in a closed system. Soils with Si cementation or coatings are pretreated with a weak NaOH solution overnight. Iron Removal (3A1a3a): Soil samples are pretreated with H2O2 to remove organic matter. The aliquot is dried in the oven.2 µm) ∆ρ = Difference in specific gravity between solvated particles and suspension liquid 63. moist particlesize analysis (procedure 3A1a1b) may be requested by project coordinator. Iron oxides are removed with bicarbonate-buffered. This procedure requires two 10-g samples of <2-mm. After dispersion with the ultrasonic probe. Dµ. After destruction of carbonates. The suspension is flocculated with saturated NaCl solution and filtered to remove soluble salts. A manometer is used to measure the pressure.

Interferences Standard SSL PSDA: The sedimentation equation that is used to measure the settling rates of particles of different sizes is as follows: ν = 2r2g(ρs-ρl)/(9η) where: ν = Velocity of fall r = Particle radius g = Acceleration due to gravity ρs = Particle density ρl = Liquid density η = Fluid viscosity This formula results from an application of Stokes' law and is referred to as Stokes' law. Carbonate-Clay Determination: The carbonate-clay analysis is semi-quantitative. Particles are smooth and spherical.(3A1a2-6b). The particle density (ρp) of the fine clay is assumed to be 2. In addition to Ca. The withdrawal rate with pipet should be constant. This method measures all forms of carbonates. There is no interaction between individual particles in the solution (Gee and Bauder. 4. a true measurement of fractions is uncertain (Drosdoff and Miles. It is assumed that all of the carbonates are converted to CO2. the radius of the particle is considered an equivalent rather than an actual radius. the carbonates of Mg. Partial flocculation may occur in some soils if excess H2O2 is not removed from the soil after its use in organic matter oxidation. Gypsum is removed by stirring and washing the soil with reverse osmosis water. and K also react with the acid.5 g cc-1 (Jackson. This procedure is effective if the soil contains <25% gypsum. 3.65 g cc-1. When sealing the vessel. Since exfoliation occurs in these soils. Since soil particles are not smooth and spherical. Both the air-dry and moist PSDA data are determined as percent of the <2-mm fraction on an oven-dry basis. Fine-Clay Determination: In the fine-clay determination. 3. The internal pressure must be equalized with the atmosphere. Settling and resistance are entirely due to the viscosity of the fluid. 1938). which causes disturbance of solution. Analytical interferences may be caused by temperature changes within the reaction vessel. Approximately 3 to 5 s are 38 . 1969). the analyst should not hold onto the vessel any longer than necessary to tighten the cap. The suspension temperature must be used to enter the correct liquid viscosity in the equation. Na. Assumptions used in applying Stokes' law to soil sedimentation measurements are as follows: 1. 2. Treatment of micaceous soils with H2O2 causes exfoliation of the mica plates and a matting of particles when dried in the oven. the distance from the center of rotation to the surface of the suspension must be constant for each centrifuge bottle. In this method. Gypsum interferes with PSDA by causing flocculation of particles. 2002). Gee and Or. particle density is assumed to be 2. Position the bottle under pipet without sudden movement of the centrifuge rotor. Terminal velocity is attained as soon as settling begins. The analyst should not touch the glass of the vessel when reading the pressure. 1986.

. aprons. perforated disk fastened to a rod 5. Mix acids in ventilated fume hoods. (Kilmer and Mullins. these special techniques in themselves may interfere with PSDA as follows: Carbonate Removal (3A1a2): The removal of carbonates with 1 N NaOAc (pH 5) results in sample acidification. The presence of cementing agents such as carbonates.13 Adjustable pipet rack (Shaw. The samples ranged from sandy to clayey soils. 1986). Perform the transfer of acid to gelatin capsules near a sink in case of leakage or spills. as they develop leaks after extensive use. Iron Removal (3A1a3): If the temperature of the water bath exceeds 80° C during Fe removal.9 Thermometer.15 Polyurethane foam. No standard procedures have been adopted using ultrasonic dispersion. The analyst should replace septa and O rings at regular intervals. 1960).1 Fleakers. 39 . Heat samples in ventilated fume hoods for removal of organic matter or cementing agents in ventilation hoods.12 Hand stirrer. Use sodium bicarbonate and water to neutralize and dilute spilled acids. 1980).6 Oven.14 Lowy pipets.1 N NaOH on the clay fraction and particle-size distribution are unknown. Opposite centrifuge bottles need to be balanced.8 Vacuum.1-3) 5.3 µm absolute retention (source currently unavailable) 5. MI 5.2 Ceramic filter candles. 1954) 5. 1932. with overflow bulb 5. Pretreatment and Dispersion Techniques: The PSDA results are dependent on the pretreatments used to disperse the soil. In these cases.4 Mechanical shaker.. However. 100°C 5. or safety glasses) when handling acid and H2O2. and gloves) and eye protection (face shields.required to equalize the internal pressure of the bottle when piercing the septa with a needle. 4. Users should be familiar with centrifuge operation. Fig. Fe. 110°C 5.7 Hot plate. tared to 1 mg 5. Centrifuge should not be opened until centrifuge rotor has completely stopped 5. This pretreatment can destroy primary mineral grains in the clay fraction (El-Swaify. Ann Arbor. 25 mL. Field-Moist PSDA: Soils that irreversibly harden when dried are difficult to disperse. 1 L. pipe insulation that fits snugly around cylinder. The PSDA for these soils can be determined on moist samples (procedure 3A1a1b) upon the request of the project coordinator. 1 ½ in strokes. Silica Removal (3A1a4): The effects of Si removal with 0.10 Desiccator 5. and hydroxides of Fe and Al. and Si often prevent complete dispersion. 0 to 150°C 5. 120 oscillations min-1. Saly (1967) reported that ultrasonic vibration did not cause the destruction of the clay crystalline lattice or the breakdown of primary grains. Equipment 5. 5. special pretreatment and dispersion procedures may be performed upon request on either an air-dry or field-moist sample. This pretreatment can destroy the primary mineral structure of clay (Gee and Bauder. Safety Wear protective clothing (coats. 300 mL. The cementing agents represented humus. sleeve guards.3 Rack to hold ceramic filter candle and sample container. carbonates.8 bars (80kPa) 5. white line fused onto glass at 1-L mark 5. However. elemental S can precipitate (Mehra and Jackson. Eberbach Corp. goggles. Eberbach 6000. Handle heated samples with leather gloves. Ultrasonic Dispersion (3A1a5): Ultrasonic dispersion has been reported to destroy primary soil particles. horizontal. 0.11 Motor driven stirrer. Watson (1971) summarized studies that reported the destruction of biotite and breakdown of microaggregates by ultrasonic dispersion.5 Cylinders.

International Equip. ±0. series and Tyler Screen Scale equivalent designations are as follows: Sand Size VCS CS MS FS VFS Opening (mm) 1.1 mg 5.0-mg sensitivity 5.94 g of Na2CO3 in 1 L of RO water.2 x 38.27 Centrifuge. 50. 90 mL.. 90 mL 5. 5 mL 5. reagent grade 6.2 Hydrogen peroxide (H2O2). 6.24 Watch glass.28 Centrifuge bottle. PCL-200A/C Series. O-ring seal 5.33 Machined PVC caps for threaded 90-mL weighing bottles.16 Sieve shaker with 12. Co. 5.30 Manometer.3 Sodium hexametaphosphate ((NaPO3)6).7-mm (1/2 in) vertical and lateral movement at 500 oscillations min1 . Stamford. Place in machined cap. 949 rotor head. No.8 Hydrochloric acid (HCl).31 Gelatin capsules.7 Calcium sulfate (anhydrous) or equivalent desiccant 6. 3.2-cm (1 1/4 in) diameter with 1. tared to 1 mg 5. with lip 5.26 Set of 76-mm (3 in) sieves.25 Evaporating dish. 23 gauge 5.23 Electronic balance. ASTM Type III grade of reagent water 6.6 Ethyl alcohol 6.25 0.S. square weave phosphor bronze wire cloth except 300 mesh which is twilled weave.5 0.10-mg sensitivity 5. aluminum 5. 19-mm (3/4 in) horn. 90 mL. 160-mm diameter.S. 300 watts 6. Dilute 1 L of concentrated HCl with 1 L of RO water 6. Omega Engineering.18 Weighing bottles. CT. 7.and 65-mm diameters 5. International No. 30 to 35% 6.105 0.4 Sodium carbonate (Na2CO3). 20 kHz.19 Weighing bottles. tared to 0.9-mm (5/16 in) diameter.6 g Na2CO3 in RO water and make to 1 L (10 mg CaCO3 40 . 25. hand-held gauge and differential pressure. 5. 18 35 60 140 300 Tyler Mesh Size 16 32 60 150 300 5. porcelain.34 O-rings.35 Septa. with No. 11.36 Hypodermic needle. See Section 7. Dissolve 35.12 for standardization of sodium hexametaphosphate solution.7 g of (NaPO3)6 and 7.4 mm (1 in). rubber. Boston. Dissolve 10. MA 5.5 Sodium hexametaphosphate solution.047 U. 5.29 Torsion balance 5.1 mm (1/8 x 1 1/2 in) 5. 500 mL 5. 3. Accommodates a nest of 76-mm (3 in) sieves.1 Reverse osmosis (RO) water.1-cm (7/16 in) diameter hole drilled in center.32 Threaded weighing bottles.21 Timer or clock with second hand 5.20 Drying dishes. tared to 1 mg 5.37 Ultrasonic probe. reagent grade 6. U. 90 mL. ±1. 6 N.9 Sodium carbonate (Na2CO3) reagent.5. with screw caps. 31-mm height.0 0. Reagents 6. technical grade.17 Weighing bottles.22 Electronic balance.

Heat the sample for an additional 45 min to decompose excess H2O2. Insert a filter candle. Dissolve 4 g NaOH pellets in 1 L of RO water. 7. connect to the vacuum trap assembly with tubing. 1 M NaHCO3 (84 g L-1) 6. 7. transfer the sample to a larger beaker.1 If the standard air-dry PSDA procedure for the <2-mm fraction is requested. 7. 6. proceed to procedure 3A1a1a. Wash the sample four 41 . air-dry soil to nearest mg on an electronic balance and place into a numbered. Make to 5-L volume with RO water.8 Place the sample on the filter rack. 7.13 Sodium dithionite (Na2S2O4 . or (d) reduce the amount of H2O2 to sample.hydrosulphite) 6.10 1 N sodium acetate (NaOAc) solution. buffered to pH 5.2 If PSDA is requested on a field-moist sample. proceed to procedure 3A1a1b. or water dispersible) are requested on air-dry soil samples. 0. or Si. Dissolve 680 g of NaOAc in 4 L of RO water. (b) remove the sample from the hot plate to slow the reaction. Add 150 mL of RO water.6 Add ≈ 50 mL of RO water and 5 to 7. Procedures Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) 7. proceed to procedures 3A1a2-6b.7 Place the sample on a hot plate and heat to 90°C. Fe. Cover the soil sample with a 50-mm watch glass. and turn on the vacuum. 7.12 Sodium bicarbonate buffer solution. or water dispersible) are requested on field-moist soil samples. respectively.4 If special pretreatment and dispersion techniques (removal of carbonate. A quality control sample is included in each batch (<24 samples). 7.5 Weigh 10 g of <2-mm. Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) Standard Pretreatments and Dispersion (3A1a1) Air-Dry (3A1a1a) 7.6. 0.5-mL increments of H2O2 at 30-min intervals. 7. (c) transfer sample to a 1000-mL beaker. 360 g L-1) 6. Record any unusual sample reactions. Aspirate until liquid is removed and only slightly dampened sample remains. fleaker.3 M Na3C6H5O7·2H2O (88. If oxidation is incomplete.14 Saturated NaCl solution (solubility at 20°C. ultrasonic dispersion. If the reaction is violent.15 Sodium hydroxide solution (NaOH).3 If special pretreatment and dispersion techniques (removal of carbonate. proceed to procedures 3A1a2-6a. Fe. Wash and tare these fleakers once every two months. Add ≈ 250 mL of acetic acid. tared 300-mL. Add four 5 to 7.5 mL of H2O2 to the soil sample at ambient temperature. or Si. ultrasonic dispersion. do one or any combination of the following: (a) add small increments of ethyl alcohol to the sample.11 Sodium citrate solution. respectively. Allow initial oxidation of organic matter to complete and then place sample on hot plate. add additional H2O2 until organic matter oxidation is complete.1 N.4 g L-1) 6. If the froth from the reaction exceeds the capacity of the fleaker.

Record the weight of each separate sand fraction (SWi) to the nearest mg. Collect the silt and clay in the 1-L cylinder. 0. Wash and rub all particles from the fleaker into the sieve. 7. to each sample. 0. 10. Prepare a RO water blank to measure temperature fluctuations. 10. Avoid using jets of water in washing the sample. Continue to wash until the suspension volume in the cylinder is ≈ 800 mL. If the sample contains >5% gypsum.047-mm) sieve mounted on a ring stand. 9.3. Add duplicate aliquots (8. Store capsules in the labeled vial. 7.1.12 A sodium hexametaphosphate standardization is performed with each new batch of solution. 7.6. 42 . 90-mL weighing bottles. Add ≈ 175 mL of RO water. and 0.3-cm vertical and lateral movements and oscillates at 500 strokes min-1. 11. Oven-dry aliquots overnight and record dry residue weight of sodium hexametaphosphate. Place a funnel below the sieve and a 1-L cylinder below the funnel.0. refer to Section 7.additional times with ≈ 150 mL of RO water.15 Transfer the dried sand to a nest of sieves that has a top-to-bottom order of 1. place the sample in a 1000-mL beaker and stir the sample with a magnetic stirrer for 5 min then wash 5 times with ≈ 750 mL of RO water each time to remove soluble gypsum. and cool to ambient temperature. Finger-rubbing of sample may be required during transfer to speed washing of sample.0. Rinse all <20-µm particles into the cylinder. then the following additional washings may be used.5.3. Remove the sample from the oven.9 Place sample in oven.0 mL) of sodium hexametaphosphate solution to numbered tared. Place pipe insulation around sample and blank cylinders to prevent rapid changes in temperatures. 7.4408 g of sodium hexametaphosphate into each sample. it may be necessary to occasionally apply backpressure to filter candle and remove build-up of soil which inhibits aspiration. 10. 7.4408 g of sodium hexametaphosphate.0. Let stand until sample is completely moistened by sodium hexametaphosphate. If the sample contains 1 to 5% gypsum.10 Record the total weight (TW) of the sample to the nearest mg.047 mm.6. stir the sample with a magnetic stirrer for 5 min and wash 5 times with ≈ 250 mL of RO water each time. 0. Determine the exact volume of sodium hexametaphosphate to add to each sample by regressing the volume of sodium hexametaphosphate against the dry residue weight of sodium hexametaphosphate and then by predicting the volume needed to dispense 0.11 Add the exact volume of sodium hexametaphosphate solution (≈ 10 mL). Wash sand dishes after every use. equivalent to 0. Use only designated weighing bottles for standardization. If optical analysis is requested.5. During aspiration. 7. 7. Shake the sand for 3 min on a shaker that has 1. place the very fine sand and fine sand fractions in gelatin capsules and the remaining sand fractions in a labeled vial. If the sample contains gypsum and flocculates.12. Sand and some of the coarse silt remain on the sieve. Fill the cylinder to 1 L and cover with a 65-mm watch glass. place in a desiccator. 9. Wash the sand into an evaporation dish and dry the sand at 110°C overnight. Wash and tare these bottles after each standardization. Subtract the weight of the sodium hexametaphosphate (DW) that is contained in the extracted aliquot from the silt and clay weights to calculate silt and clay percentages.13 Place the sample in a horizontal shaker set at 120 oscillations min-1 and shake for 15 h (overnight). To determine the exact volume of sodium hexametaphosphate to add to each sample. Stir the sample with filter candle to ensure all soil particles will be rinsed.14 Remove the sample from the shaker and pour through a 300-mesh (0. Dry the sample overnight at 110°C.25. 9. Allow the cylinder to stand overnight to equilibrate the suspension with the room temperature.

Optical Mineralogy 7. The marked line on each bottle is 13 cm which is the distance from the center of rotation to the surface of the suspension. 7. the procedural aspects of the standard air-dry PSDA for the <2-mm fraction are complete. 7. 1932). and save in the drying dish for optical mineralogy. which is dominantly 20 to 50µm. decant the suspension and transfer the sediment to a 400-mL beaker. 25-mL pipet. 43 . Refill the beaker to 5. If determination of carbonate is required. vibrationless table and stir with a hand stirrer in an up-and-down motion for 30 s. save the sediment and proceed on with the section on optical mineralogy. turn on the vacuum. weighing bottle with the aliquot. Wash and tare after every use. and withdraw an aliquot at the calculated time (Table 1).2 µm) 7. If fine-clay and/or carbonate clay are requested. Use the average of T1 and T2 and adjust the pipet depth in the suspension as indicated in Table 2.19 If optical mineralogy is requested. 7.20 Stir the silt and clay suspension with mechanical stirrer for 5 min. Record temperature (T1) of blank.16 Determine the percentage of fine silt and clay gravimetrically by removing an aliquot from the suspension in the 1-L cylinder with a Lowy. Stir again.21 Pour the suspension into a centrifuge bottle and fill to the line marked on the bottle. Rinse the pipet twice with RO water and dispense into the tared. 5. air-dry. Timing is started upon completion of the stirring. Wash and tare after every fourth use. Repeat the procedure described for the <20-µm fraction. Dispense the aliquot into a tared and numbered. Transfer the sediment. Place loads on a torsion balance and add water to the lighter bucket until both loads weigh the same. which consist of centrifuge bottle. Use the 90-mL. Dry the aliquots at 110°C overnight and cool in a desiccator that contains calcium sulfate or an equivalent desiccant. 7. allow to settle for 2 min. Regulate the vacuum such that the pipet fills in ≈12 s. use weighing bottle with screw threads.5-cm height. For the <20-µm fraction.5.5 h. Stir the sediment and allow to settle for 5 min. and then decant. trunnion carrier and bucket. Repeat the filling and the stirring. Stopper and shake well to mix the suspension. weighing bottles for the <2-µm aliquots. Record the delivery volume (DV) and use the value to calculate the results. round-bottomed.5.1mg. Record temperature (T2) of blank. Periodically.24 Centrifuge at 1500 rpm. Record the weight of the residue (RW) to the nearest 0. Record the time that stirring is stopped. . 7. gravimetrically calibrate the delivery volume of the pipet by weighing the amount of RO water dispensed from the pipet. 5. to a labeled drying dish. Fill the beaker to a 5. allow to settle for 3 min. proceed on with the sections on these analyses.23 Read the temperature of the suspension.5-cm height. or 6. weighing bottles for the <20-µm aliquots. and then decant until top half of suspension is clear. 7. Stir with the hand stirrer in an up-and-down motion for 30 s and allow the suspension to settle for 15 min. square-bottomed. For the <2-µm fraction.22 Balance opposite centrifuge loads. slowly lower the closed pipet to a 10-cm depth in the suspension. Discard the supernatant. Mount the pipet on an adjustable pipet rack (Shaw. Remove sample from mechanical stirrer and place on table.7. Wash with ethanol. Stir the silt and clay suspension with mechanical stirrer for at least 5 min. fine-clay and/or carbonate clay determinations are not requested. 90-mL weighing bottle.18 If optical mineralogy. Fine Clay Determination (<0. pipet after a time of 4.17 Use the 90-mL. Place the cylinder on a stable. If optical mineralogy is requested.

00890 0.01028 0.501 1.00978 0.00798 Delta-Density ∆ρ 1.9 32.00934 0.503 1.503 1.4 30.502 1.0 36.00816 0.2 35.9 37.502 1.502 1.9 37. lower the pipet to a 3-cm depth in the suspension.00913 0.504 Time Min 39.24.00851 0. 3A1a6a and 3A1a6b.503 1.502 1.01004 0.504 1.4 where: s = 15 cm r = 18 cm Nm = 1500 rpm ρp = 2.503 1.0 38.504 Time Min 38.00957 0.00853 0.1 29. Avoid turbulence.01002 0.5 g cc-1 7.5 33.4 7.00872 0. vary the centrifuge time according to the temperature as follows: Temp (°C) 18 19 20 21 22 23 24 25 26 27 28 29 30 Viscosity η 0.502 1.503 1.00892 0.8 32.7 32.501 1.01053 0.00911 0.00815 0.502 1.0 29.1 35.1 For procedures3A1a1-5a and 3A1a1-5b.00980 0.504 1.2 31. vary the centrifuge time according to the temperature as follows: Temp (°C) 18 19 20 21 22 23 24 25 26 27 28 29 30 Viscosity η 0.502 1.25 After centrifuging.6 32.502 1.503 1. Withdraw a 25-mL aliquot at a rate of ≈ 12 s.00871 0.00834 0.4 33.01055 0.1 31.503 1.503 1.00955 0.7. Transfer the aliquot to a weighing bottle 44 .00833 0.504 1.00799 Delta-Density ∆ρ 1.2 34.2 For procedures.4 30.7 30.8 30.0 37.501 1.24.01029 0.502 1.502 1.00933 0.1 36.3 34.

Measure the pressure inside the weighing bottle. Place the capsule into the glass bottle and immediately cap the bottle.1 mg. Approximately 3 to 5 s are required to equalize the internal pressure of the bottle. discard the capsule. In each analysis batch. 45 . Dry the standard samples in the oven overnight at 110°C. Dispense 3 mL of 6 N HCl into a gelatin capsule and place the top on the capsule. round-bottomed. Wash and tare after every use. Calibrate by placing replicated aliquots of 0.. Place the capsule into the glass bottle and immediately cap the bottle. Remove sample from oven.0 mL of the Na2CO3 reagent into numbered. lubricate the lip of the 90-mL. tared. Carbonate Clay (<2 µm): Manometer Calibration 7. Carbonate Clay: Analysis 7. Avoid changing the temperature of the container by only handling the cap. i. Allow 3 to 5 s for internal pressure in bottle to equalize. 7. discard the capsule.1mg. Dry overnight at 110°C. Release pressure in the bottle by piercing the septa with a hypodermic needle which is not connected to the manometer. place in desiccator with calcium sulfate or equivalent desiccant. place in desiccator and cool to ambient temperature.2µm aliquots. Allow sample to stand for at least 30 min. the dependent variable is the Na2CO3 weights (regressed or predicted values) and the independent variable is the corresponding manometer readings. Use the 90-mL. and cool to ambient temperature. 90-mL weighing bottles. 7. Dispense 3 mL of 6 N HCl into a gelatin capsule and place the top on the capsule. square-bottomed. 7. weighing bottle that contains the Na2CO3 with a thin film of glycerine.e.29 Calibrate the manometer quarterly or whenever equipment changes. weighing bottle that contains the <2-µm residue. Wash and tare after every fourth use. Remove samples from oven. If HCl leaks from the capsule.31 After the gelatin capsule has dissolved (several minutes). 7.36 With a thin film of glycerine. If HCl leaks from the capsule. Record the manometer readings (mm Hg) to the nearest whole number. 7. weighing bottles for the <0.30 Lubricate the lip of the 90-mL.27 Weigh residue weight (RW) to nearest 0. include an empty weighing bottle as a blank.28 Use the 90-mL. Record the weight of the standard samples to nearest 0. 7. 7. slowly tip the bottle and rotate it to saturate the standard sample adhering to the sides of the bottle. Insert the hypodermic needle in the septa stopper which is connected to the transducer. 7.32 Adjust the manometer to zero before taking measurements.34 Determine the presence of carbonates in <2-mm soil by placing soil on a spot plate and adding two or three drops of 1 N HCl. The rate of CO2 evolution indicates the relative amount of carbonates (1B1b2b5). Release any pressure in the bottle by piercing the septa with a hypodermic needle that is not connected to the manometer.33 Calculate the linear regression equation.7.0 to 20.35 If the soil contains more than a “slight” amount of carbonates. determine the amount of carbonate clay in the <2-µm dry residue.26 Place weighing bottle with aliquot in oven. weighing bottles for the <2-µm aliquots and carbonate determination.

Heat the sample for an additional 45 min to decompose excess H2O2.37 After the gelatin capsule has dissolved (several minutes).42 Place the sample on the hot plate and heat to ≈ 90°C until bubbles are no longer evident. weigh 20 g of soil. Continue to decant. The speed of dissolution can be increased by lowering the pH of the 1 N NaOAc solution (Rabenhorst and Wilding. Begin readings with the blank (BR). and cover with a watch glass.5 g of Fe2O3 can be dissolved in 40 mL of the citrate solution.44 A maximum of ≈ 0. air-dry soil sample so that any one fleaker does not contain more than 0. Handle only the cap to avoid changing the temperature of the container. Proceed to procedure 3A1a1a for remaining PSDA procedural steps. If the reaction is violent. 7. slowly tip the bottle and rotate it to saturate the clay adhering to the sides of the bottle. Allow sample to stand for at least 30 min. 7. Allow the sample to stand overnight. If a reaction occurs. and heat until all the carbonates are removed. Total sample weight after dissolution should be ≈ 10 g. Do not boil. Split the sample into different fleakers if necessary.5 g of Fe2O3.g.43 When no more carbonate bubbles are observed. e. Heating accelerates reaction. 1984). fleaker. transfer the sample to a larger beaker. 7.41 Add ≈ 200 mL of the 1 N NaOAc solution to the sample. and then place sample on hot plate. add NaOAc solution. Cover the soil sample with a 50-mm watch glass. Insert the hypodermic needle in septa stopper which is connected to the transducer. Place the <2-mm. 300-mL fleaker. air-dry carbonate-free soil sample.46 Place the sample on a hot plate and heat to 90°C. mix with a stirring rod. Adjust the weight of the <2-mm. 7. Rinse once with 200 mL of RO water. Allow initial oxidation of organic matter to complete. Decant the solution and add more 1 N NaOAc solution. add 46 . Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) Carbonate Removal (3A1a2) Air-Dry (3A1a2a) 7.45 Add ≈ 50 mL of RO water and 5 mL of H2O2 to the soil sample at ambient temperature. tared. Measure the pressure inside the weighing bottle and record the manometer readings (MR) to the nearest whole number (mm Hg).39 Compare the sample readings with those of a standard curve prepared by measuring CO2 evolved from a series of Na2CO3 aliquots with a range 0 to 200 mg. 7.38 Adjust the manometer to zero before taking measurements. if the sample contains 50% carbonates. repeat the heating procedure. Add 5-mL increments of H2O2 at 45min intervals until oxidation has completed or until 30 mL of H2O2 have been added. 7.40 Weigh sufficient sample to yield 10 g of <2-mm. 7. Place the sample into a tared. insert the ceramic filter candle into the solution. Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) Iron Removal (3A1a3) Air-Dry (3A1a3a) 7. air-dry sample into a 300-mL.7. Apply vacuum and candle the sample to dryness. If the froth from the reaction exceeds the capacity of the fleaker. labeled.

7. repeat the dissolution treatment two more times. Add 1 g of sodium dithionite powder with a calibrated scoop. 300-mL.53 Soak the sample overnight in 100 mL of 0. Wash and tare these fleakers once every two months.55 Add ≈ 50 mL of RO water and 7.5 g of Fe2O3. fleaker. For samples with more than 0. Stir constantly with a glass rod for 1 min and then occasionally for 15 min. Heat the sample for an additional 45 min to decompose excess H2O2.1 N NaOH. Cover the soil sample with a 50-mm watch glass. 7. 7. tared fleaker. but do not exceed 80°C.52 Place the sample on a hot plate and heat to 90°C. If the froth from the reaction exceeds the capacity of the fleaker.47 Add 40 mL of the citrate solution and 5 mL of the sodium bicarbonate. repeat the dissolution treatment. 7. Add 5-mL increments of H2O2 at 45min intervals until oxidation has completed or until 30 mL of H2O2 have been added. 47 . Combine the split samples into fewer fleakers. Heat to 80°C in a water bath.48 Centrifuge or candle the sample to remove the dissolved Fe2O3. Allow initial oxidation of organic matter to complete and then place sample on hot plate. Add 10 mL of saturated NaCl solution and mix. Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) Silica Removal (3A1a4) Air-Dry (3A1a4a) 7. proceed to procedure 3A1a1a for remaining PSDA procedural steps. Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) Ultrasonic Dispersion (3A1a5) Air-Dry (3A1a5a) 7. Upon completion of Fe removal. add small increments of ethyl alcohol to the sample or remove the sample from the hot plate to slow the reaction. air-dry soil to nearest mg on an electronic balance and place in a 300-mL. 7. 7.54 Weigh 10 g of <2-mm. proceed to procedure 3A1a1a for remaining PSDA procedural steps.small increments of ethyl alcohol to the sample or remove the sample from the hot plate to slow the reaction. A quality control sample is included in each batch (<24 samples). Upon removal of siliceous cementing agents.49 If the sample contains less than 0. Cover the soil sample with 50-mm watch glass.5 g of Fe2O3. transfer the sample to a larger beaker.5 mL of H2O2 to the soil sample at ambient temperature. If the reaction is violent.51 Add ≈ 50 mL of RO water and 5 mL of H2O2 to soil sample at ambient temperature. and then place sample on hot plate. transfer the sample to a larger beaker. air-dry soil to nearest mg on an electronic balance and place into a numbered. 7. Allow initial oxidation of organic matter to complete. If the froth from the reaction exceeds the capacity of the fleaker. tared.50 Weigh 10 g of <2-mm.

Insert a filter candle. (c) transfer sample to a 1000-mL beaker. Press start button.60 Add ≈ 100 mL of RO water and the exact volume of sodium hexametaphosphate solution (≈ 10 mL). Place pipe insulation around sample and 48 . If the sample contains gypsum and flocculates. or (d) reduce the amount of H2O2 to sample. Subtract the weight of the sodium hexametaphosphate (DW) that is contained in the extracted aliquot from the silt and clay weights to calculate silt and clay percentages.7. Use only designated weighing bottles for standardization. Sand and some of the coarse silt remain on the sieve. Add 150 mL of RO water.56 Place the sample on a hot plate and heat to 90°C. 7.61 A sodium hexametaphosphate standardization is performed with each new batch of solution.3. equivalent to 0. If the reaction is violent. Fill the cylinder to 1 L and cover with a 65-mm watch glass. 9. 7. place in a desiccator. Avoid using jets of water in washing the sample.59 Record the total weight (TW) of the sample to the nearest mg. 7. Remove the sample from the oven. add ≈ 75 mL RO water and pour the suspension through a 300-mesh (0. 11.0 mL) of sodium hexametaphosphate solution to numbered tared.6. Set timer to 5 min. Rinse all <20-µm particles into the cylinder. 10.4408 g of sodium hexametaphosphate into each sample.3. Wash and tare these bottles after each standardization. If the sample contains >5% gypsum.63 After ultrasonic dispersion. Collect the silt and clay in the 1-L cylinder. 9. To determine the exact volume of sodium hexametaphosphate to add to each sample. and cool to ambient temperature.4408 g of sodium hexametaphosphate. Oven-dry aliquots overnight and record dry residue weight of sodium hexametaphosphate. If oxidation is incomplete. add additional H2O2 until organic matter oxidation is complete. Between samples. During aspiration. Record any unusual sample reactions. Record any unusual sample reactions. Wash and rub all particles from the fleaker into the sieve. connect to the vacuum trap assembly with tubing. 7. Dry the sample overnight at 110°C.5.6. Ensure the power supply is properly tuned. 10. 7. 9. 7. If the sample contains 1 to 5% gypsum. do one or any combination of the following: (a) add small increments of ethyl alcohol to the sample.0. Aspirate until liquid is removed and only slightly dampened sample remains. 7. Adjust output control as required.0. refer to Section 7.047-mm) sieve mounted on a ring stand. Add duplicate aliquots (8. Determine the exact volume of sodium hexametaphosphate to add to each sample by regressing the volume of sodium hexametaphosphate against the dry residue weight of sodium hexametaphosphate and then by predicting the volume needed to dispense 0.62 Disperse the suspension with ultrasonic vibrations. it may be necessary to occasionally apply backpressure to filter candle and remove build-up of soil which inhibits aspiration. stir the sample with a magnetic stirrer for 5 min and wash 5 times with ≈ 250 mL of RO water each time. clean the probe by placing it in water or alcohol and energizing it for a few seconds.57 Place the sample on the filter rack. then the following additional washings may be used. Immerse the probe in the suspension to a 3-cm depth. Finger-rubbing of sample may be required during transfer to speed washing of sample. to sample. Consult the instruction manual. 10. 90-mL weighing bottles. Stir the sample with filter candle to ensure all soil particles will be rinsed. Continue to wash until the suspension volume in the cylinder is ≈ 800 mL. Wash the sample four additional times with ≈ 150 mL of RO water. place the sample in a 1000-mL beaker and stir the sample with a magnetic stirrer for 5 min then wash 5 times with ≈ 750 mL of RO water each time to remove soluble gypsum. Heat the sample for an additional 45 min to decompose excess H2O2. and turn on the vacuum. (b) remove the sample from the hot plate to slow the reaction.58 Place sample in oven. Add four 5 to 7.61. Place a funnel below the sieve and a 1-L cylinder below the funnel.5-mL increments of H2O2 at 30-min intervals.

Fill the cylinder to 1 L and cover with a 65-mm watch glass.69 Transfer the dried sand to a nest of sieves that has a top-to-bottom order of 1. turn on the vacuum. Wash the sand into an evaporation dish and dry the sand at 110°C overnight. 0. Remove the sample from the oven. Dispense the aliquot into a tared and numbered. Record temperature (T1) of blank. and cool to ambient temperature. Prepare a RO water blank to measure temperature fluctuations.047 mm. Place a funnel below the sieve and a 1-L cylinder below the funnel. Allow the cylinder to stand overnight to equilibrate the suspension with the room temperature. place in a desiccator.047-mm) sieve mounted on a ring stand. Record the weight of each separate sand fraction (SWi) to the nearest mg.25. Proceed to procedure 3A1a1a for remaining PSDA procedural steps. vibrationless table and stir with a hand stirrer in an up-and-down motion for 30 s. Collect the silt and clay in the 1-L cylinder. Wash and tare these fleakers once every two months. slowly lower the closed pipet to a 10-cm depth in the suspension.67 Add ≈ 175 mL of RO water to sample.0. 7. 7.blank cylinders to prevent rapid changes in temperatures.65 Dry the sample in an oven at 110°C overnight. place the very fine sand and fine sand fractions in gelatin capsules and the remaining sand fractions in a labeled vial.5. If optical analysis is requested. Record the delivery volume (DV) and use the value to calculate the results. open the pipet. Continue to wash until the suspension volume in the cylinder is ≈ 800 mL. 90-mL weighing bottle. tared 300-mL. 7. Allow the cylinder to stand overnight to equilibrate the suspension with the room temperature. Timing is started upon completion of the stirring. 7. A quality control sample is included in each batch (<24 samples). 7.1. fleaker. and withdraw an aliquot at the calculated time (Table 3).3-cm vertical and lateral movements and oscillates at 500 strokes min-1.68 Remove the sample from the shaker and pour through a 300-mesh (0. Prepare a RO water blank to measure temperature fluctuations. Regulate the vacuum such that the pipet fills in ≈ 12 s. Wash the sand into an evaporation dish and dry the sand at 110°C overnight.70 Determine the percentage of fine silt and clay gravimetrically by removing an aliquot from the suspension in the 1-L cylinder with a Lowy. Wash sand dishes after every use. gravimetrically calibrate the delivery volume of the pipet by weighing the amount of RO water dispensed from the pipet. 7. Store capsules in the labeled vial. Place the cylinder on a stable. Place the sample in a horizontal shaker set at 120 oscillations min-1 and shake for 15 h (overnight). 1932). Wash and rub all particles from the fleaker into the sieve. Stir the silt and clay suspension with mechanical stirrer for at least 5 min.66 Record the total weight (TW) of the sample to the nearest mg. Rinse all <20-µm particles into the cylinder. 0. Shake the sand for 3 min on a shaker that has 1. 25-mL pipet. and 0. Sand and some of the coarse silt remain on the sieve.64 Weigh 10 g of <2-mm. Finger-rubbing of sample may be required during transfer to speed washing of sample. Mount the pipet on an adjustable pipet rack (Shaw. For the <20-µm fraction. Avoid using jets of water in washing the sample. 0. Place pipe insulation around sample and blank cylinders to prevent rapid changes in temperatures. Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) Water Dispersion (3A1a6) Air-Dry (3A1a6a) 7. air-dry soil to nearest mg on an electronic balance and place into a numbered. Record the time that stirring is stopped. Rinse the pipet twice with RO water and dispense 49 . Periodically.

moist soil to achieve two ≈ 10-g samples of air-dry soil. 7. Record the residue weight (RW) to the nearest 0. or (d) reduce the amount of H2O2 to sample. 5. Allow initial oxidation of organic matter to complete and then place sample on hot plate. Cover the soil samples with a 50-mm watch glass.into the tared. Record temperature (T2) of blank.75 Place one of the samples in the oven and dry overnight at 110°C. Wash the sample four additional times with ≈ 150 mL of RO water. Dry the aliquots at 110°C overnight and cool in a desiccator that contains calcium sulfate or an equivalent desiccant. and cool to ambient temperature. weighing bottle with aliquot. or 6. transfer the sample to a larger beaker. place the sample in a 1000-mL beaker and stir the sample with a magnetic stirrer for 5 min then wash 5 times with ≈ 750 mL of RO water each time to remove soluble gypsum. If the sample contains >5% gypsum. (c) transfer sample to a 1000-mL beaker. If the sample contains 1 to 5% gypsum. Wash and tare these fleakers once every two months. If the froth from the reaction exceeds the capacity of the fleaker.73 Place the samples on a hot plate and heat to 90°C. Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) Standard Pretreatments and Dispersion (3A1a1) Field-Moist (3A1a1b) 7.5. oven-dry sample to the nearest mg. do one or any combination of the following: (a) add small increments of ethyl alcohol to the sample. Repeat the procedure described for the <20-µm fraction. Record any unusual sample reactions. Proceed to procedure 3A1a1a and use the H2O2-treated sample that was not dried in oven for remaining PSDA procedural steps.1 mg. 50 .74 Place the sample on the filter rack. 7. 7. If the reaction is violent. If oxidation is incomplete.71 Weigh enough <2mm. 7. tared. Use the average of T1 and T2 and adjust the pipet depth in the suspension as indicated in Table 4. it may be necessary to occasionally apply backpressure to filter candle and remove build-up of soil which inhibits aspiration. Insert a filter candle. Add four 5 to 7. stir the sample with a magnetic stirrer for 5 min and wash 5 times with ≈ 250 mL of RO water each time. A quality control sample is included in each batch (<24 samples). Add 150 mL of RO water. 5. and turn on the vacuum.5-mL increments of H2O2 at 30-min intervals. Aspirate until liquid is removed and only slightly dampened sample remains. The H202-treated. connect to the vacuum trap assembly with tubing. place in a desiccator. then the following additional washings may be used. pipet after a time of 4. add additional H2O2 until organic matter oxidation is complete. 300-mL. tared fleakers. oven-dry sample is not used in the remaining PSDA procedural steps. For the <2-µm fraction. Proceed to procedure 3A1a1a for remaining PSDA procedural steps.5. During aspiration.72 Add ≈ 50 mL of RO water and 7.76 Record the total weight (TW) of the H2O2-treated. Weigh to nearest mg on an electronic balance and place into numbered. 7.5 mL of H2O2 to both soil sub-samples at ambient temperature. Remove the sample from the oven. Stir the sample with filter candle to ensure all soil particles will be rinsed. If the sample contains gypsum and flocculates. (b) remove the sample from the hot plate to slow the reaction. Heat the sample for an additional 45 min to decompose excess H2O2.5 h.

84 Place one of the samples in the oven and dry overnight at 110°C. 7. add small increments of ethyl alcohol to the samples or remove the samples from the hot plate to slow the reaction. tared fleakers.85 Record the total weight (TW) of the H2O2-treated. Apply vacuum and candle the samples to dryness.Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) Carbonate Removal (3A1a2) Field-Moist (3A1a2b) 7. oven-dry sample to the nearest mg. Rinse once with 200 mL of RO water. Continue to decant. 7. 7. Do not boil. weigh 20 g of soil.81 Add ≈ 50 mL of RO water and 5 mL of H2O2 to both soil samples at ambient temperature. and turn on vacuum. Weigh sufficient samples to yield 10 g of <2-mm. Heating accelerates reaction. stir the samples with a magnetic stirrer for 5 min then wash 5 times with ≈ 750 mL of RO water each time to remove soluble gypsum. 7. 7. Allow initial oxidation of organic matter to complete and then place samples on hot plate. stir the samples with a magnetic stirrer for 5 min and wash 5 times with ≈ 250 mL of RO water each time. repeat the heating procedure. Allow the samples to stand overnight. 7. connect to the vacuum trap assembly with tubing. transfer the samples to larger beakers. Insert filter candle. Add 150 mL of RO water. Proceed to procedure 3A1a1a and use the H2O2-treated sample that was not dried in oven for remaining PSDA procedural steps. and cool to ambient temperature. Add 5-mL increments of H2O2 at 45-min intervals until oxidation has completed or until 30 mL of H2O2 have been added.79 Place the samples on the hot plate and heat to ≈ 90°C until bubbles are no longer evident. If the samples contain >5% gypsum. 1984). if the sample contains 50% carbonates. If the froth from the reaction exceeds the capacity of the fleakers. If a reaction occurs. mix with a stirring rod. insert the ceramic filter candle into the solution. If the reaction is violent. Remove the sample from the oven.. moist. oven-dry sample is not used in the remaining PSDA procedural steps. Heat the sampled for an additional 45 min to decompose excess H2O2. then the following additional washings may be used. place in a desiccator. carbonate-free soil sample. 51 .g. Cover the soil samples with 50-mm watch glass.80 When no more carbonate bubbles are observed.82 Place the samples on the hot plate and heat to ≈ 90°C. The speed of dissolution can be increased by lowering the pH of the 1 N NaOAc solution (Rabenhorst and Wilding. add NaOAc solution.77 Weigh two 10-g samples of <2-mm. and heat until all the carbonates are removed. and cover with a watch glass.83 Place the samples on the filter rack. moist soil to nearest mg on an electronic balance and place into 300-mL. If the samples contain gypsum and flocculates.78 Add ≈ 200 mL of the 1 N NaOAc solution to both samples. The H2O2-treated. 7. Decant the solution and add more 1 N NaOAc solution. 7. Wash the samples four additional times with ≈ 150 mL of RO water. e. If the samples contain 1 to 5% gypsum.

90 Centrifuge or candle the samples to remove the dissolved Fe2O3.5 g of Fe2O3.94 Record the total weight (TW) of the sample to the nearest mg. Heat the samples for an additional 45 min to decompose excess H2O2. tared fleakers. If the sample contains >5% gypsum. and turn on the vacuum. transfer the samples to larger beakers. Total sample weight after dissolution should be ≈ 10 g. place in a desiccator. Add 150 mL of RO water. stir the sample with a magnetic stirrer for 5 min and wash 5 times with ≈ 250 mL of RO water each time. Combine the split samples into fewer fleakers. 7. 7. but do not exceed 80°C. and then place samples on hot plate. Split the sample into different fleakers if necessary. The H2O2 oven-dry sample is not used in the remaining PSA procedural steps. If the samples contain gypsum and flocculates.Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) Iron Removal (3A1a3) Field-Moist (3A1a3b) 7.88 Place the samples on a hot plate and heat to 90°C. For samples with more than 0. Proceed to procedure 3A1a1a and use the H2O2-treated sample that was not dried in oven for remaining PSDA procedural steps. As a maximum of ≈ 0. If the froth from the reaction exceeds the capacity of the fleaker.93 Place one sample in the oven and dry overnight at 110°C. stir the sample with a magnetic stirrer for 5 min then wash 5 times with ≈ 750 mL of RO water each time to remove soluble gypsum. Insert a filter candle. 7. Remove the sample from the oven. connect to the vacuum trap assembly with tubing.5 g of Fe2O3. then the following additional washings may be used.92 Place the samples on the filter rack. Add 5-mL increments of H2O2 at 45min intervals until oxidation has complete or until 30 mL of H2O2 have been added. Allow initial oxidation of organic matter to complete. Wash the samples four additional times with ≈ 150 mL of RO water. 7. Add 1 g of sodium dithionite powder with a calibrated scoop. 7. Stir constantly with a glass rod for 1 min and then occasionally for 15 min. If the sample contains 1 to 5% gypsum. repeat the dissolution treatment. 7. Add 10 mL of saturated NaCl solution and mix. and cool to ambient temperature.86 Weigh two 10-g samples of <2-mm. repeat the dissolution treatment two more times. 7. If the reaction is violent.89 Add 40 mL of the citrate solution and 5 mL of the sodium bicarbonate. Cover the soil samples with 50-mm watch glass. adjust the weight of the <2-mm. moist soil to nearest mg on an electronic balance and place into 300-mL. moist soil sample so that any one fleaker does not contain more than 0.5 g of Fe2O3 can be dissolved in 40 mL of the citrate solution.87 Add ≈ 50 mL of RO water and 5 mL of H2O2 to both soil samples at ambient temperature.5 g of Fe2O3. 7. 52 . Heat to 80°C in a water bath.91 If the samples contain less than 0. add small increments of ethyl alcohol to the samples or remove the samples from the hot plate to slow the reaction.

98 Soak the samples overnight in 100 mL of 0. 300-mL. tared fleakers. Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) Ultrasonic Dispersion (3A1a5) Field-Moist (3A1a5b) 7. Wash and tare these fleakers once every two months. If the sample contains gypsum and flocculates.101 Record the total weight (TW) of the sample to the nearest mg. then the following additional washings may be used. If the froth from the reaction exceeds the capacity of the fleaker.103 Add ≈ 50 mL of RO water and 7. tared fleakers. stir the sample with a magnetic stirrer for 5 min then wash 5 times with ≈ 750 mL of RO water each time to remove soluble gypsum. Proceed to procedure 3A1a1a and use the H2O2-treated sample that was not dried in oven for all of the remaining PSDA procedural steps. If the reaction is violent. Allow initial oxidation of organic matter to complete and then place samples on hot plate.100 Place one sample in the oven and dry overnight at 110°C. Insert filter candle. connect to the vacuum trap assembly with tubing. The H2O2-treated. A quality control sample is included in each batch (<24 samples). If the froth from the reaction exceeds the capacity of the fleaker.1 N NaOH. ovendry sample is only used for calculation of results and is not used in the remaining PSDA procedural steps. and turn on the vacuum.Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) Silica Removal (3A1a4) Field-Moist (3A1a4b) 7. Cover the soil samples with 50-mm watch glass. tared. 7. 7. moist soil to nearest mg on an electronic balance and place in 300-mL. 7. Remove the sample from the oven. Add 150 mL of RO water.5 mL of H2O2 to the soil samples at ambient temperature. 7. 7.96 Add ≈ 50 mL of RO water and 5 mL of H2O2 to both soil samples at ambient temperature. and then place samples on hot plate. transfer the sample to larger beakers. Cover the soil samples with 50-mm watch glass. stir the samples with a magnetic stirrer for 5 min and wash 5 times with ≈ 250 mL of RO water each time. Heat the samples for an additional 45 min to decompose excess H2O2. 53 . Weigh to nearest mg on an electronic balance and place into numbered. 7. Add 5-mL increments of H2O2 at 45min intervals until oxidation has completed or until 30 mL of H2O2 have been added.102 Weigh enough <2mm.95 Weigh two 10-g of <2-mm. Allow initial oxidation of organic matter to complete.99 Place the samples on the filter rack. If the samples contain >5% gypsum.97 Place the samples on a hot plate and heat to 90°C. Wash the samples four additional times with ≈ 150 mL of RO water. add small increments of ethyl alcohol to the samples or remove the samples from the hot plate to slow the reaction. place in a desiccator. transfer the samples to a larger beaker. moist soil to achieve two ≈ 10-g samples of air-dry soil. If the samples contain 1 to 5% gypsum. and cool to ambient temperature. 7.

7.7.3. 7.111 After ultrasonic dispersion. Ensure the power supply is properly tuned. Between samples. 7.047-mm) sieve mounted on a ring stand. Determine the exact volume of sodium hexametaphosphate to add to each sample by regressing the volume of sodium hexametaphosphate against the dry residue weight of sodium hexametaphosphate and then by predicting the volume needed to dispense 0. During aspiration. (c) transfer sample to a 1000-mL beaker. oven-dry sample is only used for the calculations of results and is not used in the remaining PSDA procedural steps. Avoid using jets of 54 . 90-mL weighing bottles. Finger-rubbing of sample may be required during transfer to speed washing of sample.109 A sodium hexametaphosphate standardization is performed with each new batch of solution. clean the probe by placing it in water or alcohol and energizing it for a few seconds. Stir the sample with filter candle to ensure all soil particles will be rinsed. Wash the sample four additional times with ≈ 150 mL of RO water. Consult the instruction manual. or (d) reduce the amount of H2O2 to sample. and cool to ambient temperature.3. Adjust output control as required.110 Disperse the suspension with ultrasonic vibrations. Set timer to 5 min. 9. do one or any combination of the following: (a) add small increments of ethyl alcohol to the sample. 7. Use only designated weighing bottles for standardization.4408 g of sodium hexametaphosphate into each sample. equivalent to 0.5. connect to the vacuum trap assembly with tubing. Wash and tare these bottles after each standardization. place the sample in a 1000-mL beaker and stir the sample with a magnetic stirrer for 5 min then wash 5 times with ≈ 750 mL of RO water each time to remove soluble gypsum. add ≈ 75 mL RO water and pour the suspension through a 300-mesh (0. Collect the silt and clay in the 1-L cylinder.109. If the reaction is violent. Heat the sample for an additional 45 min to decompose excess H2O2. Record any unusual sample reactions. add additional H2O2 until organic matter oxidation is complete. Immerse the probe in the suspension to a 3-cm depth. 10.6. 9. 7. Place a funnel below the sieve and a 1-L cylinder below the funnel. If the sample contains 1 to 5% gypsum. to sample. 7. and turn on the vacuum. 10.6. (b) remove the sample from the hot plate to slow the reaction.4408 g of sodium hexametaphosphate.106 Place one sample in oven and dry overnight at 110°C. Add four 5 to 7. it may be necessary to occasionally apply backpressure to filter candle and remove build-up of soil which inhibits aspiration. Subtract the weight of the sodium hexametaphosphate (DW) that is contained in the extracted aliquot from the silt and clay weights to calculate silt and clay percentages. 10. 9.108 Add ≈ 100 mL of RO water and the exact volume of sodium hexametaphosphate solution (≈ 10 mL).0. Add duplicate aliquots (8. Aspirate until liquid is removed and only slightly dampened sample remains.104 Place the samples on a hot plate and heat to 90°C. If the sample contains gypsum and flocculates.5-mL increments of H2O2 at 30-min intervals.0. Add 150 mL of RO water. 7. Use the H2O2-treated sample that was not dried in oven for the following PSDA procedural steps. then the following additional washings may be used. Insert a filter candle.105 Place the sample on the filter rack. Press start button. If the sample contains >5% gypsum.107 Record the total weight (TW) of the H202-treated.0 mL) of sodium hexametaphosphate solution to numbered tared. To determine the exact volume of sodium hexametaphosphate to add to each sample refer to Section 7. Oven-dry aliquots overnight and record dry residue weight of sodium hexametaphosphate. If oxidation is incomplete. Remove sample from oven. stir the sample with a magnetic stirrer for 5 min and wash 5 times with ≈ 250 mL of RO water each time. oven-dry sample to the nearest mg. The H2O2-treated. 11. place in a desiccator.

gravimetrically calibrate the delivery volume of the pipet by weighing the amount of RO water dispensed from the pipet. Proceed to procedure 3A1a1a for remaining PSDA procedural steps. Continue to wash until the suspension volume in the cylinder is ≈ 800 mL. Wash the sand into an evaporation dish and dry the sand at 110°C overnight.5. Record the weight of each separate sand fraction (SWi) to the nearest mg. Wash and tare these fleakers once every two months. 1932). place the very fine sand and fine sand fractions in gelatin capsules and the remaining sand fractions in a labeled vial.117 Transfer the dried sand to a nest of sieves that has a top-to-bottom order of 1. Continue to wash until the suspension volume in the cylinder is ≈ 800 mL. Sand and some of the coarse silt remain on the sieve.0. The oven-dry sample is not used in the remaining PSA procedural steps. Weigh to nearest mg on an electronic balance and place into numbered. Finger-rubbing of sample may be required during transfer to speed washing of sample.3-cm vertical and lateral movements and oscillates at 500 strokes min-1. A quality control sample is included in each batch (<24 samples).047-mm) sieve mounted on a ring stand. Wash sand dishes after every use. Collect the silt and clay in the 1-L cylinder. moist soil to achieve two ≈ 10-g samples of air-dry soil. Record the delivery volume (DV) and use the value to calculate the results. Sand and some of the coarse silt remain on the sieve. 7.25. Allow the cylinder to stand overnight to equilibrate the suspension with the room temperature. place in a desiccator. Prepare a RO water blank to measure temperature fluctuations. 0. Stir the silt and clay 55 . Periodically. Fill the cylinder to 1 L and cover with a 65-mm watch glass.water in washing the sample. Wash the sand into an evaporation dish and dry the sand at 110°C overnight. Record temperature (T1) of blank. Place a funnel below the sieve and a 1-L cylinder below the funnel. Wash and rub all particles from the fleaker into the sieve. Store capsules in the labeled vial. 0. 7. Rinse all <20-µm particles into the cylinder. Fill the cylinder to 1 L and cover with a 65-mm watch glass. Mount the pipet on an adjustable pipet rack (Shaw. and cool to ambient temperature. If optical analysis is requested. Place pipe insulation around sample and blank cylinders to prevent rapid changes in temperatures.115 Add ≈ 175 mL of RO water to sample that was not dried in the oven. Rinse all <20-µm particles into the cylinder.116 Remove the sample from the shaker and pour through a 300-mesh (0.1. 7. Avoid using jets of water in washing the sample. Prepare a RO water blank to measure temperature fluctuations. Place pipe insulation around sample and blank cylinders to prevent rapid changes in temperatures. tared fleakers. Remove the sample from the oven.047 mm. Place sample in a horizontal shaker set at 120 oscillations min-1 and shake for 15 h (overnight).113 Dry one sample in an oven at 110°C overnight. 0. 7. Particle-Size Distribution Analysis (3A) Particles <2 mm (3A1) Pipet Analysis (3A1a) Water Dispersion (3A1a6) Field-Moist (3A1a6b) 7. 7. Regulate the vacuum such that the pipet fills in ≈ 12 s. Shake the sand for 3 min on a shaker that has 1. tared. Allow the cylinder to stand overnight to equilibrate the suspension with the room temperature. 300-mL. 25-mL pipet.112 Weigh enough <2mm.118 Determine the percentage of fine silt and clay gravimetrically by removing an aliquot from the suspension in the 1-L cylinder with a Lowy.114 Record the total weight (TW) of the sample to the nearest mg. 7. and 0. Wash and rub all particles from the fleaker into the sieve.

5. weighing bottle. Rinse the pipet with RO water into the tared. Proceed to procedure 3A1a1a for remaining PSDA procedural steps. Record the residue weight (RW) to the nearest 0. or 6.5.5.4 Coarse silt % = 100 . Use calculations in sections 8.0.1. Calculations 8. open the pipet.Clay % where: RW20 = Residue weight (g) of <20-µm fraction 8.5 h. oven-dry sample 8. Record the temperature (T2) of blank. vibrationless table and stir with a hand stirrer in an up-and-down motion for 30 s.2 – 8. 0. Repeat the procedure described for the <20-µm fraction. Calculations Use calculations in sections 8. turn on the vacuum. Record the time that stirring is stopped.10 for water dispersible PSDA (3A1a6a and 3A1a6b).4364/CF) 1000 mL/DV Dispensed pipet volume Total weight of H2O2-treated.1 mg. Also proceed to procedure 3A1a1a for determination of fine-clay and/or carbonate clay.1 – 8.DW) x (CF/TW)) where: RW2 = Residue weight (g). Place the aliquot into a tared and numbered. For the <2-µm fraction. and withdraw an aliquot at the calculated time (Table 1).5 Fine Clay (%) = 100 x ((RW-DW) x (CF/TW)) where: RW = DW = CF = DV = TW = Residue weight (g) of <0. H2O2-treated. pipet after a time of 4.3 Sand % = ∑ (SWi /TW) x 100 where: SWi = Weight of sand fractions (1. 0.25.7 – 8. Place the cylinder on a stable. 5. Use the average of T1 and T2 and adjust the pipet depth in the suspension as indicated in Table 2.4408/CF) CF = 1000 mL/DV DV = Dispensed pipet volume TW = Total weight (g). 0.5.6 for all PSDA procedures (3A1a1-5a and 3A1a1-5b) except water dispersible PSDA.2-µm fraction Dispersing agent weight (g) = (0.6 for procedures 3A1a1-5a and 3A1a1-5b as follows: 8. and 0. 90-mL weighing bottle. oven-dry sample 56 .047 mm) 8. <2-µm fraction DW = Dispersing agent weight (g) = (0. For the <20µm fraction. slowly lower the closed pipet to a 10-cm depth in the suspension. Timing is started upon completion of the stirring.(Clay % + Fine Silt % + Sand %) 8.2 Fine Silt % = 100 x ((RW20-DW) x (CF/TW)) . Dry the aliquots at 110°C overnight and cool in a desiccator that contains calcium sulfate or an equivalent desiccant.1 Clay % = 100 x ((RW 2 . 8.suspension with mechanical stirrer for at least 5 min.

3 Use the corrected (CR) linear regression equations to estimate the g of CaCO3 in the sample.0.Carbonate Clay Equivalent (%) Calculations 8.7 – 8. oven-dry sample 8.5.e.10 Coarse silt % = 100 .4 Carbonate Clay Equivalent (<2 µm) (%) = ((g CaCO3 ) x 100 x CF)/TW where: CF = 1000 mL/dispensed pipet volume (mL) TW = Total weight of H2O2-treated oven-dry sample 8.25.8..047 mm) 8.(Clay % + Fine Silt % + Sand %) 9. and 0.2 Calculate two regression equations.1.5 Noncarbonate Clay (<2 µm) (%) = Total Clay (%) . Use the Na2CO3 weights as the dependent variable (regressed or predicted values) and the corresponding manometer readings as the independent variable.6. 8. 0.7 Clay % = 100 x ((RW 2 x CF)/TW) where: RW2 = Residue weight (g). <2-µm fraction CF = 1000 mL/DV DV = Dispensed pipet volume TW = Total weight (g). 8.10 for procedures 3A1a6a and 3A1a6b as follows: 8. 8. i.6.1 percent.6 Calculate carbonate clay percentage as follows: 8. 0.1 Correct the manometer reading as follows: CR = (MR .BR) where: CR = Corrected reading MR = Manometer reading BR = Blank reading Three blanks are run with each batch (<24 samples). 0.Clay % where: RW20 = Residue weight (g) of <20-µm fraction 8. one for corrected manometer readings <100 and another for corrected readings >100.8 Fine Silt % = (100 x (RW20 x CF)/TW)) . Report Report each particle-size fraction to the nearest 0. 57 .9 Sand % = ∑ (SWi /TW) x 100 where: SWi = Weight of sand fractions (1. The average of three blanks is used as BR.6.6.6.

Ed.J. 1932. 1964. 1960. G. References Bouyoucos.T.H. 39:556-561. Mikhail.B. 1969. Govt.) Methods of soil analysis. Action of hydrogen peroxide on weathered mica. Klute (ed. p. 18:79-87. and J. R.L. U. Am. p. Particle-size analysis.F. 1986. Physical and mineralogical methods. 28:27-37. In B. 1929. Briner. No. 58 . 3. 77:437-441. Soil Sci. 383-411. Counc. Soil Sci. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys.. 436. Physical methods. DC. 229-263. Aggregate formation of allophonic soils.) Adv. V. Saly.C.G. Version No. Proc. Soil Survey Staff. Soil survey laboratory methods manual. 2nd ed. Acad. Adams Jr. Takenaka. Anal. 303-324. Physical properties of allophone soils. L. ASA and SSSA. Soc. V. and E. Meyer. Part 4. M. J. Office. 48:216-219. Miles. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 1972. Soil Sci. Jackson. Am. Rust. No. Methods of making mechanical analyses of soils. R.. The ultimate natural structure of soil. Monogr. In J. 9. 7th Conf. Agron. NY.. p.. Soil Survey Division Staff.. DC. 28:416-419.Z.) Soils with variable charge. Govt. Wisconsin.C.. Sov.J. Soil Sci.K. 11:1547-1559. Soc. In N. G. 2nd ed. ASA and SSSA. 42. E. Lower Hutt. and B. H.W. Soc. Am. Soc. El Swaify. Soil Sci. Office. DC. Press. p. Use of ultrasonic vibration for dispersing of soil samples. Soil Sci. Lincoln. Madison. Acad. 1996. Univ. 2nd ed. Kubota. Improved stirring and pipeting apparatus for mechanical analysis of soils.0. Mullins. DC. Warkentin. Part 1. Alexander. Gee.P. Handb. 1984. S.S. Routine particle size analysis of soils using sodium hypochlorite and ultrasonic dispersion. 1992. Govt. Espinoza. 46:391-395. WI. J.H.P. Rapid method to obtain carbonate-free residues from limestone and petrocalcic materials. NE.K. Bauder. Kilmer. Soil Sci.. Brady (ed. J. p. Effects of drying on the dispersion of soils. 2002. 255-293. USDA-NRCS. In A..P.. Pub. O. 1949. Iron oxide removal from soils and clays by a dithionite-citrate system buffered with sodium bicarbonate. Print. Shields. and Plant Nutr. Or. T. Natl. 4:409. and G. U. 1993. Soil Survey Staff. Washington.A.Z. In Clays and clay minerals. T. Physical and mechanical properties of Oxisols. 1980.W. Washington.H. Soil survey manual.L.W. Proc. New York. Soil Res. Book Series No. 11.L. Soil Sci. USDANRCS. W.. Chem. Carbonate clay: Measurement and relationship to clay distribution and cation exchange capacity. Am. Gee. Millet. 1967. Handb. Rabenhorst. New aliquot and filter devices for analytical laboratories. T. Am. M. M. Mehra. and M. 1999.W. Shaw. Inc.. Wilding.. and J. 5. Madison.S.) Method of soil analysis. Particle-size analysis.. Ind. University of Nebraska. Dane and G. Soil Sci. Madison. Soil Survey Investigations Report No. Washington. Office.P. Natl. Aust. Grossman.M. WI. N. Res. and R.. 1938.10. and L. Soil chemical analysis—advanced course. 18.. Print. Print. Soil Sci. Proc. 1978. 1961. Maeda. Soc.S. Kilmer. Agron. 25:325-326. 68:15-24. Soil Sci. Drosdoff. Agric. Theng (ed. U. Washington.B. USDA. G. and M.S. Soil Sci. Concepts of soil physics. Jackson. and L. Carbonate removal from soils by a modification of the acetate buffer method. 1977. R. Topp (eds. Eng.G. Characterization of mineral forms in Andepts from Chile. N. Skopp. 16:241-244. 1954. and D. and J. Proc.C. Sci. 237-317.

chemical.) Soil crusting. Soil Fertil. 1971. 59 . 1948. D.Sumner. Sumner and B. CRC Press Inc.E. M. Soc. FL. A rapid manometric method for the determination of carbonate in soils. The electrical double layer and clay dispersion. Am.A. Stewart (eds. Soil Sci. Watson. Proc. 34:127134.E. 1-32. Ultrasonic vibration as a method of soil dispersion. J. p.. 1992. In M.R. 13:127-129. Williams.E. and physical processes.. Boca Raton.

Fig 1. 1932). Shaw Pipet (Shaw. 60 .

2. 61 . Fig.Fig. Shaw Pipet used for particle-size analysis of the <2-mm fraction at the USDA-NRCS Soil Survey Laboratory. 3. Close-up of the Shaw Pipet apparatus.

50 4 29 71 43 21.75 3 43 59 28 30.00 4 46 76 17 19.75 3 48 60 46 29.25 3 56 62 48 27.00 3 57 63 9 27.1 Temp (°C) 20 µ m 5 µm min s min s 15.00 3 52 61 46 28.25 4 6 65 42 25.00 3 47 60 26 29.Table 1.00 4 2 64 35 26.00 4 32 72 35 21.50 4 36 73 29 20.25 4 1 64 13 26.50 4 11 66 50 24.25 4 24 70 27 22.65 g cc-1 particle density.50 4 17 68 24 23.50 4 50 77 13 19. Sampling times at 10-cm depth.25 4 12 67 13 24.50 3 59 63 52 26.00 4 53 78 12 18.75 3 53 62 7 28.00 5 17 84 36 16.75 4 34 73 2 21.00 4 26 70 52 22.75 4 27 71 18 22.00 4 39 74 23 20.75 4 15 68 0 24.50 4 5 65 19 25.50 4 42 75 18 20.75 3 58 63 30 27.25 4 37 73 56 20.00 4 20 69 13 23.25 3 50 61 26 28.75 4 21 69 37 23. 0.00 5 9 82 22 17.00 3 42 59 9 ____________________________________________________________________________________________________________________________________ 1 Use this table with procedures 3A1a1-5a and 3A1a1-5b.25 3 45 60 6 29.00 5 1 80 16 18.50 3 54 62 27 27.75 4 4 64 57 26.50 3 49 61 6 28.25 4 18 68 48 23.4408 g L-1 NaHMP solution.50 3 44 59 47 29. and 2.00 4 14 67 37 24.75 4 9 66 27 25.25 4 31 72 9 21. 62 .00 4 8 66 4 25.50 4 23 70 2 22.

03 7.32 10.44 25.56 8.98 6.44 20.4408 g L-1 NaHMP solution.75 7.50 5.11 7.18 8.29 6.75 7.14 6.57 9.19 7.63 10.88 7.49 8.18 8.53 10.69 7.50 6.07 23.00 5.08 8.10 7.25 7.85 7.84 7.35 8.17 9.77 8.52 8.30 8.77 26.50 7.65 21.50 6. 0.36 8.65 8.02 6.23 24.13 8.23 8.45 8.58 10.76 8. 63 .5 6.31 9.49 20.08 8.25 6.49 7.00 6.14 7.41 9.41 8.83 27.37 7.69 9.24 6.27 9. Sampling depths (cm) for 2µm clay.61 7.02 9.04 8.32 7.05 28.27 8.50 6.34 24.00 7.23 7.43 7.62 9.70 21.13 6.72 9.98 8.45 7.99 7.50 5.02 7.00 5.00 6.88 6.39 25.74 6.06 7.87 9.55 8.98 7.98 18.38 29.12 8.58 8.00 6.27 7.67 6.54 8.39 8.93 8.08 19.97 9.03 8.84 6.07 8.89 8.66 6.81 22.15 7.75 6.48 10.91 22.52 6.60 8.50 6.50 6.69 10.27 29.81 7.73 8.58 7.55 ____________________________________________________________________________________________________________________________________ 1 Use this table with procedures 3A1a1-5a and 3A1a1-5b.22 8.74 10. and 2.25 6.73 7.14 7.49 30.72 26.01 7.75 5.99 7.44 29.60 21.00 6.95 6.5 15.18 24.94 27.37 7.99 27.07 7.00 5.55 9.83 6.25 7.32 9.33 29.38 10.96 7.10 28.92 6.43 8.25 6.12 9.94 7.22 9.86 22.99 8.00 6.66 26.92 9.83 9.28 6.67 8.26 7.84 8.0 5.41 6.75 6.94 8.42 9.75 6.81 8.85 8.57 7.74 9.25 6.77 18.61 7.0 6.59 6.77 9.99 8.69 8.27 10.25 5.77 7.50 6.54 21.65 7.75 6.46 8.50 25.25 5.50 7.12 23.88 27.59 9.45 9.19 7.81 6.73 7.88 9.53 7.02 23.61 26.25 6.25 5.75 6.74 8.21 6.90 8.50 7.78 9.58 7.54 7.67 9.75 6.17 6.81 7.00 5.65 g cc-1 particle density.03 8.64 9.07 9.39 7.75 7.95 8.90 8.24 6.31 8.92 7.99 6.46 7.29 20.89 7.22 6.43 10.69 7.18 19.00 5.10 6.81 8.50 9.11 5.47 8.35 7.Table 2.00 6.86 8.00 5.18 7.13 8.38 5.00 6.1 Temp (°C) Time (h) 4.76 7.28 24.06 6.00 5.32 7.38 16.25 6.37 9.47 9.50 5.16 28.5 5.96 23.63 8.72 8.10 7.93 9.52 9.18 7.80 7.39 20.22 7.82 9.75 6.00 7.50 6.79 8.75 22.22 8.21 28.27 8.36 9.65 7.64 8.84 7.92 7.55 25.58 17.

65 g cc-1 particle density.00 4 45 76 19.75 4 3 64 26.75 4 33 72 21.25 4 37 73 20.50 3 54 62 27.25 3 55 62 27.00 4 2 64 26.50 3 44 59 29.Table 3.75 3 58 63 27.00 5 0 80 18.50 4 35 73 20.00 5 8 82 17.50 3 39 60 28.50 4 49 77 19.1 Temp (°C) 20 µ m min s min 15.75 3 47 60 29.75 3 52 61 28.00 3 41 59 1 5 µm s 26 12 7 3 4 8 9 14 47 20 53 27 0 35 9 43 18 53 29 4 40 16 52 28 5 42 19 56 34 11 49 27 6 44 23 1 40 20 59 39 18 58 38 19 59 40 21 1 ____________________________________________________________________________________________________________________________________ Use this table with procedures 3A1a6a and 3A1a6b.25 3 45 59 29.75 3 43 59 30.25 4 24 70 22.50 4 42 75 20.00 4 19 69 23.00 4 25 70 22.50 3 59 63 26.75 4 27 71 22. Sampling times at 10-cm depth and 2.00 4 7 65 25.75 4 9 66 25.00 4 38 74 20.50 4 4 65 25.50 4 16 68 23.25 4 0 64 26.00 3 51 61 28.00 5 17 84 16.50 4 28 71 21.25 4 17 68 23.00 4 32 72 21.50 4 10 66 24.50 4 22 69 22.00 4 53 78 18.75 4 21 69 23.00 3 56 63 27.25 4 12 67 24. 64 .25 3 50 61 28.00 3 46 60 29.75 4 15 67 24.25 4 6 65 25.25 4 30 72 21.00 4 13 67 24.

99 6.42 9.95 7.96 8.11 7.61 9.00 5.00 7.00 5.63 7.00 6.70 7.66 8.75 7.32 8.41 8.50 7.Table 4.38 18.12 5.69 6.91 7.00 6.55 7.10 8.01 8.25 5.34 23.82 16.40 28.07 10.80 9.68 9.85 9.64 8.28 8.66 9.75 9.00 5.85 7.59 7.05 21.12 10.96 10.00 5.90 9.03 7.24 7.33 9.14 9.88 8.50 6.50 5.5 6.22 6.57 9.41 8.71 9.24 8.59 24.50 6.75 6.00 6.78 8.29 6.09 9.69 8.28 9.75 6.19 27.50 6.54 24.25 6.40 7.37 7.65 g cc-1 particle density.59 7.66 7.79 8.87 8.05 8.50 5.55 29.0 5.90 21.29 23.55 7.48 7.14 22.86 20.93 6.44 7.82 7.51 8.39 23.10 8.76 20.00 6.79 7.57 19.35 10.93 7.77 7.26 5.69 25.20 7.52 9.29 28.03 9.55 8.15 8.19 18.25 7.42 7.00 5.83 8.41 9.14 27.74 7.04 6.75 6.60 29.89 26.97 7. Sampling depths (cm) for 2-µm clay and 2.99 7.50 7.19 22.50 5.16 7.44 23.96 8.36 9.89 7.56 8.20 7.00 6.73 8.20 8.1 Temp (°C) Time (h) 4.39 7.5 7.16 7.42 8.50 6.28 8.95 9.13 8.52 9.50 6.74 25.24 27.75 6.01 7.83 7.18 10.03 7.25 9.51 8.83 8.81 20.18 6.94 26.57 9.00 7.62 8.75 6.25 6.34 28.49 24.46 9.01 10.99 26.66 20.50 6.25 6.07 7.33 8.15 6.89 6.05 8.78 7.33 7.19 8.04 26.19 9.61 8.51 7.76 1 ____________________________________________________________________________________________________________________________________ 6.63 7.25 6.90 9.11 7.87 7.25 6.25 6.79 8.60 8.75 6.25 7.70 8.38 9.49 8.59 7.20 8.29 10.47 9.10 22.36 8.24 7.77 8.47 19.29 7.24 22.25 6.50 29.11 6.75 5.84 6.05 7.46 10.61 6.45 28.51 7.79 9.64 24.01 17.23 10.5 5.47 7.25 6.71 7.39 5.65 29.07 6.67 8.09 7.57 8.98 9.96 6.67 6.25 6.93 8.85 9.52 10.00 6.67 7.00 6.38 8.23 6. 65 .72 8.92 8.59 7.74 8.00 8.30 8.84 25.54 6.16 7.82 6.50 6.09 27.14 6.24 8.79 25.63 9.57 Use this table with procedures 3A1a6a and 3A1a6b.95 21.40 10.39 7.47 8.00 21.85 7.92 8.75 6.00 8.74 9.09 8.12 7.94 7.53 8.00 7.86 6.75 6.00 5.75 7.30 9.87 8.46 8.82 8.00 5.31 6.0 15.32 8.71 30.75 7.45 8.

the 20. and 0. fraction weights are usually recorded in pounds.to 250-mm. the particle-size fractions 2 to 5. The conversion of a volume estimate to a weight estimate assumes a particle density of 2. 75. and >250-mm fractions. If it is sieved and weighed in the laboratory. The SSL estimates weight percentages of the >2-mm fractions from volume estimates of the >20-mm fractions and weight determinations of the <20-mm fractions by procedure 3A2a2. Weight percentages of the >20-mm fractions are calculated from field volume estimates of the 20. Weight measurements of this fraction in the laboratory are not reliable. Rock fragments are generally sieved and excluded from most chemical.to 20mm fraction are laboratory measurements. 5 to 20. Rock fragments are further defined as strongly cemented or more resistant to rupture.. For any >2-mm fractions estimated by volume in the field. 20 to 75. Exceptions are described in method 1B1b2f. the minimum dry specimen sizes that need to be sieved and weighed are 1. In the field. respectively. The SSL determines weight percentages of the >2-mm fractions by field and laboratory weighings by procedure 3A2a1. 66 . Weight measurements for the 2.to 75-mm fraction is estimated in the field as a volume percentage of the whole soil.45 g cc-1. whereas in the laboratory. 2002). and mineralogical analyses. 1993). Refer to ASTM method D 2488 (American Society for Testing and Materials.g. whereas pararock fragments are less cemented than the strongly cemented class. the field samples or "moist" material should have weights two to four times larger (American Society for Testing and Materials. if required. the results are usually not reliable because of small sample size.to 75-mm fractions in the field are more accurate than visual volume estimates. fraction weights are recorded in grams. Weight measurements of the 20.0 kg.65 g cc-1 and a bulk density for the fine-earth fraction of 1. Measured values can be substituted in this volume to weight conversion. with most of these fragments broken into particles 2 mm or less in diameter during the preparation of samples for particle-size analysis in the laboratory. In the field or in the laboratory. 2004). and discarded in the field.to 75-mm fraction should be done in the field. The volume estimates that are determined in the field are converted to dry weight percentages. Soil variability and sample size are interferences to weight determinations of the >2mm particles. the SSL calculates weight percentages by procedure 3A2b. Procedures for reporting data for a size fraction base are outlined in Section 2C. available water capacity and linear extensibility (Grossman. The total >2-mm fraction is reported on a whole soil oven-dry weight percentage base.0 and 60. The visual volume estimates of the >20-mm fraction are subjective.Particle-Size Distribution Analysis (3A) Particles >2 mm (3A2) Rock and pararock fragments are defined as particles >2mm in diameter and include all particles with horizontal dimensions less than the size of a pedon (Soil Survey Division Staff. The <20-mm fractions are sieved and weighed in the laboratory. Therefore.to 75-mm fraction is generally sieved. The >250-mm fraction includes stones and boulders that have horizontal dimensions that are smaller than the size of the pedon. sieving and weighing the 20. the sieving and weighing of the >2-mm fraction are limited to the <75-mm fractions. Whenever possible. 2004). e. physical. Unless otherwise specified. In order to accurately measure rock fragments with maximum particle diameters of 20 and 75 mm. The volume estimates are visual field estimates.1 to 75 mm are reported on a <75-mm oven-dry weight percentage basis. This is the preferred and usually the most accurate method. It is necessary to know the amount of rock fragments for several applications. Enough soil material needs to be sieved and weighed to obtain statistically accurate rock fragment content. Less accurately.to 75-mm. weighed. The 20.

5 cm 5. Enough soil material needs to be sieved and weighed to obtain statistically accurate rock fragment content. 67 . The <20-mm fractions are sieved and weighed in the laboratory. Application Procedure 3A2a1 is used to determine weight percentages of the >2 mm fractions by field and laboratory weighings.4 76 mm. weight measurements for the 20.8 Brown Kraft paper 6.1 9 mesh.0 and 60. the 20to 75-mm fraction can be sieved and weighed in the laboratory. 2004).7 g of sodium hexametaphosphate (NaPO3)6 and 7. sieving and weighing the 20. weighed. 3/4 in 5. The percentage of any 2. 3 in 5. square-hole 5. Interferences Soil variability and sample size are interferences to weight determinations of the >2mm particles.2 Trays. This is the preferred method.to 75mm fraction can be determined in the laboratory. Samples received in the laboratory generally have a maximum weight of 4 kg.0 kg.to 75-mm fraction on a <75-mm oven-dry weight basis is calculated. snake bites.1 Electronic balance. In order to measure accurately rock fragments with maximum particle diameters of 20 and 75 mm.3. ±1-g sensitivity and 15-kg capacity 5.Particle-Size Distribution Analysis (3A) Particles >2 mm (3A2) Weight Estimates (3A2a) By Field and Laboratory Weighing (3A2a1) 1.3 20 mm. 2. 4.1 Reverse osmosis (RO) water 6. Refer to procedure 1B. Equipment 5.to 75-mm fraction should be done in the field. and discarded in the field or is obtained from a field volume percentage estimate. the minimum specimen sizes ("dry" weights) that need to be sieved and weighed are 1. However. Reagents 6. tared 5.4 Mechanical shaker with 9-mesh and 4-mesh sieves 5.3.5 Rubber roller 5. 3. Safety The main hazards are in the field during sample collection.3. The 20. 4.76 mm 5. Some hazards are sharpedged excavation tools. 2 mm 5.7 Scale. 5. and falls.3 Sieves. Refer to ASTM method D 2488 (American Society for Testing and Materials.to 75-mm fraction is generally sieved. When field determinations are not possible.6 Metal plate. Dissolve 35. plastic. 100-lb (45-kg) capacity 5.3. Therefore.3 Sodium hexametaphosphate solution. respectively.to 75-mm fraction.94 g of sodium carbonate (Na2C03) in L of distilled water. Summary of Method Field weights are determined for the 20.2 4 mesh. 6. The <20-mm fractions are sieved and weighed in the laboratory. The <20-mm fractions are sieved and weighed in the laboratory.2 1 N HCl. 76 x 76 x 0.

Roll and sieve until only the coarse fragments that do not slake in sodium hexametaphosphate solution on the sieve. 7. Sieve this material with a 20-mm sieve. 7. Air-dry weight is defined as a constant sample weights obtained after drying at 30±5°C (≈ 3 to 7 days). 8. As a 60-kg sample may not be feasible because of limitations of time and/or soil material. Thoroughly mix material by moving the soil from the corners to the middle of the processing area and then by redistributing the material.to 5-mm fraction. Repeat process four times. Use the AD/OD (air-dry/ovendry ratio) (procedure 3D1) to calculate the oven-dry weight of <2-mm fraction. Sieve clayey soils that contain many coarse fragments in the mechanical shaker. substitute rubber roller for wooden rolling pin.3 Process air-dry material on a flat. and discarded in the field. Air-dry. record weight. weigh the material that does not slake. adjust weight of coarse fragments with <5-mm diameters. and record weight. these weights are already in grams. Roll material with wooden rolling pin to crush clods to pass a 2-mm sieve. select a sub-sample for preparation. Weigh and record weight (lbs) of <20-mm fraction. and record moist weight. Discard the >75-mm material. air-dried weight (g) for the 2. convert these weights in pounds to grams. Laboratory 7. Weigh. 8. Calculations 8.to 75-mm fraction. Procedure Field 7. Use the following equation to determine the percentage of any 2.2 Distribute the field sample on a plastic tray. 8.to 75-mm fraction on a <75-mm oven-dry weight-basis. as this fraction is generally sieved. Label and send to laboratory for analyses. weighed.1 Sieve a representative horizon sample with a 76-mm sieve.to 75-mm fragments.3 Determine ratio of slaked. Using this ratio.5 Weigh soil material with diameters of 2 to 5 mm. 8.7. Soak in sodium hexametaphosphate solution for 12 h. Determine air-dry weight of sub-sample.2 Determine field-moist weight of the sub-sample as received in the laboratory. actual sample size may be 30 or 40 kg. and discard coarse fragments with diameters of 20 to 75 mm and 5 to 20 mm. Most laboratory samples do not contain 20. weigh.to 75-mm fractions. 7. metal plate that is covered with brown Kraft paper. Sieve about 60 kg of material to accurately measure rock fragments that have a maximum particle diameter of 75 mm. Discard the 20. Weigh sub-sample and record weight. Place a sub-sample of the <20mm material in a plastic bag. air-dried weight (g) to unslaked. If laboratory measurements are determined for the <75 mm and the 20. Air-dry.4 If more sample is received than is needed for processing. weigh. and discard. For samples with easily crushed coarse fragments.to 75-mm fraction. Weigh and record weight (lbs) of <75-mm fraction. Percentage >2 mm fraction(<75-mm basis) = (A/B) x 100 where: 68 .4 Base coarse fragment calculation on oven-dry weight-basis.1 If field weight measurements are determined for the <75-mm and the 20.

Soil Survey Division Staff.H. Dane and G.1 Weight (lbs) of field-moist. determine oven-dry weight from the field-moist weight of a sample by calculating as follows: Oven-dry weight (g) = [Field-moist weight (g)]/[Field-moist weight (g)/Oven-dry weight (g)] 8. ASA and SSSA. Section 4. Topp (eds. Handb. DC. Annual book of ASTM standards. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.to 5-mm fraction 9. 1993. Reinsch. In J.C.5 Determine oven-dry weight by weighing the sample after oven-drying at 110°c for 24 h or by calculating as follows: Oven-dry weight (g) = [Air-dry weight (g)]/ADOD where: ADOD = Air-dry/oven-dry weight 8. 11.S. 201-228. Standard Practice for Description and Identification of Soils (Visual-Manual Procedure). U. p.5 Weight (g) of air-dry processed soil sample 9.8 Weight (g) 2.7 In calculations of the oven-dry weight percentages of the >2-mm fraction. R. WI. PA. Madison. USDA. Govt. Bulk density and linear extensibility.3 Weight (g) of field-moist soil sample 9. Vol. Print.B.to 75-mm fraction Laboratory 9. 2004. geosynthesis.A = Weight of 2.08.G.to 5-mm fraction after slaking 10. Soil and rock. Base the corrections for the field-water content on the difference between the field-moist weight and air-dry weight of the bulk sample. D 2488. 20.to 20-mm fraction 9. Physical methods. make corrections for the field-water content of the <75-mm sample at sampling and for the water content of the air-dry bulk laboratory sample. Part 4. Soil Sci. and T. No. 9. Office. Philadelphia.mm fraction (g) B = Weight of <75-mm fraction (g) 8.6 Weight (g) 20-to 75-mm fraction 9.10 Weight (g) of sub-sample 2.6 Similarly. 69 . dimension stone. References American Society for Testing and Materials. ASTM. <75-mm fraction 9.9 Weight (g) of sub-sample 2.) Methods of soil analysis.7 Weight (g) 5.to 5-mm fraction before slaking 9. Am. 2002. 04. Book Series No.2 Weight (lbs) of field-moist. Construction. Report Field 9. Soil survey manual. 5..4 Weight (g) of air-dry soil sample 9. Washington. Grossman.to 75. 18.

to 250-mm. square-hole 5. the 20.0 kg.3. respectively. Enough soil material needs to be sieved and weighed to obtain statistically accurate rock fragment content.76 mm 5. The >250-mm fraction includes stones and boulders that have horizontal dimensions that are less than those of the pedon. 5. snake bites.to 75-mm. Some hazards are sharpedged excavation tools. 2004).45 g cc-1. Method 3A2b is the calculations used to derive weight percentages from volume percentages of all the >2-mm material.4 Mechanical shaker with 9-mesh and 4-mesh sieves 5. if applicable. The visual volume estimates of the >75-mm fractions are subjective. sieving and weighing the 20.3 Sieves. the minimum specimen sizes ("dry" weights) that need to be sieved and weighed are 1. The volume estimates for any fractions that are >20 mm are converted to weight percentages. The weight estimates are laboratory measurements for the 2-to 20-mm or 2.1 Electronic balance. visual field volume estimates of the 20. 2.to 75-mm fraction should be done in the field.2 Trays. tared 5. Application Procedure 3A2a2 is used to determine weight percentages of the >2 mm fractions from volume estimates and weight determinations. The <20-mm fractions are sieved and weighed in the laboratory. This is the preferred method.3 20 mm. Summary of Method Visual field volume estimates are determined for any fractions that are >20 mm. Therefore. Equipment 5.0 and 60.3.to 75-mm fraction are used rather than laboratory weights of this fraction.to 75-mm fraction may be determined. If these measurements are unavailable.65 g cc-1 and a bulk density for the fine-earth fraction of 1.Particle-Size Distribution Analysis (3A) Particles >2 mm (3A2) Weight Estimates (3A2a) From Volume and Weight Estimates (3A2a2) Volume Estimates (3A2b) 1. 4. plastic. These volume estimates include.3. Samples received in the laboratory generally have a maximum weight of 4 kg.5 Rubber roller 70 . Refer to ASTM Standard Practice D 2488 (American Society for Testing and Materials.3. The total >2-mm fraction is reported on an oven-dry weight basis for whole soil. Instead of visual field volume estimates.2 4 mesh. field weights for the 20. The volume estimates are visual field estimates for any fractions that are >20 mm.4 76 mm. In order to accurately measure rock fragments with maximum particle diameters of 20 and 75 mm. If particle density and bulk density measurements are available. they are used in the calculations.to 75-mm fractions. 2 mm 5. Safety The main hazards are in the field during sample collection. and the >250-mm fractions. 3/4 in 5. 75. and falls. 3 in 5. 3.1 9 mesh. ±1-g sensitivity and 15-kg capacity 5. Interferences Soil variability and sample size are interferences to weight determinations of the >2mm particles. 4. The conversion of a volume estimate to a weight estimate assumes a particle density of 2.

Discard the >75-mm material.3 If field weight measurements are determined for the 20. Label and send to laboratory for analyses. Place a sub-sample of the <20-mm material in an 8-mL. 7. Discard the 20. Air-dry. and discarded in the field. A 60-kg sample may not be possible because of limitations of time and/or soil material. 45-kg (100-lb) capacity 5. and record weight. 71 .5 Process air-dry material on a flat.2 1 N HCl. 6. Weigh.7 Weigh soil material with diameters of 2 to 5 mm.8 Brown Kraft paper 6. For samples with easily crushed coarse fragments. Most laboratory samples do not contain 20. Repeat process four times. Procedure Field 7. Air-dry. Weight measurements for the 20. The >250-mm fraction includes stones and boulders with horizontal dimensions less than those of the pedon. volume estimates are more accurate than laboratory weights using small samples. 7. record weight. However. Weigh and record weight of <20-mm fraction.to 75-mm fraction.5. Laboratory 7. and record moist weight. Weigh sub-sample and record weight.4 Distribute the field sample on a plastic tray. Reagents 6. and discard.7 g of sodium hexametaphosphate (NaPO3)6 and 7. Refer to procedure 1B. 7. Thoroughly mix material by moving the soil from the corners to the middle of the processing area and then by redistributing the material. Dissolve 35. Soak in sodium hexametaphosphate solution for 12 h. plastic bag.5 cm 5. select sub-sample for preparation.to 75-mm fraction. metal plate that is covered with brown Kraft paper.to 75-mm fragments as this fraction is generally weighed.1 Reverse osmosis (RO) water 6. weigh the material that does not slake. Sieve clayey soils that contain many coarse fragments in the mechanical shaker.6 If more sample is received than is needed for processing.7 Scale.6 Metal plate. 7.2 Determine either weight measurements in pounds or visual field volume estimates in percentages for the 20. Sieve ≈ 60 kg of material to accurately measure rock fragments that have a maximum particle diameter of 75 mm.to 75-mm fragments.to 250-mm and for the >250-mm fractions.94 g of sodium carbonate (Na2C03) in L of distilled water.1 Determine volume estimates as percentages of soil mass for the 75. Roll and sieve until only the coarse fragments that do not slake in sodium hexametaphosphate solution remain on the sieve. and discard coarse fragments with diameters of 20 to 75 mm and 5 to 20 mm. 7. sieved. 76 x 76 x 0. Sieve this material with a 20-mm sieve.3 Sodium hexametaphosphate solution. sieve an entire horizon sample with a 76-mm sieve. Actual sample size may be 30 or 40 kg.to 75-mm fraction are the preferred method. Weigh and record weight of <75-mm fraction. weigh. weigh. substitute rubber roller for wooden rolling pin. Roll material with wooden rolling pin to crush clods to pass a 2-mm sieve. 7.

Cm x Dbm x lab datum 8. Volume Estimates (3A2b) 8.3 Use the preceding equation to calculate any individual fraction >j mm (j = any size fraction) by substituting an appropriate value of Dbm representing the fabric <j mm. Cm x 100 8.2 Use the following equation to convert all volume estimates to weight percentages for specified fractions.5 Use the following formula to convert laboratory data on a <2-mm weight basis to moist whole soil volume basis.45 g cc-1 for <2-mm fraction.45 g cc-1 and a Dp of 2.4 Use the following equation to determine the volume of the <2-mm fraction per unit volume of whole soil. 8.65 g cc-1. unless measured) x = [volume fragments > i mm]/[volume whole soil] where: i = size fraction above which volume estimates are made and below which weight percentages are determined.7 Use the following formula to determine the volume percentage of >2-mm fabric in whole soil. Cm = [Volume moist <2-mm fabric]/[Volume moist whole-soil] = [Dp (1-y) (1-x)]/[Dp (1-y) + Dbm (y)] where: Cm = Rock fragment conversion factor Volume moist whole soil = Volume of fine earth + rock fragments on moist whole-soil basis y = [weight material between 2 mm and i mm]/[weight material < i mm] 8. assume a Dbm of 1. If measurements are unavailable.1 Calculate weight percentages from volume percentages using measured bulk density (Dbm) and particle density (Dp). Percentage >2 mm (wt basis) = [100 Dp (x)]/[Dp (x) + Dbm (1-x)] where: Dp = Particle density (2.65 g cc-1. usually 20 or 75 mm in diameter 8. 100 (1-Cm) 72 .8. unless measured) Dbm = Bulk density (1. Calculations From Volume and Weight Estimates (3A2a2) 8.6 Use the following formula to determine the volume percentage of <2-mm fabric in whole soil.

respectively. as a soil characteristic. The SSL uses the bulk density notations of Dbf. oven-dry. Report Field 9. subscripts are added to the bulk density notation.8. Db33. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.to 5-mm fraction before slaking 9.3 Volume (%) 20. 1986). Bulk density is distinguished from particle density which is mass per unit volume of only the solid phase.to 75-mm fraction (not needed if weighed in field) 9. Dbod. Soil bulk density of a sample is the ratio of the mass of solids to the total or bulk volume. Philadelphia. This total volume includes the volume of both solids and pore space. Particle density excludes pore spaces between particles. to designate the water state of the sample when the volume was measured.4 Weight (lbs) <75-mm fraction 9. Standard Practice for Description and Identification of Soils (Visual-Manual Procedure).8 Weight (g) of air-dry processed soil sample 9. Vol. Changes in soil volume due to changes in water content will alter bulk density. 11.6 Weight (g) of field moist soil sample 9. Field-state (Dbf) is the bulk density of a soil sample at field-soil water content at time of sampling. and rewet.13 Weight (g) of sub-sample 2.08.7 Weight (g) of air-dry soil sample 9.1 Volume (%) >250-mm fraction (includes stones and boulders with horizontal dimensions smaller than size of a pedon) 9. Annual book of ASTM standards. Bulk density maybe highly dependent on soil conditions at the time of sampling. Therefore.to 5-mm fraction after slaking 10.11 Weight (g) 2. References American Society for Testing and Materials.5 Weight (lbs) 20-to 75-mm fraction Laboratory 9. 2004. is actually a function rather than a single value. but the volume of soil may change as water content changes (Blake and Hartge. Soil mass remains fixed. Soil and rock.9 Weight (g) 20-to 75-mm fraction 9.2 Volume (%) 75.to 5-mm fraction 9.10 Weight (g) 5.8 Use the following formula to report weight of <2-mm fabric per unit volume of whole soil for some soils. the mass and volume of rock fragments are subtracted from the total mass and volume. dimension stone. (Cm x Dbm) 9. Section 4. geosynthesis.12 Weight (g) of sub-sample 2. ASTM.to 20-mm fraction 9. Db. 04. Construction. As bulk density (Db) is usually reported for the <2-mm soil fabric. D 2488. and Dbr for field-state. The 33-kPa equilibration (Db33) is the bulk density of a soil sample that has been 73 .to 250-mm fraction 9. SOIL PHYSICAL AND FABRIC RELATED ANALYSES (3) Bulk Density (3B) Density is defined as mass per unit volume. Bulk density. PA. 33-kPa equilibration.

If the sample is large and inclusive of the desiccation cracks.R. The Dbr is used to determine the irreversible shrinkage of soils and subsidence of organic soils.C. DC. Sobecki. The bulk density of a weak or loose soil material for which the clod or core method is unsuitable may be determined by the compliant cavity method (procedure 3B3a). Topp (eds. And may also be hard for soils subject to a large increase if taken through a rewet cycle. DC. 1986. WI. 1990. respectively.B. 2nd. Grossman and Reinsch. p. In general. 5. Agric. 436. Monogr. and T.B. R. Symp.J. and 3B1d. Pringle.S. The determinations of these bulk density values.g. Grossman. W. If the water content is at or near field capacity. 201-228. as in some excavation procedures. Soil Sci. and re-equilibrated. Three excavation procedures have been used to determine Dbf as follows: (1) compliant cavity (3B3a).. Madison. there are two broad groupings of bulk density methods as follows: (1) one for soil materials coherent enough that a field-sample can be removed. ASA and SSSA. is coated. U. there are clod methods in which the sample has an undefined volume.. (1990).. Print. Part 4. 2nd ed. Grossman. Reinsch. and (2) the other for soils too fragile to remove a sample and an excavation operation must be performed. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. air-dried. No. Govt. Bulk density. The frame-excavation provides for a larger sample area and is advantageous where there is large. 1999. then again the sample and soil bulk density are the same. Part 1. 2002). USDA-NRCS. Office. On Advanced Technology in Natural Resource Management. The complete cylinder may be inserted (3B6a) or only part of the cylinder is inserted and the empty volume is subtracted from the total volume of the core (e. However.M.G. In J. if the sample is at a water content below field-capacity through drying after sampling or because the sample was taken below field-capacity. Physical methods. 363-382. ASA and SSSA.. Soil Survey Staff. References Blake. R. Hartge. R. Washington. Agron.H. Madison. G. In Int. The rewet (Dbr) is the bulk density of soil sample that has been equilibrated. 1999) of woodlands. 3B1b. ed. Bulk density also may be determined for field-moist soil cores of known volume (procedure 3B6a). Bigler. are described in procedures 3B1a. p. Systematics and field morphology for a use-dependent. and the volume is determined by submergence.D.) Methods of soil analysis. p. and Dbr. Georgetown Univ.H. and (3) frame excavation (3B5a) (Grossman and Reinsch.) Methods of soil analysis. Dbf. 3B1c. Am. Broderson. estimates of soil bulk density at intermediate field-water contents between field capacity and oven-dryness inclusive of desiccation crack space are discussed by Grossman et al. The difference between sample and soil bulk density is particularly large for oven-dry clods (Dod) of soils with high extensibility. Also under the former there are various methods in which a cylinder of known volume is obtained of soil sufficiently coherent that it remains in the cylinder. Physical and mineralogical methods.B.. Under the former. then desiccation cracks that occur in place are excluded from the soil and the sample bulk density exceeds that of the soil. 452-460. very local variability as found in the O horizons (Soil Survey Staff. Similarly. F. Dbod. 2nd ed. variable height method. Klute (ed. Washington. (2) ring excavation (3B4a). Dane and G.desorbed to 33kPa (1/3 bar). WI. Bulk density and linear extensibility. temporal soil data base for edaphological and environmental applications. and T. 9. Db33. Grossman and Reinsch (2002) discuss the manipulation of clod bulk densities (the sample) at water contents below field capacity to obtain an estimate of the soil bulk density at such water contents. In A. and K. Handb. 74 . 2002. The oven-dry (Dbd) is the bulk density of a soil sample that has been dried in an oven at 110°C. The complication concerning the difference between bulk density of the soil and that of the sample is particularly important for the clod method as presented here which permits determination of the volume at different water contents and hence volumes. 2002). desiccation cracks are closed and the bulk density (Db33 or Dbf if field-water is near field capacity) of the soil and of the sample are considered the same. Book Series No.

Grossman and Reinsch. Penetration can be reduced by spraying water on the clod followed by immediately dipping the clod in the plastic lacquer. and a lab coat. clods with high organic matter content may need to dry longer. Additional coats of plastic lacquer are applied in the laboratory. In closed buildings. The penetration of plastic lacquer into the voids of sandy or organic soils interferes with the corrections for mass and volume of the plastic coat and with the accuracy of water content determinations. Application Bulk density is used to convert data from a weight to a volume basis.. 1986. Dbf is particularly useful if the soil layers are at or above field capacity and/or the soils have low extensibility and do not exhibit desiccation cracks even if below field capacity. Holes in the plastic coating. Inc. which are detected by escaping air bubbles from submerged clod.Bulk Density (3B) Saran-Coated Clods (3B1) Field-State (Dbf) (3B1a) 1. One coat of plastic lacquer is applied in the field. Field-bulk density (Dbf ) offers the opportunity to obtain relatively cheaply bulk density information without the expense incurred to obtain water retention. A correction is made for the mass and volume of rock fragments and plastic coatings (Brasher et al. Interferences Errors are caused by non-representative samples. 2002). However. and the short-term exposure limit (STEL) is 300 ppm (Occupational Safety and Health Administration. 1989). use a fume hood. Washington.. to estimate saturated hydraulic conductivity. NW. Summary of Method Field-occurring fabric (clods) is collected from the face of an excavation. The whole soil bulk density may be overestimated because sampled clods frequently exclude the crack space between clods (Grossman and Reinsch. Manufacturing Chemists’ Association. and to identify compacted horizons. proper gloves. Safety Methyl ethyl ketone (MEK) is extremely flammable. Blake and Hartge. Loss of soil during the procedure will void the analyses because all calculations are based on the oven-dry soil mass. After the clod is dried in oven at 110°C. The 8-h time-weighted average (TWA) exposure limit is 200 ppm. Avoid physical contact. Use with adequate ventilation. 2002). Only field-occurring fabric (clods) should be sampled. In its field-water state or after equilibration. introduce errors in volume measurement. Additional information on the safe handling of MEK is available in Chemical Safety Data Sheet SD-83. Bulk density is reported for <2-mm soil fabric. 1966. No open flames or nearby operation of electrical equipment are permitted while using MEK. 4. Wash hands immediately after handling MEK. 1825 Connecticut Ave. 75 . An inadequate evaporation of the plastic solvent results in overestimation of the soil mass. Estimate or measurement errors of rock fragment density will affect the accuracy of the value for soil bulk density. the clod is weighed in air to measure its mass and in water to measure its volume. DC. Rock fragments may contain water which complicates the application to actual waterholding capacity. its mass and volume are determined again. Keep in tightly closed containers. Use safety glasses. 2. A type B fire extinguisher should be in close proximity in the laboratory. The MEK vapor is classified as a sensory irritant. Correction for rock fragments >2-mm requires either knowledge or assumption of the rock fragment density. A drying time of 1 h is usually sufficient time for evaporation of solvent. 3. The procedure 3B1a determines the bulk density value Dbf of a soil sample at field-soil water content at time of sampling.

8 Plexiglass water tank mounted on a fulcrum and lever to elevate tank 5. No procedure for sampling clods is applicable to all soils. The SSL uses a 28-awg coated copper wire. If roots are present.3 Plastic bags.1 Electronic balance. available from Dow Chemical Company. If the value of Dbf is required.7 Hook assembly for weighing below balance 5. 6. prepare a clod by gently cutting or breaking protruded peaks and compacted material from clod. Store plastic lacquer in covered plastic or steel containers. For the initial field and laboratory coatings. high speed stirrer while slowly adding resin.6 Plastic lacquer.13 Silt loam soil 5. ±0. and Al in solution. 25. Fill to the bottom of handle rivet.1 Collect field-occurring clods. 127 x 89 x 330 mm 5. Three clods per horizon are recommended. Acetone may be substituted for MEK.01-g sensitivity 5. 7. Equipment 5. Procedure Field 7.5 Dow Saran F-310 Resin. use the 1:4 plastic lacquer. The 1:7 plastic lacquer is used to conserve the resin and to reduce cost. The SSL uses a corrugated box with compartments.10 Sieve.15 Spray bottle 5. Fill a 3. In the laboratory. Prepare plastic lacquer with resin to solvent ratios of 1:4 and 1:7 on a weight basis.4 Liquid detergent. ≈ 100 to 200 cm3 in volume (fist-sized). 1). No. Cu. 2). Reagents 6. moisten surface with a fine mist of water. stir solvent with a non-sparking.2 Make a clothesline by stretching a rope between two fixed points. Use 1:7 plastic lacquer for the last two laboratory coats. Stir plastic lacquer for 15 min at 25°C.2 Rigid shipping containers. respectively.9 Oven. 1 mL.4-mm (1-in) diameter paper tag. It is important that these clods be as representative of the bulk sample volume as possible. From this piece.5 Hairnets 5. mix solvent with a wooden stick.Saran F-310 resin will decompose rapidly at temperatures >200°C releasing hydrogen chloride gas.14 Hot plate 5. practical (2-butanone) 6. store 76 . 7.3 Alcohol 6.6 Stock tags. In the field.11 Rope. from the face of the excavation. 5. 5. Remove a piece of soil larger than clod from the face of sampling pit. The SSL uses Liqui-Nox. 110°C 5.8-L (1-gal) metal paint can with 2700 ± 200 mL of solvent. 6. Zn. Suspend clod from clothesline to dry (Fig. If clod is dry. 3 m 5.12 Clothespins 5. Avoid all contact with strong bases. with metal rim 5. 5.1 Methyl ethyl ketone (MEK). Dry clod for 30 min or until odor of solvent dissipates.2 Water 6. Tie clod with fine copper wire or place clod in a hairnet. Add 540 or 305 g of resin to make 1:4 or 1:7 plastic lacquer. 6. 10 (2-mm openings) 5. trim roots with shears. Adjust field-sampling techniques to meet field-conditions at time of sampling. The SSL constructs a tin enclosure over hot plate with a chimney and duct to transfer vapor to water stream.4 Wire.16 Liquid vapor trap. Avoid contact with Fe. Quickly dip entire clod into plastic lacquer (Fig.

Weigh oven-dry clod in air (WODC) and in water (WODCW) and record weights.7 Dry clod in an oven at 110°C until weight is constant. Cut the copper wire and loop around the clod.2 MPC = [(CC2 . Calculations 8. 7. and add hot water. remove them from clod. Wait 12 min and then dip clod in 1:7 plastic lacquer. Wait 55 min and then reweigh clod. Suspend the clod below the balance.WMCW)/WD] .1 Dbf = [WODC . Correct for rock fragments if these fragments can withstand breakdown when dry soil is placed abruptly in water or calgon.4 Prepare a round stock tag with sample identification number. The coating loses 10 to 20% of its air-dry weight when dried in oven at 110°C. allow longer drying time. 7. Heat clod on hot plate in excess of 200°C for 3 to 4 h.3 Pack clods in rigid containers to protect them during transport. square-hole sieve. If clod has adsorbed >3% plastic by clod weight or smells excessively of solvent.8 If clod contains >5% rock fragments by weight.clods in waterproof plastic bags as soon as coating dries because coating is permeable to water vapor. do not correct clod mass and volume measurement for rock fragments. submerge in water.ODPC – TAG]/{[(CC2 .3)} where: Dbf = Bulk density in g cc-1 of <2-mm fabric at field-sampled water state WODC = Weight of oven-dry coated clod RF = Weight of rock fragments ODPC = MPC x 0. Laboratory 7. then reweigh clod and record weight (CC2).6 The clod should be waterproof and ready for volume measurement by water displacement. clod should appear black and charred. Record weight (TAG) of tag and wire. Record weight of clod (CC1). 7. 7. Determine rock fragment density by weighing them in air to obtain their mass and in water to obtain their volume. Loop fine copper wire around clod.RF . leaving a tail to which round stock tag is attached.85.5 Dip clod in 1:4 plastic lacquer. 7. Dry and record weight (RF) of rock fragments that are retained on the sieve. After heating. lightly coat with liquid detergent. 7. and record weight (WMCW). The coating has an air-dry density of ≈ 1. Cover hot plate with a liquid vapor trap.3 g cm-3.9 Wet sieve the cool soil through a 2-mm. The plastic coating disintegrates at temperatures above 200°C. weight of oven-dry plastic coat TAG = Weight of tag and wire CC2 = Weight of tag and wire WMCW = Weight of coated clod in water before oven drying WD = Water density PD = Density of rock fragments 8. 7.10 Correct bulk density for weight and volume of plastic coating. 8.(MPC/1. Use a fume hood. Place clod in a beaker and place on hot plate. Wait 7 min and then dip clod in 1:7 plastic lacquer.CC1) + FCE] x RV 77 .(RF/PD) . If rock fragments are porous and have a density similar to soil sample. Remove clod from hot plate.

Reinsch. Part 4. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. ASA and SSSA. Topp (eds. R.where: MPC = Weight of plastic coat before oven-drying CC1 = Weight of clod before three laboratory plastic coats RV = Percent estimate of remaining clod volume after cutting to obtain flat surface (≈ 80%) 8. 1966. In J.B. Madison. U.R. G. 11.(RF/PD) (MPC/1. Agron. V. Report Bulk density is reported to the nearest 0. Am.S.ODPC – TAG]}x 100 where: Wf = Percent water weight in sampled clod 9. Volassis. 1986.. 54. Dane and G. 202-228.R.H. Govt. 78 . Washington. and S. DC. Hartge. Brasher. Vol.T. Physical and mineralogical methods. Grossman. Klute (ed. Soil Sci. 10. Madison. Monogr. 29 CFR Part 1910.C. 5. final rule. p. 2nd ed.01g cm-3.E. 12. and T. 2002.. Soil Sci. p.5 Wf = {[(CC2 – MPC) – (WODC – ODPC)]/[WODC . No. Franzmeier. Use of saran resin to coat natural soil clods for bulk density and water retention measurements. WI. In A.3)} where: Dbod = Bulk density in g cm-3 <2-mm fabric at oven dryness WODCW = Weight of oven-dry coated clod in water 8. 2452-2453. D. Bulk density.TAG]/{[(WODC – WODCW)/WD] . Occupational Safety and Health Administration. Bulk density and linear extensibility. 363-382. 1989. Air contaminants. ASA and SSSA.5 x [(CC2 -CC1)/3] where: FCE = Estimate of field-applied plastic coat 8. Davidson.) Methods of soil analysis. Print. 101:108. Physical methods.3 FCE = 1. p. WI. B. References Blake.RF . 9.G. Office. Federal Register.4 Dbod = [WODC – RF – ODPC . and K. Book Series No. Part 1.P.) Methods of soil analysis.H.

Fig. 79 .Fig. 1. 2. clods are tied to clothesline to dry. After dipping. Dipping clods with hairnet in plastic-lacquer.

No open flames or nearby operation of electrical equipment are permitted while using MEK. its mass and volume are determined again. Wash hands immediately after handling MEK.. Rock fragments may contain water. Penetration can be reduced by spraying water on the clod followed by immediately dipping the clod in the plastic lacquer. 1989). Additional coats of plastic lacquer are applied in the laboratory. proper gloves. The MEK vapor is classified as a sensory irritant. Keep in tightly closed containers. to determine the coefficient of linear extensibility. Avoid physical contact. Interferences Errors are caused by non-representative samples. Only field-occurring fabric (clods) should be sampled. Dipping should be done as quickly as possible to reduce penetration of plastic. which complicates the application to actual waterholding capacity. The 8-h time weighted average (TWA) exposure limit is 200 ppm. introduce errors in volume measurement. clods with high organic matter content may need to dry longer. 2002). The procedure 3B1b determines the bulk density value (Db1/3) of a soil sample equilibrated at 33 kPa. Clods placed in an unsealed plastic bag can lose moisture during storage prior to analysis. then Db1/3 values for 33 kPa will be erroneous. 2. 4. which are detected by escaping air bubbles from submerged clod. the clod is weighed in air to measure its mass and in water to measure its volume. to estimate saturated hydraulic conductivity. After the clod is dried in the oven at 110°C. The clod is desorbed to 33 kPa. A type B fire extinguisher should be in close proximity in the laboratory. Summary of Method Field-occurring fabric (clods) are collected from the face of an excavation. The whole soil bulk density may be overestimated because sampled clods frequently exclude the crack space between clods (Grossman and Reinsch. Completely seal the plastic storage bag to prevent drying. A correction is made for the mass and volume of rock fragments and for plastic coatings (Brasher et al. Safety Methyl ethyl ketone (MEK) is extremely flammable. Holes in the plastic coating. 1986). However. and a lab coat. An inadequate evaporation of plastic solvent results in overestimation of the soil mass. 3. Use with adequate ventilation. and the short-term exposure limit (STEL) is 300 ppm (Occupational Safety and Health Administration. If clods irreversibly dry below 33-kPa-water content. Use safety glasses. One coat of plastic lacquer is applied in the field. Application Bulk density is used to convert data from a weight to a volume basis. Additional information on the safe handling of MEK is 80 . Correction for rock fragments >2-mm requires either knowledge or assumption of the rock fragment density. In closed buildings. Loss of soil during the procedure will void the analyses because all calculations are based on the oven-dry soil mass. use a fume hood.Bulk Density (3B) Saran-Coated Clods (3B1) 33-kPA Desorption (Db33) (3B1b) 1. Estimate or measurement errors of rock fragment density will affect the accuracy of the value for soil bulk density. After equilibration. 1966. The penetration of plastic lacquer into the voids of sandy and organic soils interferes with the corrections for mass and volume of the plastic coat and with the accuracy of water content determinations. Bulk density is reported for <2-mm soil fabric. and to identify compacted horizons. Blake and Hartge. A drying time of 1 h is usually sufficient time for evaporation of solvent.

9 Hook assembly for weighing below balance 5.6 Wire. The 1:7 plastic lacquer is used to conserve the resin and to reduce cost. Equipment 5.13 Rope.14 Clothespins 5.1 Methyl ethyl ketone (MEK).8-L (1-gal) metal paint can with 2700 ±200 mL of solvent. 25.3 Air pressure. respectively. Inc. The SSL constructs a tension table by placing porous firebricks. 6. 10 (2-mm openings) 5. The SSL constructs a tin enclosure over hot plate with a chimney and duct to transfer vapor to water stream.4 Rigid shipping containers. In the laboratory.7 Hairnets 5. Store plastic lacquer in covered plastic or steel containers.25 Tension table. 3 m 5. use the 1:4 plastic lacquer. Avoid contact with Fe.5 Plastic bags. 5. 81 . 1825 Connecticut Ave. For the initial field and laboratory coatings. 1 mil. 5. The SSL uses a 28-awg coated copper wire.12 Sieve. Acetone may be substituted for MEK. Reagents 6. mix solvent with a wooden stick. Prepare plastic lacquer with resin to solvent ratios of 1:4 and 1:7 on a weight basis. 5. covered with reinforced paper towels.17 Silt loam soil 5.8 bar) 5. The SSL uses a corrugated box with compartments. Fill a 3.8 Stock tags. Use 1:7 plastic lacquer for the last two laboratory coats. with metal rim 5. 110°C 5. 6.19 Desiccator with ceramic plate 5.. DC.24 Reinforced paper towels or cheesecloth 5.5 Dow Saran F-310 Resin.10 Plexiglass water tank mounted on a fulcrum and lever to elevate tank 5. NW.available in Chemical Safety Data Sheet SD-83.2 Pressure plate extractor with porous ceramic plate. Washington. 5.6 Plastic lacquer.15 Knife 5. ±0. Avoid all contact with strong bases. 33-kPa 5. 127 x 89 x 330 mm 5. Saran F-310 resin will decompose rapidly at temperatures >200°C releasing hydrogen chloride gas. Manufacturing Chemists’ Association. high-speed stirrer while slowly adding resin. available from Dow Chemical Company.2 Water 6.22 Spray bottle 5. The SSL uses Liqui-Nox.23 Liquid vapor trap. practical (2-butanone) 6.16 Tile cut-off saw with diamond blade 5. No. Stir plastic lacquer for 15 min at 25°C.1 Electronic balance.3 Alcohol 6. and Al in solution.21 Metal probe 5. In the field. in a tub of water. Fill to the bottom of handle rivet. 5.20 Vacuum. Zn. 80 kPa (0.18 Hot plate 5. Cu. Add 540 or 305 g of resin to make 1:4 or 1:7 plastic lacquer.4 Liquid detergent.4-mm (1-in) diameter paper tag.11 Oven. stir solvent with a non-sparking.01-g sensitivity 5. 6.

Record weight of clod (CC1). clod is at equilibrium. 7. or by weight comparison. allow longer drying time. procedure 3B1a). Use in-house vacuum and apply suction until clod has equilibrated at saturation. After 55 min.7 If cut clod does not adsorb water. store clods in waterproof plastic bags as soon as coating dries because coating is permeable to water vapor. Remove clod and record weight (WSC). Close container and secure lid. cover ceramic plate with a 5-mm layer of silt loam soil and saturate with water. From this piece.2). Place a sheet of reinforced paper towel or cheesecloth over the silt loam soil. If roots are present. Three clods per horizon are recommended. If WMC > WSC. then reweigh clod. ≈ 100 to 200 cm3 in volume (fist-sized). Extraction usually takes 3 to 4 wk. maintained at 5-cm tension (Fig. If clod has adsorbed >3% plastic by clod weight or smells excessively of solvent. Place surface of cut clod on paper towel.9 Dip clod in the 1:4 plastic lacquer. prepare a clod by gently cutting or breaking protruded peaks and compacted material from clod. Add a few mL of alcohol. Record weight (TAG) of tag and wire. If the clod is dry. Apply gauged air pressure of 33 kPa. leaving a tail to which round stock tag is attached. Submerge only the surface of clod in the water. Suspend clod from clothesline to dry (See Fig. trim roots with shears. 2. No procedure for sampling clods is applicable to all soils. Cut the copper wire and loop around the clod (Fig. 7. 7. When water ceases to discharge from outflow tube.2 Make a clothesline by stretching a rope between two fixed points. Loop fine copper wire around clod. cut a flat surface on the clod. Compare WMC to WSC. procedure 3B1a). Wait 7 min and then dip clod in 1:7 plastic lacquer. touching. If clod has adsorbed >3% plastic by weight or smells excessively of solvent. Wait 7 min and then dip clod in 1:7 plastic lacquer. If the value of Dbf is required.4 Prepare a round stock tag with sample identification number. allow longer drying time. 7. When clod has reached equilibrium.6 With a diamond saw. Remove a piece of soil larger than clod from the face of sampling pit. Procedure Field 7. To provide good contact between clod and ceramic plate. Remove clod and record weight (WMC). 82 . 1). remove clod and record weight (WSC). 7. Wait 12 min and then dip clod in 1:7 plastic lacquer.1 Collect field-occurring clods. It is important that these clods be as representative of the bulk sample volume as possible. 7. from the face of the excavation. moisten surface with a fine mist of water. Tie clod with fine copper wire or place clod in a hairnet. Laboratory 7.3 Pack clods in rigid containers to protect them during transport.5 Dip clod in 1:4 plastic lacquer. Wait 55 min and then reweigh clod. Adjust field-sampling techniques to meet field-conditions at time of sampling. Periodically check clod to determine if it has reached equilibrium by inserting metal probe. Wait 12 min and dip clod in 1:7 plastic lacquer. Wait 12 min and then dip clod in 1:7 plastic lacquer.8 Place clod in a pressure plate extractor. reweigh clod and record weight (CC3). 1. then reweigh clod and record weight (CC2). place clod in a desiccator on a water-covered plate with a 0-cm tension. Quickly dip entire clod into plastic lacquer (See Fig. 7. equilibrate clod on tension table and repeat desorption process. Dry clod for 30 min or until odor of solvent dissipates. Place cut clod surface on a tension table.7.

RF . square-hole sieve. After heating. Use a fume hood. Remove clod from hot plate. 7. Place clod in a beaker and place on hot plate. 7. The plastic coating disintegrates at temperatures above 200°C. Determine rock fragment density by weighing them in air to obtain their mass and in water to obtain their volume.2 MPC1 = {[(CC2 .11 Dry clod in an oven at 110°C until weight is constant. 7. Suspend clod below the balance. do not correct clod mass and volume measurement for rock fragments.3)} where: Db33 WODC RF TAG ODPC CC3 WD PD MPC1 WMCW = Bulk density in g cc-1 of <2-mm fabric at 33-kPa tension = Weight of oven-dry coated clod = Weight of rock fragments = Weight of tag and wire = MPC1 x 0. Heat clod on hot plate in excess of 200°C for 3 to 4 h.CC1) + FCE] x RV} + (CC3-WMC) where: MPC1 = Weight of plastic coat before oven-drying CC2 = Weight of clod after three laboratory plastic coats CC1 = Weight of clod before three laboratory plastic coats WMC = Weight of coated clod equilibrated at 33-kPa tension RV = Percent estimate of remaining clod volume after cutting to obtain flat surface (≈ 80%) 8. The coating loses 10 to 20% of its air-dry weight when dried in oven at 110°C. Correct for rock fragments if these fragments can withstand breakdown when dry soil is placed abruptly in water or calgon.7. and record weight (WMCW).13 Wet sieve the cool soil through a 2-mm. The coating has an air-dry density of ≈ 1. remove them from clod.12 If clod contains >5% rock fragments by weight. weight of oven-dry plastic coat = Weight of equilibrated clod after four additional plastic coats = Water density = Density of rock fragments = Weight of plastic coat before oven-drying = Weight in water of coated clod equilibrated at 33-kPa tension 8.(MPC1/1.WMCW)/WD] .1 Db33 = [WODC .85.10 The clod should be waterproof and ready for volume measurement by water displacement. If rock fragments are porous and have a density similar to soil sample.3g cm-3.(RF/PD) .5 x [(CC2 -CC1)/3] where: FCE = Estimate of field-applied plastic coat 83 . 8.ODPC – TAG]/{[(CC3 .3 FCE = 1. Cover hot plate with a liquid vapor trap.14 Correct bulk density for weight and volume of plastic coating. Dry and record weight (RF) of rock fragments that are retained on the sieve. and add hot water. Weigh oven-dry clod in air (WODC) and in water (WODCW) and record weights. 7. submerge in water. lightly coat with liquid detergent. Calculations 8. clod should appear black and charred.

Brasher.B.R. Bulk density and linear extensibility. 201-228.. Govt. p.TAG]/ {[(WODC . References Blake. Part 4. 363-382. Physical and mineralogical methods. 54. Madison.H. Occupational Safety and Health Administration.) Methods of soil analysis. Use of saran resin to coat natural soil clods for bulk density and water retention measurements. 10. R. 29 CFR Part 1910.C. WI. In A.4 Dbod = [WODC– RF– ODPC . Physical methods.P. Dane and G. 1966. In J. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. U.H. Report Bulk density is reported to the nearest 0. DC. and T. and S. 2002.8. Part 1. Grossman. Am. Madison. Air contaminants. Book Series No.S. oven-dry fabric WODCW = Weight of oven-dry clod coated in water 8.RF . Franzmeier. Klute (ed.ODPC)]/[(WODC .T. Soil Sci. p. Office. and K. No.01g cm-3. B. G.G. Hartge. Soil Sci.(RF/PD) (MPC1/1. Davidson. Federal Register. 1989. 11. D. 2nd ed. Vol. Volassis. ASA and SSSA.E. ASA and SSSA. Bulk density. V. Monogr. Topp (eds. 9. Agron. 1986. 84 .) Methods of soil analysis. Print.3)} where: Dbod = Bulk density in g cc-1 <2-mm fabric. final rule.5 W33 ={[(CC3 – MPC1) – (WODC .R. WI. Washington.. p. Reinsch.ODPC – TAG)]} x 100 where: W33 = Percent water weight retained at 33-kPa tension 9. 101:108. 5. 2452-2453. 12.WODCW)/WD] .

the clod is placed on a tension table. 1. 85 . After a flat surface on the clod is cut with a diamond saw. 2. maintained at 5-cm tension. Fig. A round stock tag with sample identification number is prepared. The cut copper wire is looped around the clod.Fig.

Application Bulk density is used to convert data from a weight to a volume basis. Use with adequate ventilation. 1986). Avoid physical contact. Rock fragments may contain water. Loss of soil during the procedure will void the analyses because all calculations are based on the oven-dry soil mass. and the short-term exposure limit (STEL) is 300 ppm (Occupational Safety and Health Administration. Additional coats of plastic lacquer are applied in the laboratory. Additional information on the safe handling of MEK is available in Chemical Safety Data Sheet SD-83.. Correction for rock fragments >2-mm requires either knowledge or assumption of the rock fragment density. clods with high organic matter content may need to dry longer. The MEK vapor is classified as a sensory irritant. A type B fire extinguisher should be in close proximity in the laboratory. A drying time of 1 h is usually sufficient time for evaporation of solvent. A correction is made for the mass and volume of rock fragments and for plastic coatings (Brasher et al. The clod is dried in an oven at 110°C and then weighed in air to measure its mass and in water to measure its volume. 3. Washington. Holes in the plastic coating. Cu. Estimate or measurement errors of rock fragment density will affect the accuracy of the value for soil bulk density. An inadequate evaporation of plastic solvent results in overestimation of the soil mass. The procedure 3B1c determines the bulk density value (Dbod) of an ovendry soil sample. The whole soil bulk density may be overestimated because sampled clods frequently exclude the crack space between clods (Grossman and Reinsch. 4. Use safety glasses. One coat of plastic lacquer is applied in the field. Inc. and a lab coat. which are detected by escaping air bubbles from submerged clod. Safety Methyl ethyl ketone (MEK) is extremely flammable. Interferences Errors are caused by non-representative samples. The 8-h time weighted average (TWA) exposure limit is 200 ppm. 1966. 1989). Penetration can be reduced by spraying water on the clod followed by immediately dipping the clod in the plastic lacquer. Bulk density is reported for <2-mm soil fabric.. Avoid contact with Fe.Bulk Density (3B) Saran-Coated Clods (3B1) Oven-Dry (Dbod) (3B1c) 1. introduce errors in volume measurement. Summary of Method Field-occurring fabric (clods) is collected from the face of an excavation. Blake and Hartge. Manufacturing Chemists’ Association. DC. In closed buildings. proper gloves. which complicates the application to actual waterholding capacity. Avoid all contact with strong bases. Saran F-310 resin will decompose rapidly at temperatures >200°C releasing hydrogen chloride gas. NW. and to identify compacted horizons. Avoid physical contact. The penetration of plastic lacquer into the voids of sandy or organic soils interferes with the corrections for mass and volume of the plastic coat and with the accuracy of water content determinations. 86 . Dipping should be done as quickly as possible to reduce penetration of plastic. 2. and Al in solution. 1825 Connecticut Ave. to estimate saturated hydraulic conductivity. No open flames or nearby operation of electrical equipment are permitted while using MEK. use a fume hood. Wash hands immediately after handling MEK. Zn. Only field-occurring fabric (clods) should be sampled. Keep in tightly closed containers. 2002). However. to determine the coefficient of linear extensibility.

4 Wire. The SSL constructs a tin enclosure over hot plate with a chimney and duct to transfer vapor to water stream. Dry clod for 30 min or until odor of solvent dissipates. 5. The SSL constructs a tension table by placing porous firebricks. The SSL uses a corrugated box with compartments. In the field.3 Liquid detergent.7 Hook assembly for weighing below balance 5. practical (2-butanone). Three clods per horizon are recommended. From this piece.5 Plastic lacquer.1 Electronic balance. 3 m 5.16 Tension table. stir solvent with a non-sparking. Fill a 3. If the value of Dbf is required. If the clod is dry. 6. 6. store clods in waterproof plastic bags as soon as coating dries because coating is permeable to water vapor. 87 .8-L (1-gal) metal paint can with 2700 ±200 mL of solvent. 6. procedure 3B1a).14 Spray bottle 5. 7. ±0.10 Sieve. It is important that these clods be as representative of the bulk sample volume as possible. no. in a tub of water. available from Dow Chemical Company.15 Liquid vapor trap. Quickly dip entire clod into plastic lacquer (See Fig. 1 mil.1 Methyl ethyl ketone (MEK). The 1:7 plastic lacquer is used to conserve the resin and to reduce cost. 2. Acetone may be substituted for MEK. 6. Reagents 6.5 Hairnets 5.2 Rigid shipping containers. ≈ 100 to 200 cm3 in volume (fist-sized). Adjust field-sampling techniques to meet field conditions at time of sampling. covered with reinforced paper towels. mix solvent with a wooden stick. The SSL uses a 28-awg coated copper wire.11 Rope. from the face of the excavation. In the laboratory. 5. prepare a clod by gently cutting or breaking protruded peaks and compacted material from clod. 25.5.3 Pack clods in rigid containers to protect them during transport.6 Stock tags. Equipment 5. Prepare plastic lacquer with resin to solvent ratios of 1:4 and 1:7 on a weight basis. 127 x 89 x 330 mm 5. Stir plastic lacquer for 15 min at 25°C. trim roots with shears. Fill to the bottom of handle rivet. respectively. procedure 3B1a). 10 (2-mm openings) 5. 6. Remove a piece of soil larger than clod from the face of sampling pit.9 Oven.1 Collect field-occurring clods.8 Plexiglass water tank mounted on a fulcrum and lever 5. moisten surface with a fine mist of water. high-speed stirrer while slowly adding resin. Use 1:7 plastic lacquer for the last two laboratory coats. Add 540 or 305 g of resin to make 1:4 or 1:7 plastic lacquer.13 Hot plate 5. Procedure Field 7. 1. 110°C 5.4-mm (1-in) diameter paper tag with metal rim 5.4 Dow Saran F-310 Resin. 5. use the 1:4 plastic lacquer. Tie clod with fine copper wire or place clod in a hairnet. The SSL uses Liqui-Nox.12 Clothespins 5. For the initial field and laboratory coatings. 7.2 Water. No procedure for sampling clods is applicable to all soils. 7. If roots are present.3 Plastic bags.2 Make a clothesline by stretching a rope between two fixed points.01-g sensitivity 5. Suspend clod from clothesline to dry (See Fig. Store plastic lacquer in covered plastic or steel containers.

Determine rock fragment density by weighing them in air to obtain their mass and in water to obtain their volume. 7. The plastic coating disintegrates at temperatures above 200°C. Correct for rock fragments if these fragments can withstand breakdown when dry soil is placed abruptly in water or calgon. 7.3 g cm-3. then reweigh clod and record weight (CC2).9 Correct bulk density for weight and volume of plastic coating. Dry and record weight (RF) of rock fragments that are retained on the sieve. Cover hot plate with a liquid vapor trap. 7.6 Dry clod in an oven at 110°C until weight is constant. Remove clod from hot plate. weight of oven-dry plastic coat WD = Water density PD = Density of rock fragments WODCW = Weight of oven-dry coated clod in water 8. Record weight (TAG) of tag and wire. Wait 7 min and then dip clod in 1:7 plastic lacquer. remove them from clod. If rock fragments are porous and have a density similar to soil sample. 7.3)} where: = Bulk density in g cm-3 of <2-mm. Weigh oven-dry clod in air (WODC) and in water (WODCW) and record weights.(RF/PD) .5 Dip clod in 1:4 plastic lacquer. Cut the copper wire and loop around the clod. The coating loses 10 to 20% of its air-dry weight when dried in oven at 110°C. allow longer drying time. Record weight of clod (CC1). leaving a tail to which round stock tag is attached. square. If clod has adsorbed >3% plastic by clod weight or smells excessively of solvent. Loop fine copper wire around clod. oven-dry fabric Dbod WODC = Weight of oven-dry coated clod RF = Weight of rock fragments TAG = Weight of tag and wire ODPC = MPC1 x 0.Laboratory 7.2 MPC = [(CC2 .8 Wet sieve the cool soil through a 2-mm. do not correct clod mass and volume measurement for rock fragments. clod should appear black and charred. The coating has an air-dry density of ≈ 1. 7. and add hot water.RF-ODPC – TAG]/{[(WODC – WODCW)/WD] . If rock fragments are porous and have a density similar to soil sample. Wait 55 min and then reweigh clod. 8.CC1) + FCE] x RV where: MPC = Weight of plastic coat before oven-drying CC2 = Weight of clod after three laboratory plastic coats CC1 = Weight of clod before three laboratory plastic coats RV = Percent estimate of remaining clod volume after cutting to obtain flat surface (≈ 80%) 88 .4 Prepare a round stock tag with sample identification number. Place clod in a beaker and place on hot plate. After heating. Heat clod on hot plate in excess of 200°C for 3 to 4 h.(MPC/1.1 Dbod = [WODC.hole sieve.85. lightly coat with liquid detergent. Calculations 8.7 If clod contains >5% rock fragments by weight. Wait 12 min and then dip clod in 1:7 plastic lacquer. Use a fume hood. do not correct clod mass and volume measurement for rock fragments.

3 FCE = 1. Am. After the clod is dried in the oven at 110°C. R. WI. Madison. 1986. its mass and volume are determined again. G. Occupational Safety and Health Administration. Topp (eds. Additional coats of plastic lacquer are applied at the laboratory.E. 1966. In J. Interferences Errors are caused by non-representative samples. Agron. B. Vol. Madison. ASA and SSSA. Reinsch. and S. Use of saran resin to coat natural soil clods for bulk density and water retention measurements. 9.R..8. 2nd ed. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Physical and mineralogical methods. The rewet bulk density (Dbr) is used to determine irreversible shrinkage of soils and subsidence of organic soils. and its mass and volume remeasured. Dane and G. Only field-occurring fabric (clods) should be sampled. Hartge. Bulk Density (3B) Saran-Coated Clods (3B1) Rewet (Dbr) (3B1d) 1. Air contaminants. V. 201-228. to estimate saturated hydraulic conductivity.R. 3. 2452-2453. DC. Bulk density. References Blake. 1986.5 x [(CC2 -CC1)/3] where: FCE = Estimate of field-applied plastic coat 9. and to identify compacted horizons. final rule. Grossman. Franzmeier. Report Bulk density is reported to the nearest 0. ASA and SSSA. 54.T. Monogr.. After equilibration. No. and K. 10. Volassis. 29 CFR Part 1910. U. Soil Sci. Washington. 2002). 1989.) Methods of soil analysis. The whole soil bulk density may be overestimated because sampled clods frequently exclude the crack space between clods (Grossman and Reinsch.01g cm-3. 101:108. 5. Print. Bulk density and linear extensibility..B. and T. 12. The procedure 3B1d determines the bulk density value (Dbr) of a re-wetted soil sample. A correction is made for the mass and volume of rock fragments and for plastic coatings (Brasher et al. to determine the coefficient of linear extensibility. 11. Summary of Method Field-occurring fabric (clods) is collected from the face of an excavation. re-equilibrated. Grossman and Reinsch. One coat of plastic lacquer is applied in the field. The clod is air-dried.H. D.P. Penetration can be reduced by spraying water on the clod followed by 89 . p. Klute (ed.S. Federal Register.) Methods of soil analysis. The penetration of plastic lacquer into the voids of sandy or organic soils interferes with the corrections for mass and volume of the plastic coat and with the accuracy of water content determinations. the clod is weighed in air to measure its mass and in water to measure its volume. p. 1966. WI..G. p. Govt. 2002).C. Part 1. Part 4. 2. Soil Sci. Office. Physical methods. 2002. Book Series No. Blake and Hartge. In A. 363-382. Brasher. Davidson. Application Bulk density is used to convert data from a weight to a volume basis.H.

The SSL uses a 28-awg coated copper wire. Avoid all contact with strong bases. Avoid contact with Fe. The 8 h time weighted average (TWA) exposure limit is 200 ppm.21 Metal probe 5. Holes in the plastic coating. use a fume hood.16 Tile cut-off saw with diamond blade 5. DC.15 Knife 5.14 Clothespins 5. 1 mil. 80 kPa. 33-kPa 5. with metal rim 5.17 Silt loam soil 5.4-mm (1-in) diameter paper tag. Wash hands immediately after handling MEK. Zn.8 bar) 5. Cu. A type B fire extinguisher should be in close proximity in the laboratory.20 Vacuum. and Al in solution. In closed buildings. 5. Bulk density is reported for <2-mm soil fabric. Equipment 5. and the short term exposure limit (STEL) is 300 ppm (Occupational Safety and Health Administration. Additional information on the safe handling of MEK is available in Chemical Safety Data Sheet SD-83. 127 x 89 x 330 mm 5. A drying time of 1 h is usually sufficient time for evaporation of solvent.18 Hot plate 5. and a lab coat.10 Plexiglass water tank mounted on a fulcrum and lever to elevate tank 5. The MEK vapor is classified as a sensory irritant. 4. which are detected by escaping air bubbles from submerged clod. Inadequate drying results in overestimation of the soil mass.11 Oven.01-g sensitivity 5. However. Use safety glasses. The SSL uses a corrugated box with compartments. Washington. ±0.4 Rigid shipping containers. Manufacturing Chemists’ Association. 5. Saran F-310 resin will decompose rapidly at temperatures >200°C releasing hydrogen chloride gas. proper gloves. Dipping should be done as quickly as possible to reduce penetration of plastic. 1989).3 Air pressure. 10 sieve (2-mm openings) 5. clods with high organic matter content may need to dry longer.2 Pressure plate extractor with porous ceramic plate. Use with adequate ventilation. Rock fragments may contain water.12 Sieve.6 Wire. Loss of soil during the procedure will void the analyses because all calculations are based on the oven-dry soil mass.5 Plastic bags. Correction for rock fragments >2-mm requires either knowledge or assumption of the rock fragment density. 5.13 Rope.8 Stock tags. 1825 Connecticut Ave. 3 m 5. 25. Estimate or measurement errors of rock fragment density will affect the accuracy of the value for soil bulk density. 110°C 5.. which complicates the application to actual waterholding capacity. An inadequate evaporation of plastic solvent results in overestimation of the soil mass. introduce errors in volume measurement.22 Spray bottle 90 . No open flames or nearly operation of electrical equipment are permitted while using MEK. No. NW.1 Electronic balance.7 Hairnets 5. Avoid physical contact. Inc. Avoid physical contact. Safety Methyl ethyl ketone (MEK) is extremely flammable.immediately dipping the clod in the plastic lacquer. (0. 5. Keep in tightly closed containers.9 Hook assembly for weighing below balance 5.19 Desiccator with ceramic plate 5.

2 Make a clothesline by stretching a rope between two fixed points. 7. Prepare plastic lacquer with resin to solvent ratios of 1:4 and 1:7 on a weight basis. Acetone may be substituted for MEK.6 With a diamond saw.1 Methyl ethyl ketone (MEK). practical (2-butanone). 7. Reagents 6. Wait 55 min and then reweigh clod. allow longer drying time. Stir plastic lacquer for 15 min at 25°C. mix solvent with a wooden stick.8-L (1-gal) metal paint can with 2700 ±200 mL of solvent. The SSL uses Liqui-Nox. Three clods per horizon are recommended. 6. Loop fine copper wire around clod. The SSL constructs a tension table by placing porous firebricks. Wait 7 min and then dip clod in 1:7 plastic lacquer. 6. The SSL constructs a tin enclosure over hot plate with a chimney and duct to transfer vapor to water stream.6 Plastic lacquer. Fill a 3. Cut the copper wire and loop around the clod. It is important that these clods be as representative of the bulk sample volume as possible. in a tub of water.2 Water. Use 1:7 plastic lacquer for the last two laboratory coats. high-speed stirrer while slowly adding resin. Add 540 or 305 g of resin to make 1:4 or 1:7 plastic lacquer. available from Dow Chemical Company. 7.1 Collect field-occurring clods. covered with reinforced paper towels. stir solvent with a non-sparking. If the value of Dbf is required. 5. If clod has adsorbed >3% plastic by clod weight or smells excessively of solvent. moisten surface with a fine mist of water.4 Prepare a round stock tag with sample identification number. Fill to the bottom of handle rivet. ≈ 100 to 200 cm3 in volume (fist-sized). Store plastic lacquer in covered plastic or steel containers. If roots are present.5 Dip clod in 1:4 plastic lacquer. Wait 12 min and then dip clod in 1:7 plastic lacquer. Laboratory 7. Suspend clod from clothesline to dry (See Fig.3 Pack clods in rigid containers to protect them during transport. leaving a tail to which round stock tag is attached. Record weight (TAG) of tag and wire. Tie clod with fine copper wire or place clod in a hairnet.23 Liquid vapor trap. 1. procedure 3B1a). No procedure for sampling clods is applicable to all soils. 6. store clods in waterproof plastic bags as soon as coating dries because coating is permeable to water vapor.24 Reinforced paper towels or cheesecloth 5. 7. cut a flat surface on the clod. The 1:7 plastic lacquer is used to conserve the resin and to reduce cost. then reweigh clod and record weight (CC2). 7. From this piece. 6.4 Liquid detergent. In the laboratory. For the initial field and laboratory coatings. procedure 3B1a). Record weight of clod (CC1). Dry clod for 30 min or until odor of solvent dissipates. Procedure Field 7.5 Dow Saran F-310 Resin. If the clod is dry.25 Tension table. trim roots with shears. Remove a piece of soil larger than clod from the face of sampling pit. 2. Adjust field sampling techniques to meet field conditions at time of sampling. prepare a clod by gently cutting or breaking protruded peaks and compacted material from clod. 6. In the field. 6. Quickly dip entire clod into plastic lacquer (See Fig. respectively.3 Alcohol. use the 1:4 plastic lacquer. from the face of the excavation.5. 91 .

clod is at equilibrium. After 55 min. allow longer drying time. do not correct clod mass and volume measurement for rock fragments. If clod has adsorbed >3% plastic by weight or smells excessively of solvent.9 Place clod in a pressure plate extractor. 7. Close container and secure lid. If rock fragments are porous and have a density similar to soil sample. Add a few mL of alcohol. allow longer drying time. 7. When water ceases to discharge from outflow tube. Dry and record weight (RF) of rock fragments that are retained on the sieve.17 If clod contains >5% rock fragments by weight. 7. Submerge only the surface of clod in the water. 7. and add hot water.hole sieve. Remove clod and record weight (WSC). Heat clod on hot plate in excess of 200°C for 3 to 4 h. equilibrate clod on tension table and repeat desorption process. 7. maintained at 5-cm tension. If WMC > WSC. Correct for 92 . 7. 7. reweigh clod and record weight (CC4). Suspend clod below the balance. To provide good contact between clod and ceramic plate. then reweigh clod.7.10 Dip clod in the 1:4 plastic lacquer. Wait 12 min and dip clod in 1:7 plastic lacquer. Wait 12 min and then dip clod in 1:7 plastic lacquer. Place surface of cut clod on paper towel.8.18 Wet sieve the cool soil through a 2-mm. Use in-house vacuum and apply suction until clod has equilibrated at saturation. 7. or by weight comparison.14 Dip clod in the 1:4 plastic lacquer.7. 7. cover ceramic plate with a 5-mm layer of silt loam soil and saturate with water. Apply gauged air pressure of 33-kPa.15 After coating. When clod has reached equilibrium.12 Remove layer of plastic from flat surface of clod. place clod in a desiccator on a water-covered plate with a 0-cm tension. After 55 min. then reweigh clod. Cover hot plate with a liquid vapor trap. touching.16 Dry clod in an oven at 110°C until weight is constant. Compare WMC to WSC. Wait 7 min and then dip clod in 1:7 plastic lacquer.13 Repeat steps 7. remove clod and record weight (WSC). 7. The plastic coating disintegrates at temperatures above 200°C. Wait 7 min and then dip clod in 1:7 plastic lacquer. square.8 If cut clod does not adsorb water. remove clod and record weight (WAR). submerge in water. After equilibrium is obtained. Extraction usually takes 3 to 4 wk.9.7 Place cut clod surface on a tension table. Weigh oven-dry clod in air (WODC) and in water (WODCW) and record weights. Place a sheet of reinforced paper towel or cheesecloth over the silt loam soil. After heating. Remove clod from hot plate. If rock fragments are porous and have a density similar to soil sample. If clod has adsorbed >3% plastic by weight or smells excessively of solvent. Wait 12 min and then dip clod in 1:7 plastic lacquer. and 7. record weight of clod suspended in air (CC4) and in water (WARW). and record weight (WMCW). Place clod in a beaker and place on hot plate. lightly coat with liquid detergent. Wait 12 min and dip clod in 1:7 plastic lacquer.11 The clod should be waterproof and ready for volume measurement by water displacement. clod should appear black and charred. Remove clod and record weight (WMC). Use a fume hood. Determine rock fragment density by weighing them in air to obtain their mass and in water to obtain their volume. reweigh clod and record weight (CC3). 7. remove them from clod. do not correct clod mass and volume measurement for rock fragments. Dry clod at 40 to 50°C for 2 to 3 days or until weight is constant. Air-dry clod at room temperature (~ 20 to 25°C) for 4 to 6 days. Periodically check clod to determine if it has reached equilibrium by inserting metal probe. 7.

3 g cm-3.RF .5 x [(CC2 -CC1)/3] where: FCE = Estimate of field-applied plastic coat. The coating loses 10 to 20% of its air-dry weight when dried in oven at 110°C.85. The coating has an air-dry density of ≈ 1. Calculations 8.(MPC1/1.2 MPC1 = {[(CC2 .19 Correct bulk density for weight and volume of plastic coating.3)} where: Db33 = Bulk density in g cm-3 of <2-mm fabric at 33-kPa tension WODC = Weight of oven-dry coated clod RF = Weight of rock fragments ODPC = MPC1 x 0. weight of oven-dry plastic coat TAG = Weight of tag and wire CC3 = Weight of equilibrated clod after four additional plastic coats WD = Water density PD = Density of rock fragments WMCW = Weight in water of coated clod equilibrated at 33-kPa tension 8. 7.WMCW)/WD] . 8.3)} where: = Bulk density in g cm-3 <2-mm fabric at 33-kPa tension after rewetting Dbr CC4 = Weight of clod after twelve plastic coats WARW = Weight in water of coated clod equilibrated at 33-kPa tension after rewet 8.WARW)/WD] .1 Db33 = [WODC .4 Dbr= [WODC – RF – ODPC .(RF/PD) .3)} where: Dbod = Bulk density in g cm-3 of <2-mm fabric at oven dryness 93 .(MPC2/1.TAG]/ {[(CC4 .rock fragments if these fragments can withstand breakdown when dry soil is placed abruptly in water or calgon.5 MPC2 = {[(CC2 .CC1) + FCE] x RV} + (CC3-WMC) where: MPC1 = Weight of plastic coat before air-drying and rewet CC2 = Weight of clod after three laboratory plastic coats CC1 = Weight of clod before three laboratory plastic coats RV = Percent estimate of remaining clod volume after cutting to obtain flat surface (≈ 80%) WMC = Weight of coated clod equilibrated at 33-kPa tension 8.(RF/PD) .ODPC – TAG]/{[(CC3 .CC1) + FCE] x RV2} + (CC3-WMC) + (CC4-WAR) where: MPC2 = Weight of plastic coat after rewet and before oven drying WAR = Weight of clod after rewet equilibration RV2 = Percent estimate of remaining clod volume after remaining layer of plastic (≈ 0.6 Dbod = [WODC– RF– ODPC-TAG]/{[(WODC-WODCW) /WD] .(RF/PD) .3 FCE = 1.95) 8. 8.(MPC2/1.

) Methods of soil analysis. 2002. Grossman and Reinsch. References Blake. 2nd ed. Bulk density and linear extensibility.7 W1/3 = {[(CC3 . G. Physical and mineralogical methods.ODPC – TAG]} x 100 where: Wr = Percent water weight retained at 33-kPa tension after rewet 9. 383-382. 94 . ASA and SSSA. U.R.RF . Part 4.G. The clod is desorbed to 33kPa. 201-228.. final rule. Klute (ed. 2452-2453. Physical methods. D. Agron. and K. DC. B. 54.ODPC)]/ [WODC . 11. 2. Grossman. Brasher. Am. 1986. Volassis. Use of saran resin to coat natural soil clods for bulk density and water retention measurements.ODPC – TAG)} x 100 where: W33 = Percent water weight retained at 33-kPa tension 8. 9. Madison.C. and to identify compacted horizons. Book Series No. Office. 1989.P. Soil Sci.. Plastic lacquer is applied in the laboratory to form an impermeable coat on the clod. Soil Sci.). Print. 5. Air contaminants. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Federal Register. 1966. After equilibration.. Application Bulk density is used to convert data from weight to volume basis.01g cm-3. 101:108. p. Govt.B. V. Washington. to determine the coefficient of linear extensibility. 29 CFR Part 1910.WODCW = Weight in water of oven-dry coated clod 8. Bulk density.RF . to estimate saturated hydraulic conductivity. Bulk Density (3B) Reconstituted (3B2) 33 kPa Desorption (Db33) (3B2a) Oven-Dry (Dbod) (3B2b) 1. In A. Occupational Safety and Health Administration. Summary of Method In this procedure (3B2c) A <2-mm sample is formed into a clod by wetting and desiccation cycles that simulate reconsolidating by water in a field setting.R. Methods of soil analysis. WI. No.MPC1) – (WODC . After the clod is oven dried at 110°C. ASA and SSSA.E.H. Madison.T. and T. Topp (eds. Vol. Franzmeier. p. Monogr. In J. and S. 12. 1986. The reconstituted bulk density provides a single.ODPC)]/(WODC . Reinsch. Hartge. 10.S.8 Wr ={[(CC4 . WI. 2002). 1995).H. Report Bulk density is reported to the nearest 0. 1966. reproducible value for horizons that are subject to tillage or other mechanical disturbances followed by an extreme water-state cycle (Reinsch and Grossman. p.MPC2) – (WODC . R. Dane and G. Some models and programs require one bulk density to represent a given horizon. the clod is weighed in air to measure the mass and in water to measure the volume.. Blake and Hartge. Davidson. Part 1. its mass and volume are determined again (Brasher et al.

01-g sensitivity 5.2 Water. Interferences Some samples disintegrate when they are removed from the cells. 1825 Connecticut Ave.13 Paper discs cut from water insoluble.4 Dow Saran F-310 Resin. to a 100-kPa ceramic plate with waterproof glue and caulk 5. available from Dow Chemical Company. ±0. and the short-term exposure limit (STEL) is 300 ppm (Occupational Safety and Health Administration. use a fume hood.3 Alcohol. 6.6 Wire.17 Vacuum.20 Reinforced paper towels or cheesecloth 5. The 8-h time-weighted average (TWA) exposure limit is 200 ppm. Wash hands immediately after handling MEK.5-cm openings and 5.5 Anti-sorting device. SSL uses 28-awg-coated copper wire 5. high-speed stirrer while slowly 95 .15 Silt soil 5. We construct a tension table by placing porous firebricks. permeable paper 5.4-cm diameter and 6 to 7 cm high.. Safety Methyl ethyl ketone (MEK) is extremely flammable. We construct a wire screen with 0. and a lab coat.2 cm diameter with a perpendicular wire attached to the center to reduce natural sorting caused by placing the sample in the cell 5. covered with reinforced paper towels.2 Pressure plate extractor with porous ceramic plate 5. 1989). In closed buildings. Washington. proper gloves.5 Plastic lacquer.1 Electronic balance.21 Tension table. Use with adequate ventilation.11 Oven. DC.1 Methyl Ethyl Ketone. Reagents 6. NW.10 Plexiglas water tank mounted on a fulcrum and lever to elevate tank 5. Use safety glasses. 4. Keep in tightly closed containers.18 Metal probe 5.9 Hook assembly for weighing below balance 5. 110°C 5. The 1:7 plastic lacquer is used to conserve the resin and reduce cost.4 Clod forming cylinder. Avoid physical contact. Stir the solvent with a non-sparking.8 bar) 5.19 Spray bottle 5. The MEK vapor is classified as a sensory irritant.3 Air pressure. Equipment 5. 33-kPa 5. 6. 1-inch diameter paper tag with metal rim 5. respectively. 5. 6. We fill a metal gallon paint can with 2700 ± 200 ml of solvent (fill to the bottom of the handle rivet) and add 540 g or 305 g of resin to make 1:4 or 1:7 plastic lacquer. We construct the cell by attaching a brass ring or schedule 20 or 40 PVC pipe. 5.12 Plastic tub at least 10 cm deep 5.16 Desiccator with ceramic plate 5. Additional information on the safe handling of MEK is available in Chemical Safety Data Sheet SD-83. Inc. A type B fire extinguisher should be in close proximity in the laboratory. practical (2-butanone). No open flames or nearby operation of electrical equipment are permitted while using MEK. Manufacturing Chemists’ Association. Prepared the plastic lacquer with resin to solvent ratios of 1:4 and 1:7 on a weight basis.7 Hairnets 5. Use the 1:4 plastic lacquer for the first field and lab coats and the 1:7 plastic lacquer for the last two coats.3.14 Tile cut-off saw with diamond blade 5. in a tub of water 6. 80 kPa (0. 6.8 Stock tags.

Check the clod periodically by inserting a metal probe. remove the clod and record the weight (WSC). Compare WMC to WSC. reweigh the clod. Close the container and secure the lid. dip the clod in the 1:4 plastic lacquer. cover the ceramic plate with a 5-mm layer of silt and saturate with water. Cut the copper wire to loop around the clod. The reconstituted clod is used to measure bulk density and water retention. If WMC is greater than or equal to WSC.6 Cut a flat surface on the clod with a diamond saw. Place a paper disc in the bottom of the cell. After 7 min. allow longer drying time. 7. dip the clod in the 1:7 plastic lacquer. Stir the plastic lacquer for 15 min at 25°C.3 Remove the cell from the tub and allow to dry at room temperature.1 Drape a hairnet in the cell. Remove the clod and record the weight (WSC). then reweigh the clod and record the weight (CC2). place the cell into a tub and add water to a level higher than the surface of the soil in the cell but below the top lip of the cell. When the clod has reached equilibrium. Add a few ml of alcohol. After 55 min.7 If the clod does not adsorb water. After 55 min. After 12 min. dip the clod in the 1:7 plastic lacquer. Procedure Reconstituted Clod Construction 7. 7.4 Prepare a round stock tag with sample identification number. After 7 min. dip the clod in the 1:7 plastic lacquer. dip the clod in the 1:7 plastic lacquer.5 Mist the clod with water to create a film of water on the surface of the clod. the clod is at equilibrium. Allow the sample to equilibrate. When water stops discharging from the outflow tube (usually after 3 or 4 wk in the extractor). 7.2 Place the cell on a tension table with the height 5-cm below the top of the table. or weight comparison to determine if it has reached equilibrium. In the field. equilibrate the clod on the tension table and repeat the desorption process. Lift the anti-sorting screen from the cell. Place the cut surface of the clod on the paper towel. reweigh the clod and record the weight (CC3). Add <2-mm. Remove the clod and record the weight (WMC). 7. 7.8 Place the clod in a pressure plate extractor. dip the clod in the 1:7 plastic lacquer. Record the weight of the clod (CC1). This allows the soil to become inundated from beneath. If the clod has 96 . Store the plastic lacquer in covered plastic or steel containers. After 12 min. Apply suction using in-house vacuum for 24 hours. prepared sample to within a few mm of the top of the cell. 7. To provide good contact between the clod and ceramic plate. After 12 min. 7. Bulk Density Measurement 7.adding the resin. Record the weight of the tag and wire (TAG). place the clod in a desiccator that has water covering the desiccator plate. 7. If the clod has adsorbed more than 3 percent plastic by clod weight or smells excessively of solvent. Dip the clod in the 1:4 plastic lacquer. After equilibration. mix with a wooden stick. touching. Loop fine copper wire around the clod leaving a tail to which the round stock tag is attached. Place the cut clod surface on a tension table maintained at 5-cm tension. After drying remove the clod by lifting on the hairnet or inverting the cell and lightly tamping the base of the cell. Acetone may be substituted for MEK. Place the antisorting screen into the cell.9 Dip the clod in the 1:4 plastic lacquer. Place a sheet of reinforced paper towel or cheesecloth over the silt . Apply gauged air pressure of 33kPa. After 7 min.

01 g cm-3.(MPC/1.2 MPC1 = {[(CC2-CC1)] x RV} + (CC3-WMC) where: MPC1 CC2 CC1 RV WMC = Weight of plastic coat before oven-drying = Weight of clod after four laboratory plastic coats = Weight of clod before four laboratory plastic coats = Percent estimate of remaining clod volume after cutting to obtain flat surface (≈95%) = Weight of coated clod equilibrated at 33-kPa tension 8.adsorbed more than 3 percent plastic by clod weight or smells excessively of solvent.(MPC1/1. The coating has an air-dry density of about 1. Suspend the clod below the balance. 9.1 Db33 = [WODC .3)} where: Db33 = Bulk density in grams per cubic centimeter of < 2-mm fabric at 33-kPa tension WODC = Weight of oven dry coated clod ODPC = MPC x 0. weight of oven dry plastic coat TAG = Weight of tag and wire CC3 = Weight of equilibrated clod after four additional plastic coats WMCW = Weight of coated clod equilibrated at 33-kPa tension in water MPC1 = Weight of plastic coat before oven-drying WD = Water density 8. and record the weight (WMCW). The coating loses 10 to 20 percent of its airdry weight on oven drying at 110°C. 7. 97 . allow longer drying time.ODPC – TAG]/{[(CC2 .4 W33 = {[(CC3 – MPC1) .12 It is necessary to correct bulk density for weight and volume of the plastic coating.(RF/PD) .WMCW)/WD] . submerge in water. then reweigh the clod. Report Bulk density is reported to the nearest 0.ODPC – TAG)]} x 100 where: W33 = Weight percentage of water retained at 33-kPa tension 9.TAG]/{[(WODC – WODCW)/WD] . 7. Weigh the oven dry clod in air (WODC) and in water (WODCW) and record the weights.(WODC . 7. 8. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.ODPC)]/[WODC .85.3)} where: Dbod = Bulk density in grams per cubic centimeter of < 2-mm fabric at oven-dryness WODCW = Weight of oven dry coated clod in water 8.RF .10 The clod should now be waterproof and ready for the volume measurement by water displacement.3 Dbod = [WODC – ODPC . Calculations 8.3 g/cm3.11 Dry the clod in an oven at 110°C overnight.

Dane and G. 2002). Summary of Method By this procedure (3B3a). 2002). B. 1995. 1989. Make three 16-mm diameter holes that are 10 mm from the outer edge of ring. Brasher. Soil is quantitatively excavated in a cylindrical form to the required depth. The difference between the initial volume and that after excavation is the sample volume. p. Excavation procedures (e. Physical methods. the surficial zone is usually not altered (Grossman and Reinsch. 9. WI. Occupational Safety and Health Administration. Washington. 34: 95-104. final rule. 1986. 98 . Bulk density and linear extensibility. No. Equipment 5. 2002.11. Vol. Soil Sci. and for which the clod method is unsuitable (Grossman and Reinsch. On the other side. 2002). 5. 25 x 50 mm. Monogr.T. to estimate saturated hydraulic conductivity. R.e. Plexiglass pieces as guides. Grossman. 3. Physical and mineralogical methods.H. ring. and T. D. 363-382. WI.) Methods of soil analysis. Safety Follow standard field and laboratory safety precautions. Print. Federal Register. Madison. 29 CFR Part 1910.1 Fabricated Plexiglass rings. DC. Madison. Volassis. p. and K. 130-mm inside diameter. Franzmeier.R.P. Bulk Density (3B) Compliant Cavity (3B3) Field-State (3B3a) 1. ASA and SSSA. position the single piece in line with the longer leg of the "L" so that an adjacent.G. Topp (eds. 201-228.. Bulk density.H. the cavity volume on the zone surface is lined with thin plastic and water is added to a datum level. and R. Air contaminants. or thin (<5 cm thick). Klute (ed.S. Federal Register. 9-mm thick.G. Grossman.E. and frame) have applicability to layers that can be described as cohesionless. Position holes equidistant apart. ASA and SSSA. In A. Use of saran resin to coat natural soil clods for bulk density and water retention measurements. Use three. 4. and to identify compacted horizons. Soil and Tillage Res. Davidson.C. Agron. and S. Application Bulk density is used to convert data from a weight to a volume basis. This method has the important advantage that it is not necessary to flatten the ground surface on steep slopes or remove irregularities. 5. In J. Part 4. 12. The compliant cavity method was designed for fragile cultivated near-surface layers and O horizons of forestland soils. Interferences Bulk density by compliant cavity can be made on soils with rock fragments but is more complex (Grossman and Reinsch. A correction is made for the weight and volume of rock fragments. 54. 2nd ed. Govt. compliant cavity. V.) Methods of soil analysis. and >200-mm outside diameter. 101:108. A method to predict bulk density of tilled Ap horizons. 2452-2453. Book Series No.g. Part 1. G.B.. 2. i. Hartge. Office.. Attach two pieces on one side to form an "L". high in rock fragments > 5mm. 1966..R. U. Am. The excavated soil is dried in an oven and then weighed. Reinsch.. Allow a 15-mm gap to permit removal of soil material. Soil Sci. Reinsch. References Blake.B. T. parallel line forms a diameter. p.

The weight of macroscopic vegetal material (g cm-3) also may be reported. Procedure 7.5 The excavated soil is dried in oven and weighed. If necessary. 10. sharply bend the bolt upward to form a U-shape. Measure the volume of water. Sharpen the rods. Drill a hole 100 mm from one end of the crossbar and 7 mm from the edge and through which a No.3 5. square-hole. Fill the excavation cavity to tip of hook gauge with water from graduated cylinder. small Scissors. Measure the volume of water to tip of hook gauge. The foam rings have the same inside diameter as the Plexiglass rings.16 5. make a correction for weight and volume of >2-mm material (Vg) in sample and compute bulk density. Make hook gauge from No. use clothespins for corners of plastic film. 7. Syringe. 6. Drill a hole in the center of the crossbar. Hold the machine bolt by the tightened nuts and heat the bolt.11 5.to 400-mm long. Reagents 6.12 5. small Kitchen knife. Sharpen the machine bolt to a sharp point.6 5. 2 mm 6. 60 mL Plastic film. Place nuts above and below the crossbar.17 5. 100-mm long machine bolts and from hexagonal nuts.9 5. Hard rubber or plastic mallet Sieve. Insert the machine bolt in the hole. with ties Sharpie pen Graduate cylinders. 7.7 5. 99 .4 Excavate soil quantitatively and in a cylindrical form to the required depth. small. After softening. Fill cavity to tip of hook gauge with a known quantity of water from graduate cylinder. 10 mesh.8 5. 7.4 5. Mount hook gauge on crossbar. 110°C-capability. threaded rods to mount and position the compliant cavity.2 5.Vd) is the volume of excavated soil (Ve). The difference between the two water volumes (Vf . to cut fine roots Hack saw blade to cut large roots Weights for plastic film Clothespins. 380-mm wide or wider.3 Remove plastic film and water. plastic. Mount the assembly on the soil surface by securely driving threaded rods into the ground through holes in ring and by tightening ring with wing nuts. 1/2 mil. Fabricate a 240-mm crossbar from 5 x 18 mm metal stock to which legs (25-mm high and 180 x 180 mm in cross section) are welded. If wind. 250 to 2000 mL Level. 6 machine bolt is placed.15 5.1 Place a ring of plastic foam on ground and cover with rigid ring (130-mm inside diameter).1 Water 7. The two nuts adjust the hook length below the crossbar and provide rigidity. 460-mm wide for larger ring. 250. Obtain the machine bolts from toggle bolt assemblies.2 Line cavity with 1/2-mL plastic. round-headed.13 5.10 5.5 5. This volume (Vd) is the measurement of cavity volume prior to excavation (dead space).18 Make 50-mm thick foam rings from flexible polyurethane with an "Initial Load Displacement" of 15 to 18 kg. Place two regular nuts at the end of threaded rod to increase the area of surface struck.to 13-mm diameter.5. This volume (Vf) is the measurement of excavated soil and dead space. Use wing nuts and three. Plastic bags.14 5. 7.

A limit of 2 cm on the minimum thickness of the sample should be considered. 10. ring. p.3 Db = Wf/Ve where: Db = Bulk density (g cc-1) Wf = Oven-dry weight of <2-mm soil (g) Ve = Excavation volume of <2-mm material (cc) 9. 5.G.H. Bulk density and linear extensibility. and to identify compacted horizons. high in rock fragments > 5mm. compliant cavity. In J. This method is good for O horizons in the woods where local variability is large.fraction) (cc).Wc where: Wf = Oven-dry weight of <2-mm soil (g) Wo = Oven-dry weight of excavated soil (g) Wc = Oven-dry weight of rock fragments (g) 8. 2.. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Soil Sci. WI. and rapid method.g. Report Bulk density is reported to the nearest 0. Dane and G. and T. Calculate Vg by dividing the weight of >2-mm fraction by particle density of the >2-mm fraction..) Methods of soil analysis.01 g cm-3. and frame) have applicability to layers that can be described as coheshionless. Summary of Method A 20-cm ring is inserted into the ground. Physical methods. Bulk Density (3B) Ring Excavation (3B4) Field-State (3B4a) 1. simple. Excavation procedures (e. R. The distance to the ground surface is measured at eight points equally 100 . Madison.C. Book Series No. 8. Reinsch.2 Wf = Wo .65 g cc-1. The ring excavation is a robust. to estimate saturated hydraulic conductivity. A piece of shelf standard is placed across the ring near to a diameter.Vg where: Ve = Excavation volume of <2-mm fraction (cc) Vf = Water volume measurement of excavated soil and dead space (cc) Vd = Water volume measurement of dead space (cc) Vg = Gravel volume (>2mm. It is not necessary to excavate from the whole area within the ring. Default value of 2. 11. The diameter can range down to 15 cm and upwards to 30 cm or more. or thin (<5 cm thick).B. Topp (eds. Application Bulk density is used to convert data from a weight to a volume basis.8. Part 4.1 Ve = Vf . 201-228. ASA and SSSA. 2002. and for which the clod method is unsuitable (Grossman and Reinsch. Am. References Grossman. Calculations 8. 2002).Vd .

1 Metallic cylinder. 30-cm long with 0. Procedure 7. 1.3 Rotate the piece of shelf standard 90° and make eight more measurements.6 The excavated soil is dried in oven and weighed. 10 x 10 x 30 cm 5. the weight and volume of >2-mm material in sample are corrected and bulk density computed. 7. Repeat the distance measurements. The piece of shelf is rotated 90° and eight more measurements are made.5-cm wide.3 Piece of retractable ruler. The soil is excavated to the desired depth. 8. 4. The weight of macroscopic vegetal material (g cm-3) also may be reported. 20-cm diameter. 7.6 Depth-measurement tool (Grossman and Reinsch. If rock fragments are present. Equipment 5. 1-cm high.1-mm divisions 5. Reagents None.4 Piece of wood.4 Excavate the soil to the desired depth. 7. 3.to 20-cm high. and 25-cm long 5. Average the 16 measurements. 7. Calculations 8. Interferences Rock fragments may make insertion of ring into the ground impossible.spaced along the diameter using the depth-measurement tool to measure the distance.2 Place a piece of shelf standard across the ring near to or along a diameter.1 Insert a 20-cm diameter ring below the depth of excavation. The excavated soil is oven-dried and weighed. 10. 5. and the distance measurements repeated. This change in distance is then multiplied by the inside cross-sectional area of the ring to obtain the volume of soil. 7.1 Wf = Wo – We where: Wf = Oven-dry weight of <2-mm soil (g) Wo = Oven-dry weight of excavated soil (g) Wc = Oven-dry weight of rock fragments (g) 101 . Multiply the change in distance by the inside cross-sectional area of the ring to obtain the volume of the soil (Ve). If necessary.5 Calculate the change in distance on removal of the soil. make a correction for weight and volume of >2-mm material in sample and compute bulk density. 7. Safety Follow standard field and laboratory safety precautions. and about 1-mm depth 5.2 Shelf standard (slotted rod). Bulk density of soil is reported in g cm-3 by procedure 3B4a. The 16 measurements are then averaged. 2002) 6. Measure the distance to the ground surface at eight points equally spaced along the diameter using the depth-measurement tool to measure the distance.5 Hand digging equipment 5. The change in distance is calculated on the removal of the soil.

References Grossman. 2002. Topp (eds. Madison. Interferences None. Reinsch. Frame is made from 8 pieces of wood: 2 pieces. In J.H.C. compliant cavity. Bulk Density (3B) Frame Excavation (3B5) Field-State (3B5a) 1.g. Summary of Method The assembled frame is placed on the ground surface.G. WI. and to identify compacted horizons. Soil Sci. The plate is then removed and soil is excavated and retained. Equipment 5. The rock fragments up to 20 mm are included in the sample. Am. Safety Follow standard field and laboratory safety precautions. Book Series No. and T. ASA and SSSA. Report Bulk density is reported to the nearest 0. 11. and frame) have applicability to layers that can be described as coheshionless. 201-228.01 g cm-3.) Methods of soil analysis. The frame is then secured onto the soil surface by screwing down wing nuts and plastic placed over the frame and secured. Bulk density of soil is reported in g cm-3 by procedure 3B5a. Excavated soil is oven-dried and weighed..2 Square Plexiglass. This method is good for O horizons in the woods where local variability is large and commonly rock fragments are present.6 cm thick. 2 x 4 x 46 cm. to estimate saturated hydraulic conductivity. 2002).. with 5 parallel equally spaced slots. 9. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.1 m2 inside area. ring.1 Lumber for square wooden frame with 0. and measurements of the distance to the ground surface are made at about 40 regularly spaced intervals. 1.8.6-cm diameter with wing nuts 102 .B.1 m2 is sufficient to encompass considerable local variability. The slots are traversed. 35 cm on edge x 0. Dane and G. The size of the 0. The depth-measurement tool is placed on top of a slot to measure the distance to the soil surface.5 cm across x 28 cm long 5. p. 4. 5.3 Four threaded rods. Part 4. 2. Bulk density and linear extensibility. 5. 2 x 4 x 53 cm. and for which the clod method is unsuitable (Grossman and Reinsch. Application Bulk density is used to convert data from a weight to a volume basis. Excavation procedures (e. The four threaded rods are pushed through the holes in the corners of the frame deep enough to hold. Measurements of the distance to the ground surface are repeated. R.2 Db = Wf/Ve Db = Bulk density (g cm-3) Wf = Oven-dry weight of <2-mm soil (g) Ve = Excavation volume of <2-mm material (cm-3) 9. 2 pieces. high in rock fragments > 5mm. 4 x 5 x 9 cm 5. and 4 blocks. The volume of soil is determined by taking the difference in height and multiplying by 1000 cm2. Physical methods. or thin (<5 cm thick).. 50 cm long x 0. 3.

Report Bulk density is reported to the nearest 0. Determine the difference in height and multiply by 1000 cm2 to obtain the volume of soil excavated. 7.5. p.6 Excavate and retain the soil.4 Depth-measurement tool (Grossman and Reinsch. 7.2 Db = Wf/Ve Db = Bulk density (g cm-3) Wf = Oven-dry weight of <2-mm soil (g) Ve = Excavation volume of <2-mm material (cm-3) 9.1 Assemble the square wooden frame by attaching the 4 x 5 x 9 x cm blocks to the 9 cm of each end of both 53-cm long pieces. Usually rock fragments up to 20 mm are included in the sample. Remove the plate. 103 .0 to 1.2 Place the frame on the ground surface. The walls of the cavity should be vertical and coincident with the edge of the frame. If necessary.8 The excavated soil is dried in oven and weighed. The four pieces are joined by the vertical half-lap joints to form a square frame. Secure onto the soil surface by screwing down wing nuts. Reagents None. 7. 2002. The weight of macroscopic vegetal material (g cm-3) also may be reported. 7. Procedure 7. Push the four threaded rods through the holes in the corners of the frame sufficiently deeply to hold.5 cm in diameter are drilled in the center of the attached blocks. 7. 7.and 53-cm-long pieces to provide half-lap joints.5 Traverse the slots. 8. 209) 5.3 Place the plastic plate over the frame and secure. making measurements of the distance to the ground surface at about 40 regularly spaced intervals. 7.1 Wf = Wo – We where: Wf = Oven-dry weight of <2-mm soil (g) Wo = Oven-dry weight of excavated soil (g) We = Oven-dry weight of rock fragments (g) 8.4 Place the depth-measurement tool on top of a slot and measure the distance to the soil surface. Calculations 8.5 Hand digging equipment 6. The cuts are 5 cm in for the 46-cmlong pieces. 7.7 Repeat the measurements of the distance to the ground surface. Two-centimeter-wide cuts are made half-way across each of the 46. Holes 1. make a correction for weight and volume of >2-mm material in sample and bulk density computed.01 g cm-3.

Physical methods.B. Reinsch.. 201-228. make measurements between the cracks and determine the aerial percentage of total cracks or of cracks in specimen. 2. to estimate saturated hydraulic conductivity. The moist sample weight is recorded. p. ±0. 6. References Grossman.) Methods of soil analysis. Soil Sci. 10 (2 mm-openings) 5.G. Am. No. Sources described in Grossman and Reinsch (2002). Part 4.C. compaction of the sample is a common problem.5 Coring equipment. Dane and G. Field bulk density (Dbf ) offers the opportunity to obtain relatively cheaply bulk density information without the expense incurred to obtain water retention. Procedure 3B6a determines the bulk density value of a moist soil core of known volume. with lids 5. Dry or hard soils often shatter when hammering the cylinder into the soil. In J. Procedure 7. The cylinder is removed extracting a sample of known volume. 11. 5. tared. to determine the coefficient of linear extensibility. If compression is excessive. The sample is then dried in a oven and weighed. Application Bulk density is used to convert data from a weight to a volume basis. 3. WI.3 Oven 110°C 5. air-tight. If soil cracks are present. Interferences During coring process. Topp (eds. Compression can be observed by comparing the soil elevation inside the cylinder with the original soil surface outside the cylinder. if possible. Dbf is particularly useful if the soil layers are at or above field capacity and/or the soils have low extensibility and do not exhibit desiccation cracks even if below field capacity. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Book Series No. select the sampling area so that crack space is representative of sample. R. ASA and SSSA.01-g sensitivity 5. Reagents None 7. If this is not possible. Bulk Density (3B) Soil Cores (3B6) Field-State (3B6a) 1. Bulk density and linear extensibility. 5.H. Summary of Method A metal cylinder is pressed or driven into the soil.2 Electronic balance. Pressing the cylinder into the soil reduces the risk of shattering the sample. soil core may not be a valid sample for analysis. 2002. Equipment 5. Safety No known hazard exists with this procedure. and to identify compacted horizons.4 Sieve. Rock fragments in the soil interfere with core collection.10. 104 .1 Record the empty core weights (CW).1 Containers. and T. 4. Madison.

Madison.01 g cm-3. If soil is too loose to remain in the liner.7. Dry and weigh the rock fragments that are retained on sieve. Topp (eds. Calculations Db = (ODW . 7. Physical methods. 10. whether the water is absorbing into or desorbing from the soil. Record weight of rock fragments (RF).C. Use caution to prevent compaction.4 Dry core in an oven at 110°C until weight is constant. 201-228. i. trim protruding soil flush with ends of cylinder.. 7. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.6 If sample contains rock fragments.G. organic matter. and T. For fibrous organic materials. The data collected in these procedures are from water desorption. 11. WI. 105 . 1993). Bulk density and linear extensibility. Dane and G.H.. 5. Record oven-dry weight (ODW). Reinsch. either horizontal or vertical. clay mineralogy.e. Report Bulk density is reported as g cc-1 to the nearest 0. at the required depth in sampling pit. ASA and SSSA.3 Press or drive core sampler into soil. and rooting patterns (Topp et al. Part 4. and place in air-tight container for transport to laboratory. Soil Sci. p. field water state (g cm-3) ODW = Oven-dry weight RF = Weight of rock fragments CW = Empty core weight CV = Core volume PD = Density of rock fragments 9. PHYSICAL AND FABRIC-RELATED ANALYSES (3) Water Retention (3C) Water retention is defined as the soil water content at a given soil water suction. 8. This relationship is dependent on particle-size distribution. Am. By varying the soil suction and recording the changes in soil water content.RF – CW)/[CV . infiltration. Moisture cans can also be pushed directly into a prepared face. wet sieve sample through a 2-mm sieve. plant available water. trim sample to fit snugly into a moisture can. a water retention function or curve is determined. Water retention or desorption curves are useful directly and indirectly as indicators of other soil behavior traits such as drainage.B. 7. R. Remove core from the inner liner. 2002.2 Prepare a flat surface.5 Measure and record cylinder volume (CV). and structure or physical arrangement of the particles as well as hysteresis. Determine density of rock fragments (PD).(RF/PD)] where: Db = Bulk density of < 2-mm fabric at sampled.) Methods of soil analysis. aeration. use core sampler without the inner liner and deposit only the soil sample in air-tight container. Book Series No. In J. 7. References Grossman.

Print. 1954) with either a pressure-plate or pressure-membrane extractor. 10. 1954. Soc.A. 33. 100. G. or 200 kPa (3C1a-e) <2-mm (sieved).S. or 2 bar. clods. 60.) Diagnosis and improvement of saline and alkali soils. In M.. The SSL uses the pressure method (U. Office.) Soil sampling and methods of analysis. respectively (0. air-dried. 3. air-dry soil samples of non-swelling soils. 10.S. Procedures 3C1a-e1 (pressure-plate extraction) are used to determine water retention at 6. or 200 kPa. Can.Two desorption procedures are commonly used to measure water retention. air-dry soil samples. Procedure 3C2a1b is used to measure water retention at 1500 kPa for <2-mm (sieved). Air-Dry Samples (3C1a-e1a) 1. Procedure 3C1c4 (pressure-plate extraction) is used to determine the water retention of a clod equilibrated at 33-kPa. Govt. Carter. loamy sand or coarser soil and for some sandy loams. 2. Washington. 1993. U. and M. the porous ceramic plate becomes clogged and water outflow is restricted. 1000 mL 106 . loamy sand or coarser soil and for some sandy loams. 10. Summary of Method The pressure desorption method (U. for <2-mm (sieved). The plate is cleaned by flushing sequentially with 500 mL of 10% H2O2. 1986). 1/3. With extended use. DC. The sample is equilibrated at the specified pressures. a suction method and a pressure method. The plate is covered with water to wet the samples by capillarity. Richards (ed. air-dry soil samples of non-swelling soils. 33. Procedures 3C1a-e1a (pressure-plate extraction) are used to determine water retention at 6. respectively) for sieved.1. and saturated conductivity of a soil sample at specific water contents. Procedures 3C1a-d2 and 3C1a-d3 are usually used in conjunction with the bulk density procedure 3B1b. 33. Boca Raton. Check for outflow air to verify that the pressure-plate extractor is functioning properly and does not leak. The pressure is kept constant until equilibrium is obtained (Klute. L. References Topp. Water Retention (3C) Pressure-Plate Extraction (3C1) 6. p. CRC Press. pore-size distribution. <2-mm. respectively. and re-equilibrated. Ball..06. Procedure 3C2a1a (pressure-membrane extraction) is used to determine water retention at 1500 kPa (15 bar) for <2-mm (sieved). The pressure should be monitored for stability. FL.R. Salinity Laboratory Staff. Galganov. Y. B. Salinity Laboratory.C. Interferences A leaking pressure extractor prevents equilibration of samples. Carter (ed. 100. 0. or 200 kPa. Soil Sci. Procedures 3C1a-d2 and 3C1a-d3 (pressure-plate extractions) are used to measure water retention of natural clods or cores that have been equilibrated at 6. 569-579. field moist soil samples.S. or bulk samples. water-holding capacity. The gravimetric water content is determined.R. Application The data collected are used for the water retention function. 100.S. U. air-dry soil is placed in a retainer ring sitting on a porous ceramic plate in a pressure-plate extractor. 1. The data are also used to calculate unsaturated hydraulic conductivity. USDA Handb. A sample of <2-mm (sieved).C. or 100 kPa. 33. Salinity Laboratory Staff. The resulting data are called rewet water-retention data and are usually used in conjunction with the rewet bulk density data in procedure 3B1d to estimate changes in physical properties of a soil as it undergoes wetting and drying cycles. 1954) is used. Equilibration must be done at constant temperature and humidity.T. porosity. Soil water desorption curves. 10. Procedure 3C3 is used to determine field water content at the time of sampling for cores.

and 33 kPa. especially for fine-textured soils that contain significant amounts of swelling clays. regulator. apply ethyl alcohol to the surface of the samples. Safety High pressure plumbing must be maintained in good working order. technical grade 7. Water retention data for soils with expansive clay is overestimated when sieved samples are used in place of natural soil fabric for tensions of 6. 5.2 Place the saturated ceramic plate in a pressure plate extractor. Ensure that the bolts are tightened before applying pressure.1 Saturate the ceramic plate by applying RO water through the adapter and apply enough pressure so that the rubber membrane is bulging a few centimeters. respectively. 7.1 Reverse osmosis (RO) water 6. 6. Include a quality control (QC) sample in each pressure-plate extractor. 1986). 1 N. 107 . Procedure 7. the plate is removed from service. If samples do not moisten. (Young and Dixon. Equipment 5. Use 40mm diameter rings for all other soils. 1966). Aerated 0. in l L of RO water. air-dry soil. and gauge. affecting the water content at a given pressure head (Dane and Hopmans. technical grade. Close the apparatus and let stand overnight. If air bubbles escape from the membrane. 7. Use 50-mm diameter rings for soils that have >12% in organic matter.3 Oven. 10. and 500 mL of reverse osmosis (RO) water.3 Hydrochloric acid (HCl).1 Pressure plate extractor 5. Continue to add water until all samples have moistened by capillarity. ±0. Care should be taken to remove all air. 7. water retention data are usually higher than field-determined water retention data.2 Electronic balance. Distilled or deionized water can possibly promote dispersion of clays in samples and freshly drawn tap water is often supersaturated with air.4 Pressure source. Dilute 83. The solutions are pulled through the plate with a vacuum.01-g sensitivity 5.2 Hydrogen peroxide (H2O2). 10% solution.3 mL of concentrated HCl in 1 L of RO water. 5. 5.4 Ethyl alcohol. 110°C 5. The membrane is inflated and then submerged in water. Reagents 6. Do not drop the heavy lid.005 M CaSO4 has also been recommended (Dane and Hopmans. 2002).4 Add water to cover the ceramic plate but not to cover the rings. because the confining soil pressure is not present in the laboratory (Bruce and Luxmoore.5 Retainer rings. The rubber membrane on the bottom of the plate is checked for leaks. Dilute 333 mL of 30% H2O2. Use 10-mm high and 50-mm diameter rings for organic soils and 10-mm high and 40-mm diameter rings for all other soils. Place retainer rings on the ceramic plate. 95%.6 Metal weighing cans with lids 6. 2002). and the waste is captured in a trap. Ensure that the pressure is zero before removing bolts from the pressure extractor lid. Laboratory-determined.3 Fill retaining ring with 10 to 15 g of <2-mm or fine-grind.of 1 N HCl. 6. 4.

8. Water retention: Laboratory methods..C. Washington.1 percent. Monogr. p.S. W. and saturated conductivity of a soil sample at specific water contents.Ms)/(Ms .J. 33. The data are also used to calculate unsaturated hydraulic conductivity. K. 675720.A.H. U. (ed. cover with lids. References Bruce. USDA Handb. Am. and dry at 110°C overnight. Book Series No. 10. L. Part 1. Physical methods. Monitor the outflow tube for water discharge.H. Topp (eds. Record weights (Ms). WI. Calculations H2O % = 100 x [(Ms+w . water-holding capacity. ASA and SSSA. Water retention and storage: Laboratory. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. A. 11. U. porosity. Procedures 3C1a-d2 are used to determine the water retention of natural clods at 6. pore-size distribution.Mc)] where: H2O % = Percent gravimetric water content Ms+w = Weight of solids + H2O + container Ms = Weight of solids + container Mc = Weight of container 9. 7. Hopmans. 9.7. 101:104-107. Soil Sci. Samples are equilibrated when water ceases to emit from the outflow tube. Govt.) Methods of soil analysis. Overestimation of water content at field capacity from sieved-sample data. respectively. p. and J. ASA and SSSA. Madison. Young. The outflow tube can be submerged under water in a burette to measure when water ceases to emit from the outflow tube. 2002. WI. 5. In J. Madison.S. Madison. Klute.) Diagnosis and improvement of saline and alkali soils. Application The data collected are used for the water retention function. Office.5 Apply the specified pressure. Part 1.. Water retention: field methods. In A.D. Physical and mineralogical methods. In Klute. 10. Luxmoore. 1986. quickly transfer the samples to tared water cans (Mc). Water Retention (3C) Pressure-Plate Extraction (3C1) 6.K. and R. ASA and SSSA. or 100 kPa (3C1a-d) Natural Clods (3C1a-d2) 1. Monogr. p. J.6 When samples have equilibrated.R. or 100 kPa. Report Report water content to the nearest 0. 108 . and record the weights (Ms+w).7 Remove lids. Richards (ed. Klute (ed. Print. Periodically submerge the outflow tube in water to monitor for air bubbles that indicate ceramic plate failure. 7. and J..) Methods of soil analysis. Salinity Laboratory Staff. Dane and G. 635-662. Soil Sci. WI. Dane. 1966. 9. Dixon. R.) Methods of soil analysis. 60. Agron. A. place samples in oven. 663-686. 2nd ed. Part 4. DC. 33. Agron. Physical and mineralogical methods. 10. 1954. 1986.

11 Desiccator with ceramic plate 5. The rubber membrane on the bottom of the plate is checked for leaks in the gasket.14 Sieve.12 Vacuum. 2002). 10-mm height and 40-mm diameter 5. 4. The solutions are pulled through the plate with a vacuum.8 Knife 5.2.3 Pressure source. 1986). The sample is equilibrated at the specified pressures. Do not drop the heavy lid.5 Retainer rings. GSA 5. the porous ceramic plate becomes clogged and water outflow is restricted. ±0. 1000 mL of 1 N HCl. 80 kPa (0. The pressure is kept constant until equilibrium is obtained (Klute. Safety High pressure plumbing must be maintained in good working order. 109 . Equilibration must be done at constant temperature and humidity.8 bar) 5. Salinity Laboratory Staff. The plate is cleaned by flushing sequentially with 500 mL of 10% H2O2.2 Pressure plate extractor with porous ceramic plate (Fig. affecting the water content at a given pressure head (Dane and Hopmans. 2002). Natural clods are placed on a tension table and equilibrated at a 5-cm tension at the base of the sample. 110°C 5.1 and 2) 5. The gravimetric water content is determined. Ensure that the bolts are tightened before applying pressure. the plate is removed from service. especially for fine-textured soils that contain significant amounts of swelling clays.01-g sensitivity 5.005 M CaSO4 has also been recommended (Dane and Hopmans. and the waste is captured in a trap. Check outflow air to verify that each pressure-plate extractor is functioning properly and does not leak. With extended use. water retention data because the confining soil pressure is not present in the laboratory (Bruce and Luxmoore. If air bubbles escape from the membrane. and 500 mL of RO water. The clods are then transferred to a porous ceramic plate which is placed in a pressure-plate extractor. water retention data are usually higher than field-determined. Summary of Method The pressure desorption method (U.16 Fume hood 5.13 Needle probe 5.7 Clothespins 5.9 Tile cut-off saw with diamond blade 5. Interferences A leaking pressure extractor prevents equilibration of samples. 1986).S. Laboratory-determined. 10 (2-mm openings) 5.4 Oven. Equipment 5.15 Hot plate 5. regulator. 5. Aerated 0.10 Silt loam soil 5. 5. The SSL constructs a tin enclosure over hot plate with a chimney and duct to transfer vapor to water stream.17 Reinforced paper towels with nylon fibers. Distilled or deionized water can possibly promote dispersion of clays in samples and freshly drawn tap water is often supersaturated with air.1 Electronic balance. The membrane is inflated and then submerged in water. 1954) is used. The pressure should be monitored for stability. Ensure that the pressure is zero before removing bolts from the pressure-apparatus lid.18 Liquid vapor trap. No.6 Metal weighing cans with lids 5. 3. and gauge.

It is necessary to wet the clod above the initial desorption point. Fill a 3.3 Hydrochloric acid (HCl). Submerge only the surface of clod in the water. For the initial field and laboratory coatings.8 Plastic lacquer.19 Tension table. 7. allow longer drying time. Dilute 83. Add 540 g or 305 g of resin to make 1:4 or 1:7 plastic lacquer. 25.3 Dip the clod in the 1:4 plastic lacquer. in l L of RO water 6. 1 N. Periodically check the clod by inserting a needle probe. Wait 55 min and then reweigh the clod. practical (2-butanone) 6. technical grade. in a tub of water.1 This procedure is usually combined with the bulk density procedure (3B1b). 6. with metal rim 5. high speed stirrer while slowly adding resin.7 Dow Saran F-310 Resin. The SSL uses Liqui-Nox 6. mix solvent with a wooden stick.9 Microbiocide. Wait 7 min and then dip the clod in the 1:7 plastic lacquer. 110 . Reagents 6. Stir plastic lacquer for 30 min at 25°C. available from Dow Chemical Company 6.4 Ethyl alcohol.21 Wire. Record the weight of the clod (CC1). Acetone may be substituted for MEK.8-L (1-gal) metal paint can with 2700 ± 200 mL of solvent. Cut the copper wire and loop around the clod. In the field. When the clod has reached equilibrium.4 Cut a flat surface on the clod with a tile saw. The SSL uses a 28-awg coated copper wire. 7. use the 1:4 plastic lacquer.22 Retainer rings.4-mm (1-in) diameter paper tag.6 Methyl ethyl ketone (MEK).3 mL of concentrated HCl in 1 L of RO water. Use 10-mm high and 50-mm diameter rings for organic soils and 10-mm high and 40-mm diameter rings for all other soils. Procedure 7.2 Hydrogen peroxide (H2O2). If the clod has absorbed >3% in plastic by clod weight or smells excessively of solvent. Dilute 333 mL of 30% H2O2.2 Prepare a round stock tag with sample identification number. stir solvent with a non-sparking. This is accomplished by placing the cut clod surface on a tension table that is maintained at 5-cm tension. Prepare plastic lacquer with resin to solvent ratios of 1:4 and 1:7 on a weight basis. respectively. The 1:7 plastic lacquer is used to conserve the resin and to reduce cost. covered with reinforced paper towels. Use 1:7 plastic lacquer for the last two laboratory coats. Fill to the bottom of handle rivet. Store plastic lacquer in covered plastic or steel containers. 5. then reweigh the clod and record the weight (CC2). 10% solution. or by weight comparison to determine if it has reached equilibrium (clod has wetted up). Use in-house vacuum and apply suction until clod has equilibrated at saturation.5 If cut clod does not absorb water. Add a few mL of alcohol.5 Liquid detergent. technical grade 6. Remove the clod and record the weight (WSC). 7. leaving a tail to which the round stock tag is attached. for tension table. 6. Record the weight of the tag and wire (TAG). 7. 5.1 Reverse osmosis (RO) water 6.20 Stock tags. Wait 12 min and then dip the clod in the 1:7 plastic lacquer. 95%. touching. remove the clod and record the weight (WSC). 6.5. The SSL constructs a tension table by placing porous firebricks. Loop fine copper wire around the clod. place clod in a desiccator on a water-covered plate with a 0-cm tension. Fisher Scientific 7. In the laboratory.

7. continue with procedure 3B1b. If the water content of the QC is within acceptable limits. If WMC > WSC. This determination of the percent rock fragments is based on particle-size data of >2mm fraction.CC1) + FCE] x RV} 111 . then repeat the desorption process at the next higher pressure.MPC) . Boil ≈ 1 h. To provide good contact between the clod and ceramic plate. The plastic coating loosens from soil material upon heating.12 Wet sieve the cool soil through a 2-mm sieve. Place cut clod surface on the paper towel.9 Remove the clod and record the weight (WMC). 7. 8. Periodically submerge the outflow tube in water to monitor for air bubbles that indicate ceramic plate failure. Place several retaining rings in the extractor.1 H2O % =[(WMC . 33. Compare WMC to WSC.8 Apply gauged air pressure of 6. When water stops discharging from the outflow tube. re-equilibrate the clod on the tension table and repeat the desorption process.7. Allow to cool. The outflow tube can be submerged under water in a burette to measure when water ceases to emit from the outflow tube. or 100 kPa. 10. Use a fume hood. rewet the clods and desorb again. Discard plastic coating. 7. do not correct the clod mass for the rock fragments. Submerge the remaining soil material in a beaker of water and place on a hot plate. Remove beaker from the hot plate. coated clod WODC= Weight of oven-dry coated clod RF = Weight of rock fragments ODPC = MPC x 0. begin with the lowest pressure.7 Place the saturated ceramic plate in a pressure plate extractor. remove the rock fragments from the clod. Recheck the QC. Place a sheet of reinforced paper towel over the silt loam soil. Samples are equilibrated when water ceases to emit from the outflow tube. Determine the gravimetric water content of the QC. Calculations 8.10 Dry the clod in an oven at 110°C overnight and record oven-dry weight (WODC). 7.11 If the clods contains >5% in rock fragments by weight. weight of oven-dry plastic coat TAG = Weight of tag and wire 8.. If the rock fragments have similar properties to the soil sample.6 Saturate the ceramic plate by applying RO water through the adapter and apply enough pressure so that the rubber membrane is bulging a few centimeters.(WODC . sieved soil as a quality control (QC) sample. If the water content of the QC is higher than twice the standard deviation.RF . 7. 7. Prepare a saturated. When the clod is equilibrated at 33 kPa and bulk density is to be measured. Care should be taken to remove all air. apply pressure for additional time. Fill the retaining rings with the soil standard. If additional water retention points are requested. then the apparatus has functioned properly.2 MPC = {[(CC2 .ODPC) x 100]/(WODC . Dry and record the weight (RF) of the rock fragments that are retained on the sieve. If the water content of the QC is lower than twice the standard deviation. Close the container and secure lid.ODPC – TAG) where: H2O % = Percent gravimetric water content WMC = Weight of equilibrated. the clod is at equilibrium. If more than one water retention point is requested.85. cover the ceramic plate with a 5-mm layer of silt loam soil and saturate with water.

p. WI.) Methods of soil analysis.. Part 4. 635-662. U. 1986. p. Madison. USDA Handb. and J.A. R.) Methods of soil analysis.1 percent. Print. WI. Madison. Richards (ed. Book Series No. and R. In J. Physical and mineralogical methods.5 x [(CC2 . 5. Dane and G. L. 2nd ed. 1954. 60. 1986. ASA and SSSA. 2002. Soil Sci. DC. J. Dane. Office. References Bruce. 9. Physical methods.CC1)/3] where: FCE = Estimate of field-applied plastic coat. Agron. 675720. ASA and SSSA.) Methods of soil analysis. Topp (eds. Govt. 663-686. ASA and SSSA. In A. p. 9. Salinity Laboratory Staff.. if applied 9.where: MPC = Weight of plastic coat before oven-drying CC2 = Weight of clod after three laboratory plastic coats CC1 = Weight of clod before three laboratory plastic coats RV = Percent estimate of remaining clod volume after cutting to obtain flat surface (≈ 80%) 8.C.S. U. In A. 112 .H. Part 1. Luxmoore.3 FCE = 1. Agron. Monogr. Klute (ed. WI.R. Physical and mineralogical methods. Report Report water content to the nearest 0. Klute (ed. Water retention and storage: Laboratory. Hopmans.S. A. W. Klute. Part 1. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 11. Madison. Am. Washington. Water retention: Laboratory methods.J.) Diagnosis and improvement of saline and alkali soils. 2nd ed. Water retention: field methods.H. 10. Monogr.

113 . Fig. Pressure-plate extraction at 33-kPa for clods. 2.Fig 1. Clods placed in pressure-plate extractor following saturation.

1000 mL of 1 N HCl. 1986). With extended use. 1954) is used. The sample weight is recorded. Laboratory-determined. 2002). water-holding capacity. and 500 mL of RO water. pore-size distribution. 10. The cores are then transferred to a porous ceramic plate which is placed in a pressure-plate extractor. 1986). Pressing the cylinder into the soil reduces the risk of shattering the sample. and the waste is captured in a trap. water retention data are usually higher than field-determined. Do not drop the heavy lid. If compression is excessive. A metal cylinder is pressed or driven into the soil. Compression can be observed by comparing the soil elevation inside the cylinder with the original soil surface outside the cylinder. The pressure should be monitored for stability. Aerated 0. Procedures 3C1a-d3 are used to determine the water retention of soil cores at 6. or 100 kPa (3C1a-d) Soil Cores (3C1a-d3) 1. porosity. Application The data collected are used for the water retention function. 114 . If air bubbles escape from the membrane. The sample is dried in the oven and then weighed. The sample is equilibrated at the specified pressures. The data are also used to calculate unsaturated hydraulic conductivity. Dry or hard soils often shatter when hammering the cylinder into the soil. soil core may not be a valid sample for analysis. 33. 2. and saturated conductivity of a soil sample at specific water contents. Salinity Laboratory Staff. the porous ceramic plate becomes clogged and water outflow is restricted. 10. The solutions are pulled through the plate with a vacuum. 3. 2002).S. the cylinder extracts a sample of known volume. has also been recommended (Dane and Hopmans. Soil core is placed on a tension table and equilibrated at a 5-cm tension at the base of the sample. The rubber membrane on the bottom of the plate is checked for leaks in the gasket. The gravimetric water content is determined. Rock fragments in the soil interfere with core collection. The pressure is kept constant until equilibrium is obtained (Klute. Compaction of the sample during the sampling process is a common problem. Upon removal from the soil. The plate is cleaned by flushing sequentially with 500 mL of 10% H2O2.Water Retention (3C) Pressure-Plate Extraction (3C1) 6. the plate is removed from service. 4. affecting the water content at a given pressure head (Dane and Hopmans. Interferences A leaking pressure extractor prevents equilibration of samples. Ensure that the bolts are tightened before applying pressure. 33. Summary of Method The pressure desorption procedure (U. especially for fine-textured soils that contain significant amounts of swelling clays. respectively. water retention data because the confining soil pressure is not present in the laboratory (Bruce and Luxmoore. Distilled or deionized water can possibly promote dispersion of clays in samples and freshly drawn tap water is often supersaturated with air.005 M CaSO4. Check for outflow air to verify that the extractor is functioning properly and does not leak. Ensure that the pressure is zero before removing bolts from the pressure-apparatus lid. Safety High pressure plumbing must be maintained in good working order. Equilibration must be done at constant temperature and humidity. or 100 kPa. The membrane is inflated and then submerged in water.

covered with reinforced paper towels. place core in a desiccator on a water-covered plate with a 0cm tension. for tension table.2 Hydrogen peroxide (H2O2).9 Vacuum.3 Prepare a flat surface in the sampling pit.16 Retainer rings.7 Silt loam soil 5. Care should be taken to remove all air. 80 kPa (0. Use inhouse vacuum and apply suction until core has equilibrated at saturation. Remove the core and record the weight (WSC). Submerge only the surface of core in the water.11 Sieve. 6.2 Pressure plate extractor with porous ceramic plate 5.6 Metal weighing cans with lids 5. 6. Periodically. at the required depth. and gauge 5.8 bar) 5.6 Microbiocide. touching. Add a few mL of alcohol. Press or drive the core sampler into the soil. Use 10-mm high and 50-mm diameter rings for organic soils and 10-mm high and 40-mm diameter rings for all other soils. The SSL constructs a tension table by placing porous firebricks. When the core has reached equilibrium. 7. Dilute 83.8 Desiccator with ceramic plate 5. ±0.3 mL of concentrated HCl in 1 L of RO water. 10% solution. 5. technical grade. Use caution to prevent compaction. 7.13 Coring equipment. either horizontal or vertical. and place core in an air-tight container for transport to the laboratory. Dilute 333 mL of 30% H2O2. 1 N. Equipment 5.5 Liquid detergent. regulator. Sources described in Blake and Hartge (1986). check the core by inserting a needle probe.01-g sensitivity 5. Procedure 7.4 It is necessary to wet the core above the initial desorption point. This is accomplished by placing the flat core surface on a tension table maintained at 5-cm tension.3 Pressure source. trim the protruding soil flush with the cylinder ends. 10 (2-mm openings) 5.6 Saturate the ceramic plate by applying RO water through the adapter and apply enough pressure so that the rubber membrane is bulging a few centimeters. remove the core and record the weight (WSC). in l L of RO water. 6. 5. The SSL uses Liqui-Nox.12 Fume hood 5.1 Reverse osmosis (RO) water 6.4 Alcohol 6. Fisher Scientific 7.5.15 Reinforced paper towels with nylon fibers.14 Tension table. No. 6. Reagents 6.4 Oven. 10-mm height and 40-mm diameter 5. 110°C 5. 7. 7. Remove the core from the sample holder.10 Needle probe 5. GSA 5.5 If core does not absorb water. or by weight comparison to determine if core has reached equilibrium (core has wetted up).5 Retainer rings.3 Hydrochloric acid (HCl). 7. in a tub of water. 115 .1 This procedure can be combined with the bulk density procedure (3B1b).1 Electronic balance.2 Record the weight (CW) of the sampling cylinders.

Part 1. 11. Soil Sci. Hopmans.8 Apply gauged air pressure of 6. WI. 8. p.7 Place the saturated ceramic plate in a pressure plate extractor. ASA and SSSA.J. Prepare a saturated. Am. Dane. 7.7.) Methods of soil analysis. 1986. 5. the core is at equilibrium.. Water retention: field methods. Madison. In J. and R. Recheck the QC. Place a sheet of reinforced paper towel over the silt loam soil. Monogr. If the water content of the QC is higher than twice the standard deviation. Book Series No. If WMC > WSC..) Methods of soil analysis. Report Report water content to the nearest 0. do not correct the clod mass for the rock fragments. Place the flat core surface on the paper towel. Klute (ed. Water retention and storage: Laboratory. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. WI. If additional water retention points are requested. W. R.10 Dry core in an oven at 110°C overnight and record oven-dry weight (WODC). J. 663-686. re-equilibrate core on the tension table and repeat the desorption process. Close the container and secure lid. Part 4. Topp (eds. and J. When water stops discharging from the outflow tube. begin with the lowest pressure. Calculations H2O % = 100 x [(WMC .C. 7.R. Determine the gravimetric water content of the standard. 33. References Bruce. Luxmoore. wet sieve the sample through a 2-mm sieve. If the water content of the QC is within acceptable limits. Dane and G. 675720. Record the weight of the rock fragments (RF). Dry and weigh the rock fragments that are retained on the sieve. Physical and mineralogical methods.9 Remove core and record the weight (WMC). then repeat the desorption process at the next higher pressure. 9. apply pressure for additional time.WODC)/(WODC . . In A. If more than one water retention point is requested. Compare WMC to WSC. If the rock fragments have similar properties to the soil sample. Madison. 7. continue with method 3B1b. Agron.H. 2002. Physical methods. 116 . 10. 2nd ed. rewet the cores and desorb again. If the water content of the QC is lower than twice the standard deviation. 10.RF)] where: H2O % WMC CW WODC RF = Percent gravimetric water content = Weight of solids + H2O + container = Weight of solids + container = Weight of container = Weight of rock fragments 9. ASA and SSSA. cover the ceramic plate with a 5-mm layer of silt loam soil and saturate with water. then the apparatus has functioned properly. or 100 kPa.CW . When the core is equilibrated at 33 kPa and bulk density is to be measured. sieved soil as a quality control (QC) sample. Fill the retaining rings with the soil standard. Place several retaining rings in the extractor.H. 7. To provide good contact between the core and ceramic plate.11 If sample contains rock fragments. p.1 percent.

Interferences A leaking pressure extractor prevents equilibration of samples.) Diagnosis and improvement of saline and alkali soils. ASA and SSSA. If air bubbles escape from the membrane. 2002). L. The equilibrated clod weight is recorded. Check outflow air to verify each pressure-plate extractor is functioning properly and does not leak. Monogr. A. Ensure that the pressure is zero before removing bolts from the pressure-plate lid. The rubber membrane on the bottom of the plate is checked for leaks in the gasket. U.S. Distilled or deionized water can possibly promote dispersion of clays in samples and freshly drawn tap water is often supersaturated with air. USDA Handb. 2002). Washington. especially for fine-textured soils that contain significant amounts of swelling clays. 1954) is used. 1986. Office. 1954. 117 . The pressure should be monitored for stability. With extended use. Klute (ed. The plate is cleaned by flushing sequentially with 500 mL of 10% H2O2. Madison.A. Richards (ed. pore-size distribution. Agron. and saturated conductivity of a soil sample at specific water contents. Part 1. The rewet water retention data (3C1c4) are used in conjunction with the rewet bulk density (3B1d) to estimate the change in physical properties of a soil as it undergoes wetting and drying cycles. and 500 mL of RO water. Ensure that the bolts are tightened before applying pressure. Summary of Method The pressure desorption method (U. Water retention: Laboratory methods. Laboratory-determined. Salinity Laboratory Staff. Aerated 0. Govt.S. Salinity Laboratory Staff. The solutions are pulled through the plate with a vacuum. 2nd ed. affecting the water content at a given pressure head (Dane and Hopmans. the plate is removed from service. Water Retention (3C) Pressure-Plate Extraction (3C1) 33 kPa (3C1c) Rewet (3C1c4) 1. U. 4. Application The data collected are used for the water retention function. 60.005 M CaSO4. The data are also used to calculate unsaturated hydraulic conductivity.) Methods of soil analysis. Physical and mineralogical methods. Equilibration must be done at constant temperature and humidity. 1986). After the second equilibration. Safety High pressure plumbing must be maintained in good working order. Print. The clods are then transferred to a porous ceramic plate which is placed in a pressure-plate extractor. DC. 635-662. water retention data because the confining soil pressure is not present in the laboratory (Bruce and Luxmoore. In A. porosity. 9. and the waste is captured in a trap. Natural clods are placed on a tension table and equilibrated at a 5-cm tension at the base of the sample. The clod is air dried and then placed on a tension table and desorbed again. Do not drop the heavy lid. The sample is equilibrated at 33kPa. 3. has also been recommended (Dane and Hopmans. the porous ceramic plate becomes clogged and water outflow is restricted. 2. 1000 mL of 1 N HCl. p. the gravimetric water content is determined.S. WI. water-holding capacity. The membrane is inflated and then submerged in water. 1986). water retention data are usually higher than field-determined.Klute. The pressure is kept constant until equilibrium is obtained (Klute.

4 Oven.15 Hot plate 5.8 bar) 5. 95%. 80 kPa (0. Acetone may be substituted for MEK. technical grade 6. Record the weight of the clod (CC1). The SSL uses Liqui-Nox.5 Retainer rings.1 Reverse osmosis (RO) water 6.2 Hydrogen peroxide (H2O2). 6. In the laboratory.14 Sieve. Reagents 6. 6. Use 1:7 plastic lacquer for the last two laboratory coats. covered with reinforced paper towels. Add 540 g or 305 g of resin to make 1:4 or 1:7 plastic lacquer. Procedure 7. 10-mm height and 40-mm diameter 5.17 Reinforced paper towels with nylon fibers. regulator. For the initial field and laboratory coatings. Cut the copper wire. with metal rim 5.4 Ethyl alcohol. 25. Fill a 3.13 Needle probe 5. high speed stirrer while slowly adding resin. 10% solution. The 1:7 plastic lacquer is used to conserve the resin and to reduce cost.3 Pressure source. Equipment 5.05 N.20 Stock tags.4-mm (1-in) diameter paper tag. for tension table. and gauge 5. 6. ±0. Dilute 8 mL of concentrated HCl in 1 L of RO water. GSA 5.10 Silt loam soil 5. stir solvent with a non-sparking.7 Dow Saran F-310 Resin. Fisher Scientific 7.8 Knife 5. 6. 10 (2-mm openings) 5.6 Methyl ethyl ketone (MEK).5. Stir plastic lacquer for 15 min at 25°C. practical (2-butanone) 6. in a tub of water. Fill to the bottom of handle rivet. mix solvent with a wooden stick.19 Tension table.21 Wire.5 Liquid detergent.1 Electronic balance.2 Prepare a round stock tag with sample identification number. The SSL uses a 28-awg coated copper wire. technical grade.9 Microbiocide. respectively.8 Plastic lacquer. 6.11 Desiccator with ceramic plate 5. 6. Store plastic lacquer in covered plastic or steel containers. Loop fine copper wire around the clod.2 Pressure plate extractor with porous ceramic plate 5. 110°C-capability 5. Prepare plastic lacquer with resin to solvent ratios of 1:4 and 1:7 on a weight basis. 5. In the field. The SSL constructs a tension table by placing porous firebricks. 5.1 This procedure is usually used in conjunction with the bulk density procedure 4A1i. 118 .16 Fume hood 5.8-L (1-gal) metal paint can with 2700 ±200 mL of solvent. Record the weight of the tag and wire (TAG).6 Metal weighing cans with lids 5. use the 1:4 plastic lacquer.3 Hydrochloric acid (HCl). No.12 Vacuum.18 Liquid vapor trap.01-g sensitivity 5. The SSL constructs a tin enclosure over hot plate with a chimney and duct to transfer vapor to water stream. Use 10-mm high and 50-mm diameter rings for organic soils and 10-mm high and 40-mm diameter rings for all other soils. 0. 7. in l L of RO water. leaving a tail to which the round stock tag is attached.9 Tile cut-off saw with diamond blade 5. 5. Available from Dow Chemical Company.7 Clothespins 5. Dilute 333 mL of 30% H2O2.22 Retainer rings.

13 Dry the clod in oven at 110°C overnight and record oven-dry weight (WODC). 7. 7. continue with procedure 3B1d 7. Care should be taken to remove all air. 7.9 Apply gauged air pressure of 6. This is accomplished by placing the cut clod surface on a tension table that is maintained at 5-cm tension. This determination of the percent rock fragments is based on particle-size data of >2-mm fraction. 7. If additional water retention points are requested. cover the ceramic plate with a 5-mm layer of silt loam soil and saturate with water. 119 . re-equilibrate the clod on the tension table and repeat the desorption process. 10. Wait 7 min and then dip the clod in the 1:7 plastic lacquer.6 If cut clod does not absorb water. Wait 12 min and then dip the clod in the 1:7 plastic lacquer. Use in-house vacuum and apply suction until clod has equilibrated at saturation. Place cut clod surface on the paper towel. 7. Add a few mL of alcohol. and 7. apply pressure for additional time. the clod is at equilibrium. Remove the clod and record the weight (WSC). Periodically check the clod by inserting a needle probe. 33. Prepare a saturated.11 Air-dry the clod at room temperature (≈ 20 to 25°C) for 4 to 6 days. Submerge the remaining soil material in a beaker of water and place on a hot plate.14 If the clod contains >5% in rock fragments by weight. rewet the clods and desorb again. 7. Dry the clods at 40 to 50°C for 2 to 3 days or until weights are constant.7.3 Dip the clod in the 1:4 plastic lacquer. then reweigh the clod and record the weight (CC2). When the clod is equilibrated at 33 kPa and bulk density is to be measured. remove the rock fragments from the clod. When water stops discharging from the outflow tube. Place a sheet of reinforced paper towel over the silt loam soil. Determine the gravimetric water content of the QC. sieved soil as a quality control (QC) sample. Place several retaining rings in the extractor.5.8 To provide good contact between the clod and ceramic plate. 7. begin with the lowest pressure. If WMC > WSC. Close the container and secure lid.8. If the water content of the QC is lower than twice the standard deviation. touching. Compare WMC to WSC. Wait 55 min and then reweigh the clod. If the water content of the QC is higher than twice the standard deviation. then the apparatus has functioned properly. place clod in a desiccator on a water-covered plate with a 0-cm tension. 7. Fill the retaining rings with the soil standard. or by weight comparison to determine if it has reached equilibrium (clod has wetted up). 7. When the clod has reached equilibrium. allow longer drying time.7 Saturate the ceramic plate by applying RO water through the adapter and apply enough pressure so that the rubber membrane is bulging a few centimeters. Determine bulk density as described in method 3B1d. If the clod has absorbed >3% in plastic by clod weight or smells excessively of solvent.4 Cut a flat surface on the clod with a tile saw. 7.10 Remove the clod and record the weight (WMC). If more than one water retention point is requested.7.12 Repeat steps 7.6. Recheck the QC. If the water content of the QC is within acceptable limits. 7. or 100 kPa. Record clod weight after equilibration (WMC2). Submerge only the surface of clod in the water.5 It is necessary to wet the clod above the initial desorption point. 7. then repeat the desorption process at the next higher pressure. remove the clod and record the weight (WSC).

weight of oven-dry plastic coat TAG = Weight of tag and wire 8. p. do not correct the clod mass for the rock fragments.R. W. Part 1.1 H2O % =[(WMC . 663-686. Madison.J.85. Luxmoore. Book Series No. Am. In A.4 H2Or % = {[(WMC2 .ODPC) x 100]/(WODC . 11. ASA and SSSA.85. Calculations 8. Monogr. J.Use a fume hood. 10. and R. 8. p. Physical methods. ASAS and SSSA. Water retention: Field methods. 5. coated clod WODC= Weight of oven-dry coated clod RF = Weight of rock fragments ODPC = MPC x 0. 675-720. If the rock fragments have similar properties to the soil sample.) Methods of soil analysis. if applied 8. Water retention and storage: laboratory.(WODC .ODPC2)] x 100}/(WODC . Dane and G. References Bruce.15 Wet sieve the cool soil through a 2-mm sieve. Discard plastic coating. Dane. Physical and mineralogical methods. Same as MPC unless additional plastic coats were added. Report Report water content to the nearest 0.) Methods of soil analysis. Part 4. Dry and record the weight (RF) of the rock fragments that are retained on the sieve. Hopmans. Madison. Agron.RF – ODPC – TAG) where: H2Or % = Percent water weight retained at 33-kPa tension after rewetting WMC2 = Weight of equilibrated. OPC2 = MPC2 x 0.5 x [(CC2 – CC1)/3] where: FCE = Estimate of field applied plastic coat.MPC) .C. 2002. 2nd ed.RF – ODPC – TAG) where: H2O % = Percent gravimetric water content WMC = Weight of equilibrated. coated clod after rewetting MPC2 = Weight of moist plastic coat after rewetting.(WODC . R.1 percent.2 MPC = {[(CC2 – CC1) + FCE] x RV} where: MPC = Weight of plastic coat before oven-drying CC2 = Weight of clod after three laboratory plastic coats CC1 = Weight of clod before three laboratory plastic coats RV = Percent estimate of remaining clod volume after cutting to obtain flat surface (≈ 80%) 8. Soil Sci.MPC2) . Boil ≈ 1 h. weight of oven-dry plastic coat. The plastic coating loosens from soil material upon heating. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.H. 9. 7.. In J. and J. WI. 120 .. Remove beaker from the hot plate.H.3 FCE = 1. 1986. Allow to cool. 9. WI. Klute (ed. Topp (ed.

Salinity Laboratory Staff. The gravimetric water content is determined. DC. Laboratory-determined. 635-662. 2002). Water Retention (3C) Pressure-Plate Extraction (3C1) 33 kPa (3C1c) Reconstituted (3C1c5) 1. 2. With extended use. Ensure that the bolts are tightened before applying pressure. 1986). 4. especially for fine-textured soils that contain significant amounts of swelling clays. Natural clods are placed on a tension table and equilibrated at a 5-cm tension at the base of the sample. Interferences A leaking pressure extractor prevents equilibration of samples. 2002). If air bubbles escape from the membrane. ASA and SSSA. water-holding capacity. Richards (ed. 2nd ed. U. 1986. Klute (ed. porosity. 1986). Washington. Physical and mineralogical methods.005 M CaSO4 has also been recommended (Dane and Hopmans. Govt. 60. Dept.01-g sensitivity 5. The sample is equilibrated at the specified pressures. and 500 mL of RO water. 1954) is used. Application The data collected are used for the water retention function. Ensure that the pressure is zero before removing bolts from the pressure-apparatus lid. Print. Part 1.) Diagnosis and improvement of saline and alkali soils. p. Safety High pressure plumbing must be maintained in good working order. The plate is cleaned by flushing sequentially with 500 mL of 10% H2O2. WI. Equipment 5. Summary of Method The pressure desorption method (U. 3. Methods of soil analysis.S.S. Water retention: Laboratory methods. The solutions are pulled through the plate with a vacuum. affecting the water content at a given pressure head (Dane and Hopmans. Madison.S. L. ±0. 5. Procedure 3C1c5 is used to determine the water retention of a reconstituted clod at 33 kPa. The clods are then transferred to a porous ceramic plate which is placed in a pressure-plate extractor. water retention data are usually higher than field-determined. the porous ceramic plate becomes clogged and water outflow is restricted. Salinity Laboratory Staff. 9. Aerated 0. U. Distilled or deionized water can possibly promote dispersion of clays in samples and freshly drawn tap water is often supersaturated with air.A. water retention data because the confining soil pressure is not present in the laboratory (Bruce and Luxmoore. Handb. U. Agron. Check outflow air to verify that each pressure-plate extractor is functioning properly and does not leak. 1000 mL of 1 N HCl. The pressure should be monitored for stability. the plate is removed from service. Office. and saturated conductivity of a soil sample at specific water contents.S. 1954. The membrane is inflated and then submerged in water.2 Pressure plate extractor with porous ceramic plate 121 . Monogr. The pressure is kept constant until equilibrium is obtained (Klute.). pore-size distribution. In A. of Agric. The rubber membrane on the bottom of the plate is checked for leaks in the gasket. and the waste is captured in a trap. Equilibration must be done at constant temperature and humidity. The data are also used to calculate unsaturated hydraulic conductivity.1 Electronic balance.Klute. A. Do not drop the heavy lid.

technical grade. Cut the copper wire and loop around the clod.8-L (1-gal) metal paint can with 2700 ± 200 mL of solvent. with metal rim 5.1 This procedure is usually combined with the bulk density procedure (3B2b). Use 10-mm high and 50-mm diameter rings for organic soils and 10-mm high and 40-mm diameter rings for all other soils.17 Reinforced paper towels with nylon fibers.14 Sieve.21 Wire. 10% solution.19 Tension table. The 1:7 plastic lacquer is used to conserve the resin and to reduce cost. 122 . technical grade 6.3 mL of concentrated HCl in 1 L of RO water. Store plastic lacquer in covered plastic or steel containers.4 Oven. Procedure 7. 6.4 Ethyl alcohol. Prepare plastic lacquer with resin to solvent ratios of 1:4 and 1:7 on a weight basis. and gauge 5. GSA 5. stir solvent with a non-sparking. 7. 1 N. For the initial field and laboratory coatings.7 Clothespins 5. Record the weight of the tag and wire (TAG). The SSL uses Liqui-Nox. Reagents 6. in a tub of water. The SSL constructs a tin enclosure over hot plate with a chimney and duct to transfer vapor to water stream. 5.1 Reverse osmosis (RO) water 6.3 Hydrochloric acid (HCl). 25.6 Methyl ethyl ketone (MEK). 10-mm height and 40-mm diameter 5. Dilute 83. Dilute 333 mL of 30% H2O2. 6. 80 kPa (0.18 Liquid vapor trap.5. mix solvent with a wooden stick.9 Tile cut-off saw with diamond blade 5. Add 540 g or 305 g of resin to make 1:4 or 1:7 plastic lacquer. practical (2-butanone) 6. Record the weight of the clod (CC1). covered with reinforced paper towels. The SSL uses a 28-awg coated copper wire.5 Retainer rings.9 Microbiocide. Fill to the bottom of handle rivet.13 Needle probe 5. No.6 Metal weighing cans with lids 5.2 Hydrogen peroxide (H2O2). Loop fine copper wire around the clod. leaving a tail to which the round stock tag is attached.8 Plastic lacquer.16 Fume hood 5.5 Liquid detergent. 5. The SSL constructs a tension table by placing porous firebricks. 95%. use the 1:4 plastic lacquer. Stir plastic lacquer for 30 min at 25°C. Available from Dow Chemical Company. 10 (2-mm openings) 5.22 Retainer rings. for tension table.12 Vacuum.8 Knife 5. in l L of RO water.2 Prepare a round stock tag with sample identification number.11 Desiccator with ceramic plate 5. Fisher Scientific. Fill a 3.15 Hot plate 5. 7. 6. high speed stirrer while slowly adding resin. In the field.20 Stock tags. 6.4-mm (1-in) diameter paper tag. 6. 110°C 5. In the laboratory.3 Pressure source. Acetone may be substituted for MEK. Use 1:7 plastic lacquer for the last two laboratory coats.7 Dow Saran F-310 Resin.8 bar) 5. 5. 6. regulator. respectively.10 Silt loam soil 5.

Determine the gravimetric water content of the QC. 7. The outflow tube can be submerged under water in a burette to measure when water ceases to emit from the outflow tube. This determination of the percent rock fragments is based on particle-size data of >2mm fraction. Submerge only the surface of clod in the water. Prepare a saturated. Discard plastic coating. Wait 7 min and then dip the clod in the 1:7 plastic lacquer.7 Place the saturated ceramic plate in a pressure plate extractor. or by weight comparison to determine if it has reached equilibrium (clod has wetted up). If the water content of the QC is within acceptable limits.5 If cut clod does not absorb water. then the apparatus has functioned properly. 7. rewet the clods and desorb again. If more than one water retention point is requested. 7.10 Dry the clod in an oven at 110°C overnight and record oven-dry weight (WODC). If the water content of the QC is lower than twice the standard deviation. Fill the retaining rings with the soil standard. Use a fume hood. begin with the lowest pressure. Use in-house vacuum and apply suction until clod has equilibrated at saturation. This is accomplished by placing the cut clod surface on a tension table that is maintained at 5-cm tension. Place cut clod surface on the paper towel.. To provide good contact between the clod and ceramic plate.3 Dip the clod in the 1:4 plastic lacquer. When the clod has reached equilibrium. 123 . Compare WMC to WSC. If the clod has absorbed >3% in plastic by clod weight or smells excessively of solvent.6 Saturate the ceramic plate by applying RO water through the adapter and apply enough pressure so that the rubber membrane is bulging a few centimeters. Wait 12 min and then dip the clod in the 1:7 plastic lacquer. Boil ≈ 1 h. Submerge the remaining soil material in a beaker of water and place on a hot plate. remove the clod and record the weight (WSC). 7. If WMC > WSC. 7. Wait 55 min and then reweigh the clod.8 Apply gauged air pressure of 33 kPa. cover the ceramic plate with a 5-mm layer of silt loam soil and saturate with water. then repeat the desorption process at the next higher pressure. Add a few mL of alcohol. the clod is at equilibrium. re-equilibrate the clod on the tension table and repeat the desorption process. If the water content of the QC is higher than twice the standard deviation. allow longer drying time. apply pressure for additional time. If additional water retention points are requested. sieved soil as a quality control (QC) sample. continue with procedure 3B1b. Place several retaining rings in the extractor. 7.7. remove the rock fragments from the clod. Periodically submerge the outflow tube in water to monitor for air bubbles that indicate ceramic plate failure. The plastic coating loosens from soil material upon heating. Periodically check the clod by inserting a needle probe. Care should be taken to remove all air.4 Cut a flat surface on the clod with a tile saw. touching. When water stops discharging from the outflow tube. Allow to cool. When the clod is equilibrated at 33 kPa and bulk density is to be measured.11 If the clods contains >5% in rock fragments by weight. 7. It is necessary to wet the clod above the initial desorption point. Samples are equilibrated when water ceases to emit from the outflow tube. place clod in a desiccator on a water-covered plate with a 0-cm tension. 7. Recheck the QC. Remove beaker from the hot plate. Remove the clod and record the weight (WSC).9 Remove the clod and record the weight (WMC). Close the container and secure lid. then reweigh the clod and record the weight (CC2). Place a sheet of reinforced paper towel over the silt loam soil.

do not correct the clod mass for the rock fragments.R.7. Physical methods. 675720. 1954.RF . Water retention and storage: Laboratory. weight of oven-dry plastic coat TAG = Weight of tag and wire 8.(WODC . and J. USDA Handb. References Bruce.) Methods of soil analysis. Calculations 8.5 x [(CC2 . Part 1.S.CC1)/3] where: FCE = Estimate of field-applied plastic coat.1 H2O % =[(WMC . p. 2nd ed. DC. Dane and G. ASA and SSSA. 124 .J.) Methods of soil analysis. Hopmans. 635-662.H. A. In A. 2nd ed. Dane. coated clod WODC= Weight of oven-dry coated clod RF = Weight of rock fragments ODPC = MPC x 0.ODPC – TAG) where: H2O % = Percent gravimetric water content WMC = Weight of equilibrated. Soil Sci. 2002.2 MPC = {[(CC2 . 60. Am. W. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.1 percent. Report Report water content to the nearest 0.H. if applied 9. In J. Book Series No. If the rock fragments have similar properties to the soil sample. Physical and mineralogical methods. Physical and mineralogical methods. 8. WI. Print. ASA and SSSA. ASA and SSSA. Govt.. Water retention: field methods. 12. WI. 10. p. Monogr. p. Madison. L. U.MPC) . Luxmoore. Salinity Laboratory Staff. Dry and record the weight (RF) of the rock fragments that are retained on the sieve. 1986. In A.85. Agron. Topp (eds.CC1) + FCE] x RV} where: MPC = Weight of plastic coat before oven-drying CC2 = Weight of clod after three laboratory plastic coats CC1 = Weight of clod before three laboratory plastic coats RV = Percent estimate of remaining clod volume after cutting to obtain flat surface (≈ 80%) 8. Madison. Part 1. 5.12 Wet sieve the cool soil through a 2-mm sieve. Office. Agron.C. 9. Water retention: Laboratory methods. Klute (ed. 9. Monogr. WI. and R. Klute (ed.. U. R.ODPC) x 100]/(WODC . Madison.) Methods of soil analysis.A.S. Klute. 1986. Part 4. Washington.) Diagnosis and improvement of saline and alkali soils. J.3 FCE = 1. Richards (ed. 663-686.

1986).4 Electronic balance. 5. porosity. The pressure should be monitored for stability. Safety High-pressure plumbing must be maintained in good working order. technical grade 6. The sample is equilibrated at 1500 kPa. water retention data are usually higher than field-determined. and gauge 5. Aerated 0.6 Pressure source. Reagents 6. Distilled or deionized water can possibly promote dispersion of clays in samples and freshly drawn tap water is often supersaturated with air. The pressure is kept constant until equilibrium is obtained (Klute.1 Ethyl alcohol.Water Retention (3C) Pressure-Membrane Extraction (3C2) 1500-kPa (3C2a) <2-mm (sieved). 2002). Use 10-mm height and 50-mm diameter rings for organic soils and 10-mm height and 40-mm diameter rings for all other soils. 3.005 M CaSO4 has also been recommended (Dane and Hopmans. 2002). Equipment 5. 2.7 Metal weighing cans. water retention data because the confining soil pressure is not present in the laboratory (Bruce and Luxmoore. Ensure that the pressure is zero before removing bolts from the pressure-apparatus lid. Air-Dry Samples (3C2a1a) 1. Application The data collected are used for the water retention function.01-g sensitivity 5. Check outflow air to verify that the pressure membrane extractor is functioning properly and does not leak. The membrane is covered with water to wet the samples by capillarity. 1954) is used. Ensure that the bolts are tightened before applying pressure. Samples that do not wet by capillarity are moistened with ethyl alcohol.5 Oven.9 Vacuum. water-holding capacity. affecting the water content at a given pressure head (Dane and Hopmans. air-dry soil is placed in a retainer ring sitting on a cellulose membrane in a pressure-membrane extractor. Procedure 3C2a1a is used to determine the water retention at 1500 kPa for <2-mm (sieved).1 and 2) 5. pore-size distribution. 80 kPa (0. Do not drop the heavy lid.8 bar) 6. Laboratory-determined. 1986).1 Pressure membrane extractor (Fig. The data are also used to calculate unsaturated hydraulic conductivity. Interferences A leaking pressure extractor prevents equilibration of samples. Equilibration must be done at constant temperature and humidity. air-dry soil samples. 95%.2 Cellulose membrane 5. Summary of Method The pressure desorption procedure (U. with lids 5. ±0.2 Reverse osmosis (RO) water 125 . The gravimetric water content is determined. Salinity Laboratory Staff. 4.S. A sample of <2-mm (sieved). regulator.3 Retainer rings. tared. and saturated conductivity of a soil sample at specific water contents. especially for fine-textured soils that contain significant amounts of swelling clays. 5.8 Vacuum trap assembly 5. 110°C 5.

and record the weights (Ms). place samples in the oven. 7.1 percent. Procedure 7.8 Remove the lids. 7.Ms)/ (Ms . Properties of gypsiferous soils such as 1500-kPa water content that are reported on an oven-dry weight basis are converted to include the weight of crystal water in gypsum. Report Report water content to the nearest 0.4 Remove excess water on the plate with a vacuum and trap assembly. and let stand overnight.2 Add water and retaining rings. Use 5-cm diameter rings for soils that are >12% in organic matter. 7. 126 .1 Submerge a cellulose membrane in RO water for 12 h or more before use. Gypsum content of the soil is determined in procedure 4E2a1a1. The samples are equilibrated when water ceases to emit from the outflow tube. Install the wet cellulose membrane in the pressure extractor. The 1500-kPa water content is corrected when the gypsum content of the soil is >1%. open the extractor and quickly transfer the samples to water cans.5 kPa (150 psi). 9. Calculations H2O % = 100 x [(Ms+w . Remove samples from the oven. allow cans to cool to ambient temperature.7 At equilibrium. Include a quality control (QC) sample with each plate. Cover samples with a sheet of plastic to reduce evaporation.5 Assemble the extractor and uniformly tighten the bolts. 7. Torque the remaining bolts to 103. Use 4-cm diameter rings for all other soils. apply ethyl alcohol to the surface of the sample.3 Fill retaining rings with 10 to 15 g of <2-mm or fine-grind. This forces the rubber diaphragm against the top of the samples. Allow ethyl alcohol to evaporate. After 4 h. cover with lids. 8. Continue to add water until all samples have moistened by capillarity.6 Increase air pressure ≈ 150 kPa every 15 min until 1500 kPa is reached. Quickly close the pressure release valve. and dry at 110°C overnight.Mc)] where: H2O % = Percent gravimetric water content Ms+w = Weight of solids + H2O + container Ms = Weight of solids + can Mc = Weight of container Gypsiferous soils are a special case because gypsum (CaSO4·2H2O) loses most of its two water molecules at 105°C.7. air-dry soil sample. Refer to procedure 3D3 for these conversion calculations. close the extractor.0 kPa (200 psi). apply the pressure differential by closing the valve that joins the mercury circuit and by opening the pressure release valve until air is forced through the mercury. Torque the bolts on both sides of the hinge to 138. 7. Add enough water to keep membrane moist. If samples do not moisten. 7. replace the lids. and record the weights (Ms+w).9 Record the weights of the empty cans (Mc). 7. 7. Water level should be less than height of retaining rings.

J. and R. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 127 . Print. L. Agron. DC. Soil Sci. Water retention: Laboratory methods. Soc. Determining soil content and expressing properties of gypsiferous soils. Water retention and storage: Laboratory. Salinity Laboratory Staff. Madison. Handb. Part 1. Physical methods. 2002.. 9. A. 5. 1986. Nettleton. p.R. ASA and SSSA. WI. Nelson.10. USDA Agric.H. J. Washington.S. Klute (ed. ASA and SSSA. 60. Klute. Luxmoore. Richards (ed. Monogr. Part 1. U. Am. R. 1986. WI. L. Dane..D. 663-686. Water retention: Field methods.. Physical and mineralogical methods. References Bruce. 1978. U. Agron. 11. Klute (ed.) Methods of soil analysis. Klameth. and J. In A. 2nd ed. p. Soil Sci.S. and W. Am. Office. 9.H. Madison. Hopmans. W. 675720. R. Madison.) Methods of soil analysis. Govt. WI. Book Series No. Monogr.) Methods of soil analysis. Topp (eds. J. In A. 42:659-661.A. 1954. 635-662.E.C. Dane and G.C. ASA and SSSA.) Diagnosis and improvement of saline and alkali soils. p. In J. 2nd ed. Physical and mineralogical methods. Part 4.

Figure 2. Pressure-membrane extraction at 1500-kPa for <2-mm samples. 128 .Figure 1. Sieved (<2-mm) soil placed in pressure-membrane extractor.

Ensure that the pressure is zero before removing bolts from the pressure-plate apparatus lid.005 M CaSO4 has also been recommended (Dane and Hopmans. Aerated 0.6 Pressure source. 2. The pressure is kept constant until equilibrium is obtained (Klute.4 Electronic balance. tared. water retention data are usually higher than field-determined. water retention data because the confining soil pressure is not present in the laboratory (Bruce and Luxmoore.1 Ethyl alcohol. porosity. The sample is equilibrated at 1500 kPa. water-holding capacity. Interferences A leaking pressure extractor prevents equilibration of samples. Check outflow air to verify that the pressure membrane extractor is functioning properly and does not leak. regulator. and gauge. 95%. 1986). 5. Use 10-mm height and 50-mm diameter rings for organic soils and 10-mm height and 40-mm diameter rings for all other soils. 1986).S.2 Cellulose membrane 5. Safety High-pressure plumbing must be maintained in good working order. and saturated conductivity of a soil sample at specific water contents. 80 kPa (0. A sample of <2-mm (sieved) moist soil is placed in a retainer ring sitting on a cellulose membrane in a pressure-membrane extractor. Equipment 5. Do not drop the heavy lid.8 Vacuum trap assembly 5. Field-Moist Samples (3C2a1b) 1. ±0. pore-size distribution. Equilibration must be done at constant temperature and humidity. Laboratory-determined.01-g sensitivity 5.3 Retainer rings. affecting the water content at a given pressure head (Dane and Hopmans. The membrane is covered with water to wet the samples by capillarity.5 Oven. 2002). 1954) is used. 4. Distilled or deionized water can possibly promote dispersion of clays in samples and freshly drawn tap water is often supersaturated with air. with lids 5. Procedure 3C2a1b is used to determine the water retention at 1500 kPa for <2-mm (sieved). Ensure that the bolts are tightened before applying pressure. The gravimetric water content is determined. 5. 110°C 5.9 Vacuum. 5.1 Pressure membrane extractor 5. 3. 2002).Water Retention (3C) Pressure-Membrane Extraction (3C2) 1500-kPa (3C2a) <2-mm (sieved).8 bar) 6. Samples that do not wet by capillarity are moistened with ethyl alcohol. especially for fine-textured soils that contain significant amounts of swelling clays. Reagents 6.7 Metal weighing cans.2 Reverse osmosis (RO) water 129 . The pressure should be monitored for stability. field-moist soil samples. Summary of Method The pressure desorption method (U. technical grade 6. Application The data collected are used for the water retention function. The data are also used to calculate unsaturated hydraulic conductivity. Salinity Laboratory Staff.

Calculations H2O % = 100 x [(Ms+w . Water level should be less than height of retaining rings. Quickly close the pressure release valve.0 kPa (200 psi).7. and record the weights (Ms). Cover samples with a sheet of plastic to reduce evaporation. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Torque the bolts on both sides of the hinge to 138. place samples in the oven. replace the lids. 10. The samples are equilibrated when water ceases to emit from the outflow tube.Ms)/(Ms . 7. Use 5-cm diameter rings for soils that are >12% in organic matter.5 kPa (150 psi). Use 4-cm diameter rings for all other soils. After 4 h. allow cans to cool to ambient temperature. 7.3 Fill retaining rings with 10 to 15 g of <2-mm or fine-grind. Install the wet cellulose membrane in the pressure apparatus. 7. field moist soil sample. This forces the rubber diaphragm against the top of the samples. 8. Remove samples from the oven. If samples do not moisten.6 Increase air pressure ≈ 150 kPa every 15 min until 1500 kPa is reached. and dry at 110°C until weights are constant. open the apparatus and quickly transfer the samples to water cans. and let stand overnight. Continue to add water until all samples have moistened by capillarity. Include a quality control (QC) sample with each plate. 130 .1 percent. 7. Add enough water to keep membrane moist.5 Assemble the extractor and uniformly tighten the bolts. 7. Report Report water content to the nearest 0.1 Submerge a cellulose membrane in RO water for 12 h or more before use. 7. Procedure 7.2 Add water and retaining rings.9 Record the weights of the empty cans (Mc).Mc)] where: H2O % = Percent gravimetric water content Ms+w = Weight of solids + H2O + container Ms = Weight of solids + container Mc = Weight of container 9. apply ethyl alcohol to the surface of the sample. 7. and record the weights (Ms+w).8 Remove the lids. close the extractor.4 Remove excess water on the plate with a vacuum and trap assembly.7 At equilibrium. Torque the remaining bolts to 103. 7. cover with lids. apply the pressure differential by closing the valve that joins the mercury circuit and by opening the pressure release valve until air is forced through the mercury.

WI. and R. In A. Place samples in airtight. 7. Madison. 2nd ed.H.. U. and J. Klute. Hopmans. Madison. Part 1. J. Richards (ed. Safety Use insulated gloves to remove samples from the oven. 663-686.) Diagnosis and improvement of saline and alkali soils. 675720. 1986. ASA and SSSA.1 Collect soil samples in the field. Dane and G. W. WI. Luxmoore. ASA and SSA.C.R. Water retention: Laboratory methods. Handb. 4. Madison.H. R.Mc)] 131 . ASA and SSSA. p. 9. Part 4.3 Dry sample in an oven at 110°C overnight. Part 1. 7. Salinity Laboratory Staff. L. 2. Topp (eds. Calculations H2O % = 100 x [(Ms+w . 2002. 60. 7. Govt.2 Record sample weight (Ms+w). Water Retention (3C) Field-State (3C3) 1. DC. ±0.2 Oven. 3. drying. Physical and mineralogical methods. Physical and mineralogical methods.Ms)/(Ms . 9.) Methods of soil analysis. Agron. 1986. U. and re-weighing a soil sample (3C3). Application Field-water content can be determined by weighing. Monogr.4 Record weight of container (Mc). resulting in an underestimation of the field water content.01-g sensitivity 5. Monogr. metal or plastic containers.S. 110°C 5. Procedure 7. 635-662. 5. 1954. WI. Washington.) Methods of soil analysis. Physical methods. Gravimetric water content is determined (Gardner.11. p. References Bruce.A. tared 6. Print. Water retention: Field methods. In A. Klute (ed. Record oven-dry weight (Ms). The samples are stored in plastic or metal containers to prevent drying and then transported to the laboratory. 2nd ed. A.S. 5. p. USDA Agric. Office.3 Moisture cans.1 Electronic balance. Am.) Methods of soil analysis. Dane. In J. Agron.. 8. Book Series No.J. Reagents None 7. Equipment 5. The resulting data are used to estimate the water content at the time of sampling. Klute (ed. Soil Sci. Interferences Leaks in the plastic or metal storage containers cause the samples to dry. 1986). Water retention and storage: Laboratory. Summary of Method Soil samples are collected in the field.

p. 1978). In A. PHYSICAL AND FABRIC-RELATED ANALYSES (3) Ratios and Estimates Related to Particle-Size Analysis. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. the crystal water content must be subtracted from the total oven-dry water content. In procedure 3D1. Part 1. 1982). and reweighed. 2.where: H2O % = Percent gravimetric water content Ms+w = Weight of solids + H2O + container Ms = Weight of solids + container Mc = Weight of container 9. 493-544.) Methods of soil analysis. This ratio is used to convert soil properties to an oven-dry basis. Gypsiferous soils are a special case because gypsum (CaSO4·2H2O) loses most of its two water molecules at 105°C. This conversion also avoids the possible calculation error of obtaining >100% gypsum when the data are expressed on an oven-dry basis (Nelson. The AD/OD ratio is corrected to a crystal water basis when the gypsum content of the soil is >1%. The inclusion of weight of crystal water in gypsum allows the properties of gypsiferous soils to be compared with those properties of nongypsiferous soils. and Water Retention (3D) Air-Dry/Oven-Dry Ratio (AD/OD) (3D1) Field-Moist/Oven-Dry Ratio (FM/OD)(3D2) Correction for Crystal Water (3D3) 1. Application Soil properties generally are expressed on an oven-dry weight basis. Klute (ed. 9. the AD/OD ratio is converted to a crystal water basis (Nelson et al. W. Report Report water content to the nearest 0. 11. 10. ASA and SSA. The calculation of the air-dry/oven-dry (AD/OD) ratio (procedure 3D1) or field-moist/oven-dry (FM/OD) ratio (procedure 3D2) is used to adjust all results to an oven-dry basis and. 1986. The moisture content is expressed as a ratio of the air-dry to the oven-dry weight (AD/OD) or as a ratio of field-moist to the oven-dry weight (FM/OD). 2nd ed. WI. Bulk Density. Agron.1 percent. Monogr. Soil properties of gypsiferous soils that are reported on an oven-dry weight basis are converted to include the weight of the crystal water. Gypsum content of the soil is determined in procedure 4E2a1a1. to calculate the sample weight that is equivalent to the required oven-dry soil weight. References Gardner. the AD/OD ratio is calculated. dried to a constant weight in an oven. In procedure 3D3. Properties of gypsiferous soils that are reported on an oven-dry weight basis should be converted to include the weight of crystal water in gypsum. Madison. When reporting the water content of gypsiferous soils. if required in a procedure..H. Water content. Physical and mineralogical methods. Summary of Method A sample is weighed. 132 .

with covers 6. Allow the sample to remain in the oven overnight (12 to 16 h). sample contamination. or sample loss may lead to erroneous results. 5. 7.4 Do not allow the sample dish to remain at room temperature for >30 min before reweighing. Soil samples may adsorb significant amounts of moisture from the atmosphere after cooling. The removal of structural water. i. 7. Samples may not reach a constant weight with overnight drying.3. 7.2 Add 10 to 20 g <2mm or fine-grind. 0 to 200°C 5. can produce a positive error. Record each sample number and associated dish number. thermostatically controlled. 7. <30 min after samples have cooled. the most frequently used definition for a dry soil is the soil mass after it has come to a constant weight at a temperature of 100 to 110°C (American Society for Testing and Materials. 110 ± 5°C 5.3 Thermometer. Temperatures that are >50°C may promote oxidation or decomposition of some forms of organic matter.2 Oven.1 Tare the moisture dishes. helps to eliminate this problem. 7.e. ± 1-mg sensitivity 5. 4.2 for AD/OD ratio (procedure 3D1) are as follows: 133 . Gypsum. add enough <2mm or fine-grind. 8.1 – 8.3 Remove the sample dish and allow it to cool before re-weighing. Prompt weighing. No other significant hazard is associated with this procedure. Reagents No reagents are required for this determination.. most commonly in gypsum. Calculations Calculations 8. Weigh the dish plus the sample and record the weight to the nearest 1mg. the crystal water content must be subtracted from the total oven-dry water content. Safety Use heat resistant gloves to remove weighing containers from a hot oven. Follow standard laboratory procedures. When reporting the water content of gypsiferous soils. and amorphous material may be affected.5 Discard the sample. For FM/OD determination. the non-uniform weight of weighing vessels.5-cm diameter x 3-cm height. 4. Many laboratory ovens are not capable of maintaining this prescribed temperature range. moist soil to achieve ≈ 10 to 20 g sample of air-dry soil. air-dry soil to each moisture dish for AD/OD determination. 2004).1 Electronic balance. Do not add moist samples to an oven with drying samples unless the drying samples have been in the oven for at least 12 to 16 h. Interferences Traditionally. Place the sample dish in a drying oven set at 110 ± 5°C.4 Tin dishes.6 Refer to the calculations for the correction for crystal water of gypsum in gypsiferous soils. Procedure 7. 7. During the weighing or drying processes. Record the oven-dry weight to the nearest 1mg. hydrous oxides. Equipment 5.

001942)] where: H2Oc = % Water content.5 (AD/OD)c = (AD/OD)uc /[1 + (Gypsum x 0.2 H2O = [(AD – OD) x 100]/OD where: H2O = % Water content AD = (Air-dry weight) – (Tin tare weight) OD = (Oven-dry weight) – (Tin tare weight) Calculations 8.3 – 8.4 for FM/OD ratio (procedure 3D2) are as follows: 8. uncorrected basis Gypsum = % Gypsum uncorrected (procedure 4E2a1a1) 8.8. corrected basis. uncorrected basis (calculation 8.2) Gypsum= % Gypsum uncorrected (procedure 4E2a1a1) AD/OD Data Use The following equation is used to calculate the weight of air-dry soil needed to provide a given weight of oven-dry soil for other analytical procedures. gypsiferous soils H2Ouc = % Water content.1942)]/ [1 + (Gypsum x 0.1 AD/OD ratio = AD/OD where: AD = (Air-dry weight) – (Tin tare weight) OD = (Oven-dry weight) – (Tin tare weight) 8.2) 134 .5 – 8.001942)] where: AD/ODc = Air-dry/oven-dry ratio.7 AD = (ODr)/[1-(H2O/100)] where: AD = Required weight of air-dry soil ODr = Desired weight of oven-dry soil H2O = Percent water determined from AD/OD (calculation 8.6 for gypsum H2O correction (procedure 3D3) are as follows: 8. gypsiferous soils AD/ODuc = Air-dry/oven-dry ratio.6 H2Oc = [H2Ouc .4 H2O = [(FM – OD) x 100]/OD where: FM = (Field-moist weight) – (Tin tare weight) OD = (Oven-dry weight) – (Tin tare weight) Calculations 8. corrected basis. 8.(Gypsum x 0.3 FM/OD ratio = FD/OD where: FM = (Field-moist weight) – (Tin tare weight) OD = (Oven-dry weight) – (Tin tare weight) 8.

01 unit. and D. The LEP is not the same as LE.Cm)]}1/3 . and W. Standard practice for description and identification of soils (visual-manual procedure). Soil and rock. p. Nelson. 2nd ed. 2004. WI. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Chemical and microbiological properties. Bulk Density. Db/33<2mm = Bulk density at 33-kPa water content on a <2-mm base (g cc-1).. i. In soil taxonomy (Soil Survey Staff. 1968). Page. Miller. R. oven-dry or air-dry. 10. 1999). 1999). Keeney (eds.D. multiplied by the COLE of the layer in question. Calculate COLE when coarse fragments are present as follows: 8. 11.1 COLEws = {1/[Cm x (Db33<2mm/Dbd<2mm) + (1 . 04. Dbd<2mm = Bulk Density. The LE of a soil is defined as the sum of these products for all soil horizons (Soil Survey Staff. ASTM. This shrink-swell potential is important for soil physical qualities (large. Klameth.R.1 where: COLEws = Coefficient of linear extensibility on a whole-soil base. Holmgren. J. COLE may be used to make inferences about shrinkswell capacity and clay mineralogy. and Water Retention (3D) Coefficient of Linear Extensibility (COLE) (3D4) Air-Dry or Oven-Dry to 33-kPa Tension (3D4a) The SSL calculates the COLE for the whole soil by procedure 4D1 (air-dry or oven-dry to 33-kPa suction) by procedure 3D4a.9. 1968. Bulk Density.L. PA. 1968. Ratios and Estimates Related to Particle-Size Analysis. Agron. R. linear extensibility percent (LEP). in centimeters..e.H.08. Vol. The COLE concept does not include irreversible shrinkage such as that occurring in organic and some andic soils. 1982. Nettleton. ASA and SSSA. Grossman et al. Philadelphia. and Water Retention (3D) Coefficient of Linear Extensibility (COLE) (3D4) Coefficient of linear extensibility (COLE) is a derived value that denotes the fractional change in the clod dimension from a moist to a dry state (Franzmeier and Ross. Part 2. Report Report the AD/OD and/or FM/OD ratio as a dimensionless value to the nearest 0. 159-165. 9. L.C. Nelson. Madison. 135 .E. References American Society for Testing and Materials.E.) Methods of soil analysis. 1980). The COLE value is reported in cm cm-1. 1978. Monogr. Construction. Section 4.. Refer to Soil Survey Staff (1999) for additional discussion of LE. In A. COLE can also be expressed as percent. Ratios and Estimates Related to Particle-Size Analysis.. LEP = COLE x 100. Am. R. Soc. deep cracks in dry seasons) as well as for genetic processes and soil classification (Buol et al. on a <2-mm base (g cc-1).. dimension stone. Soil Sci. geosynthesis. Determining soil content and expressing properties of gypsiferous soils. linear extensibility (LE) of a soil layer is the product of the thickness. D 2488. Annual book of ASTM standards. Certain soils with relatively high contents of smectite clay have the capacity to swell significantly when moist and to shrink and crack when dry. Carbonate and gypsum. 42:659-661.

Govt. Soil Sci. the previous equation reduces as follows: COLEws = (Dbd<2mm/Db33<2mm)1/3 – 1 where: COLEws = Coefficient of linear extensibility on a whole-soil base Dbd<2mm = Bulk Density. Proc. and S.. The lower suctions. Franzmeier. Hole.L. 8. 10 or 5-kPa.and 1500-kPa gravimetric water contents are then converted to a whole soil volume basis by multiplying by the bulk density (Db33) and adjusting downward for the volume fraction of rock fragments.B. Soc. Jr.D.J. Office. 1968.2 If no coarse fragments. Proc. Usually the volume of rock fragments is considered a diluent containing no water between the suctions that define WRD.S. B. Print. 2nd ed. Soc. Brasher. and Water Retention (3D) Water Retention Difference (WRD) (3D5) The calculation of the water retention difference (WRD) is considered the initial step in the approximation of the available water capacity (AWC).P. Cm = 1. Ross. Soil genesis and classification. No. Handb. Bulk Density..J. Refer to Soil Survey Staff Division Staff 136 .. Agric. The 10-. DC. Ames IA. 33. on a <2-mm base (g cc-1) Db33<2mm = Bulk Density at 33-kPa water content on a <2-mm base (g cc-1) References Buol. are used for coarse materials.R. The upper limit (lower suction) is selected so that the volume of water retained approximates the volume of water held at field capacity. Am.W.Cm = Coarse fragment (moist) conversion factor. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. Soil swelling: Laboratory measurement and relation to other soil properties. Cm = 1. F. WRD is a calculated value that denotes the volume fraction for water in the whole soil that is retained between 1500-kPa suction and an upper limit of usually 33 or 10-kPa suction. If coarse fragments are present. and R. 436.3 Cm = (100 – Vol>2mm)/100 where: Vol>2mm = Volume percentage of the >2-mm fraction 8. Walker. 32:568-570. 32:573-577. Amer. Ratios and Estimates Related to Particle-Size Analysis. Holmgren. D. and J. oven-dry or air-dry. Linear extensibility as calculated from natural-clod bulk density measurements. Grossman.g.4 If no coarse fragments. Soil Survey Staff. Proc. S. Soil Sci. R. calculate Cm as follows: Cm = Vol<2mm /Volwhole where: Vol<2mm = Volume moist <2-mm fabric (cm3) Volwhole = Volume moist whole soil (cm3) OR (alternatively) 8. D. McCracken. 32:570573. Press. 1999. George G. 2nd ed USDA-NRCS.P. Soc. Washington. 1968. Amer. if present in the soil. WRD does not allow for restriction of roots from the soil layer or osmotic pressure. 1980. 1968. Soil Sci. Nomographic calculation of linear extensibility in soils containing coarse fragments. Franzmeier. Iowa State Univ. e..

= Weight percentage of water retained at 33-kPa suction on a <2-mm soil basis. Ratios and Estimates Related to Particle-Size Analysis.g. but the numbers do not change when other units.(1993) and Grossman et al. 137 . 5 and 10 kPa. Cm = 1. Ratios and Estimates Related to Particle-Size Analysis. = Weight percentage of water retained at 1500-kPa suction on a <2-mm soil basis. = Bulk density at 33-kPa water content on a <2-mm base (g cm-3). If no coarse fragments. This WRD is calculated on a whole-soil base as follows: WRDws = [(W33<2mm . Bulk Density. (1994) for additional discussion on coarse materials and the significance of soil water content at lower suctions. = Density of water (1 g cm-3). and Water Retention (3D) Water Retention Difference (WRD) (3D5) Between 33-kPa and 1500-kPa Tension (3D5a) The SSL calculates the WRD between 33 and 1500-kPa suctions in the whole soil by procedure 3D5a. Bulk Density.Vol>2mm)/100 where: Vol>2mm = Volume percentage of the >2-mm fraction. as well as suggestions for the selection of these lower suctions for the determination of water retention difference (WRD). The WRD is reported as centimeters of water per centimeter of depth of soil (cm cm-1).g. and Water Retention (3D) Water Retention Difference (WRD) (3D5) Between 10-kPa and 1500-kPa Tension (3D5b) The SSL also calculates the WRD between 10-kPa (W10) and 1500-kPa suctions (W1500) by procedure 3D5b. in in-1 or ft ft-1 are needed. dry 1500-kPa (procedure 3c2a1a) is used.. e. The W10 may be used as the upper limit of plant available water for coarse soil materials. calculate Cm as follows: Cm = Vol<2mm/Volwhole where: Vol<2mm = Volume moist <2mm fabric (cm3) Volwhole = Volume moist whole soil (cm3) OR (alternatively) Cm = (100 .W1500<2mm) x (Db33<2mm) x Cm]/ (Pw x 100) where: WRDws W33<2mm W1500<2mm Db33<2mm Pw Cm = Volume fraction (cm3 cm-3) of water retained in the whole soil between 33-kPa and 1500-kPa suction reported in cm cm-1. moist 1500-kPa (procedure 3C2a1b) is the first option in the WRD calculation. The WRD with W33 as the upper limit is reported as cm cm-1.. e. If coarse fragments are present. This WRD value can be calculated by substituting the W10 in place of W33 in the equation for procedure 3D5a. = Coarse fragment material conversion factor. If available. otherwise.

USDA.05-mm particle diameter. Bulk Density. Govt. refer to Soil Survey Staff (1995). fine pebbles (Soil Survey Staff. Bulk Density. Total sand is reported as a weight percentage on a <2-mm basis (3D8). fine sand (FS). Soil Water. Total sand is the sum of the very fine sand (VFS). Soil survey manual. sandy loam and loamy sand.g. e.to 5-mm divisions correspond to the size of opening of the No.0-mm particle diameter. and Water Retention (3D) Water Retention Difference (WRD) (3D5) Between 33-kPa Rewet and 1500-kPa (Air-Dry) Tension (3D5c) The SSL also calculates the WRD between 33-kPa rewet (Wr) and W15 by procedure 3D5c.to 5-mm particle diameter by procedures outlined in 3A2. Print. The rationale for five subclasses of sand and the expansion of the texture classes of sand.to 0. the ratios of 1500-kPa water:clay have been reported as g g-1. Bulk Density.mm Fraction (3D9) The SSL determined coarse fraction with 2.. and very coarse sand fractions VCS). The Wr is used for organic materials. Handb. refer to Soil Survey Staff (1995. respectively.to 5. Workbook. For more detailed information on the application of this ratio. coarse sand (CS). The 2. Ratios and Estimates Related to Particle-Size Analysis. Tech. Total silt is reported as a weight percentage on a <2-mm basis (3D7). Office. Bulk Density. This WRD value can be calculated by substituting the Wr in place of W33 in the equation for 3D5a. NE. Ratios and Estimates Related to Particle-Size Analysis. Lincoln.002. 10 and No. The SSL determines the sand fractions by sieve analysis (3A1a).Ratios and Estimates Related to Particle-Size Analysis. DC. Ratios and Estimates Related to Particle-Size Analysis. U. and Water Retention (3D) Total Sand Fraction (3D8) Total sand is a soil separate with 0.B. This ratio is reported as a dimensionless value. Soil Survey Division Staff. medium sand (MS). For more information on the application of these data. Schoeneberger. USDA-SCS. The SSL determines the fine silt separate by pipet analysis and the coarse silt separate by difference (3A1a). T. used in engineering. Coarse fractions with 2. 1993. and Water Retention (3D) 2. 1994.mm particle-diameter correspond to the rock-fragment division. Soil interpretations for resource soil scientists. No.05. refer to Soil Survey Staff (1995). Sobecki.to 2. Ratios and Estimates Related to Particle-Size Analysis. 138 . 1999). R. References Grossman. Bulk Density. and Water Retention (3D) 1500-kPa Water Content/Total Clay (3D6) Divide the 1500-kPa water retention (procedure 3C2a) by the total clay percentage (procedure 3A1a).S. 18. and Water Retention (3D) Total Silt Fraction (3D7) Total silt is a soil separate with 0. Washington. For more information on these data.to 5. and P. is that the sand separates are the most visible to the naked eye and the most detectable by "feel" by the field soil scientist.76 mm). In the past.. 4 screen (4.

The 75-mm division corresponds to the size of opening in the 3-in screen (76.to 20-mm Fraction (3D10) The SSL determined coarse fraction with 5 to 20-mm particle diameter by procedures outlined in 3A2. i. and Water Retention (3D) 20. The 5.to 20.mm particle-diameter are reported as a weight percentage on a <75-mm basis (3D10). For more information on these data.1 to 75-mm particle diameter by procedures outlined in 3A1a and 3A2. These data are listed for taxonomic placement for particle-size class. U. For more information on these data. respectively.mm particle diameter are reported as a weight percentage on a <75-mm basis (3D11). References Soil Survey Division Staff.1 mm). Coarse fractions with 20. DC 139 . Version No.to 75.S. USDA. 1993). Office.0. Washington. Bulk Density. 1999) for additional discussion on particle-size classes. Soil survey laboratory information manual.76 mm) and the ¾-in screen (19. For more information on coarse fraction with >2-mm particle diameters. Coarse fractions with >2-mm particle diameter are reported as a weight percent on a whole-soil basis (3D13). 18. 1993). 1995. For more information on these data. U. Ratios and Estimates Related to Particle-Size Analysis. Refer to Soil Survey Staff (1995. USDANRCS. to distinguish loamy and silty family particle-size classes.to 20-mm divisions correspond to the size of opening of the No.mm particle-diameter correspond to the rock fragment division.to 5. coarse pebbles (Soil Survey Staff.e.to 75-mm divisions correspond to the size of opening of the ¾-in screen (19. respectively.1 to 75-mm Fraction (3D12) The SSL determines coarse fractions with 0. and Water Retention (3D) >2-mm Fraction (3D13) The SSL determine coarse fractions with >2-mm particle diameter by procedure outlined in 3A2. 1999). Soil Survey Investigations Report No. Coarse frations with 20. 42.1 to 75-mm particle diameter are reported as a weight percentage on a <75-mm basis (3D12). Govt. medium pebbles (Soil Survey Staff. 4 screen (4. 1995. Bulk Density. Ratios and Estimates Related to Particle-Size Analysis. Coarse frations with 2. Print. Print.S. The 20.1 mm) used in engineering.05 mm) and the 3-in screen (76. refer to Soil Survey Staff (1993. Soil Survey Staff. No.mm particle-diameter correspond to the rock fragment division. Ratios and Estimates Related to Particle-Size Analysis. Govt. Soil survey manual. Coarse fractions with 0. Bulk Density.05 mm). Office.mm particle diameter are reported as a weight percentage on a <75-mm basis (3D9). 1. 1993. DC. used in engineering.1993).to 20. For more information on these data. Handb. Coarse frations with 5.to 75-mm Fration (3D11) The SSL determined coarse fraction with 20 to 75-mm particle diameter by procedures outlined in 3A2. used in engineering. Washington. refer to Soil Survey Staff (1995). Coarse fractions with 5.to 75. refer to Soil Survey Staff (1995). Ratios and Estimates Related to Particle-Size Analysis. refer to Soil Survey Staff (1995). and Water Retention (3D) 0. Bulk Density. and Water Retention (3D) 5..

et al. The SSL uses EPO-MIX from Buehler. Washington. 3. automotive coolant/anti-freeze 140 . 305 mm 5. gray.14 Metal probes or dissecting needles 5. 30-µm thickness is estimated by examining the slide under polarized light. A flat surface of the soil sample is glued to a glass slide.3 Diamond saw 5. 5. USDA-NRCS. and technique.8 bars (80 kPa) 5. No. 1987). pressure.3 Ethylene glycol. Bubbles are avoided by using proper temperature. 1970).2 Metallographic polisher with cast-iron laps 5.15 Small forceps 5.16 Art brush 5.e. Industrial Electric Products Division. The thin section is examined with a petrographic microscope (Anon. Micromorphology (3E) Thin Sections (3E1) Preparation (3E1a) 1. The final.1 Scotchcast resin. 1987. rough-textured plate glass. and pale yellow. 6. Agric.5 Hot plate with temperature control or a petrographic slide warmer 5. thin sectioning system. Air bubbles interfere with petrographic examination. heating. weathering intensity.Soil Survey Staff. 1999..6 Polarizing microscope 5. i. Govt. 1986).18 Small chisel. Handb. Cady.S. 0. skeleton grains. 3M Center.13 Squares of thick. ordinary hacksaw.10 Standard petrographic slides 5. a soil clod is impregnated with a polymer resin (Innes and Pluth. 2. white.1 Petro-thin. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. Reagent 6. If the quartz interference colors are of first order. 4.4 Electric oven 5.9 Porcelain crucibles 5. Application Micromorphology is used to identify fabric types. 2nd ed. DC. Lake Bluff. 3M Company. Interferences Impregnation of the soil sample must be complete. Use tongs or heat resistant gloves when handling hot slides or resins. St.7 Vacuum. probe (ice pick). 6. Equipment 5.12 Silicon carbide abrasives 5.17 Razor blade 5. or jeweler's hacksaw 6. and to investigate genesis of soil or pedological features. illuviation of argillans. Summary of Method In this procedure (3E1a). Safety Use adequate ventilation when mixing. Paul. 436.. the sample is ≈ 30 µm (Anon. MN 55101. or the sample will disintegrate during processing. IL 5. U.11 Cover glass 5. Buehler.2 Epoxide. The soil sample is cut and ground to a thickness of ≈ 30 µm.8 Desiccator 5. and applying the resins. Office. Print.

In preparation for the proceeding step. grind one surface smooth on the revolving lap until the surface is highly polished. 7. or pin to ensure proper orientation. Remove specimens from the sample with a small chisel.11 With a slurry of successively finer abrasives. Pack irregular clods in box cells or containers with light weight material to avoid breakage. a probe (ice pick). If the sample surface tends to pull apart or to react with water. 7. and evacuate all the air from the sample. Impregnation 7.and chemical-resistant beaker and place in a glass desiccator. 7. Unless fragility is affected. Add two parts of part A by weight to three parts of part B. the block is ready for sectioning. Weigh parts to an accuracy of 2% before mixing.4 Place clods in small plastic bags to avoid contamination from other samples during transit. staple.3 Select clods from bulk samples if orientation is of no interest. After curing.7 Many good resins are on the market. dry and re-impregnate the small chip or polish it by 141 . Impregnation of the freeze-dried samples may be an improvement over oven-dried samples. Mark the top of clod with a thumb tack. Mix until a uniform color is obtained. add the heated plastic solution.2 Place clods in an upright position in the container.7. Avoid coated clods with Saran or other plastic because coatings interfere with the grinding after the clod is sectioned. 7. matchbox. 7.6 Place the soil sample in a disposable heat. Disposable containers can be cut with the cooled samples during sectioning. Mixing plastic solution 7.5 The whole core or clod can be impregnated. Cutting and Rough Grinding 7. Procedure Sample Collection 7. Sample Preparation 7. raise part A and part B to ≈ 80°C before mixing.1 Collect samples by any procedure that does not disturb the natural structure. 7. but better results are generally obtained with specimens that are 5 cm3 or smaller. Do not mistake boiling solution under evacuated conditions for escaping air bubbles from the sample material. or a jeweler's hacksaw. Experience is required to determine the mixture of abrasive and water that gives the best results for each grade of abrasive. bring the freeze-dried or oven-dried sample to ≈ 80°C. the prevention of moisture loss is usually unnecessary as most samples are usually dried before impregnation. Evacuate the air from the desiccator and dry the sample overnight at 80°C. or a round ice-cream container.10 With a diamond saw blade. The NSSL uses Scotchcast. cut the sample block into 13-mm thick chips that are small enough to fit on a regular petrographic slide. a tin box.9 Cure the impregnated soil overnight in the oven at 110°C. The natural structure of the soil samples is better preserved by the technique of freeze-drying. For best results.8 Open the desiccator which contains the dry samples. an ordinary hacksaw. Release the vacuum and again evacuate the air. Core samplers are commonly used. A satisfactory procedure for some soils is to use a knife or trowel to carve a clod that fits in bulk density box cells.

Without using water. If quartz is present in the sample.18 If a Petro-thin is not available. 190) on the ground-glass plate and commence to drygrind one face of the sample by hand.. Wait a few seconds for the air bubbles to escape. Seating Cover Glass 7. 7. grind the block with an abrasive and lubricate with ethylene glycol. Use successively finer abrasives. 7.22 Aroclor 5460. Place the cover glass obliquely on one end of the section and lower very slowly. i. a thermoplastic chlorinated diphenyl resin (Monsanto). 7. Place pieces of air-dry soil material in xylene and evacuate. Examine the section frequently under a polarizing microscope during the final stages of grinding.e.17 Use the Petro-thin to cut off the excess sample and grind the sample to ≈ 30 µm with the diamond lap.16 Clean the glass of excess cement. Proceed with the standard mounting technique. Alternatively. 7. Move the chip back and forth with moderate pressure to remove entrapped air bubbles and excess epoxide.20 Heat the finished section and the cover slip to ≈ 40°C.14 Firmly attach the chip to the burnished slide with a strong. use it to judge thickness. 142 . Spread a small quantity of epoxide over the surface of the thin section and the cover slip. white. Use a thermoplastic cement or epoxide. Sprinkle a coarse abrasive (American Optical No. Place the chip obliquely on the slide and lower slowly. Mounting 7. transparent bonding agent. Mix the resin and hardener according to the product instructions. Use the finest abrasive to finish grinding on ground-glass plates.19 Care and considerable practice are needed to develop the dexterity required to handle an almost finished section without over-grinding.hand on a glass plate.15 Consult the Petro-thin operation and maintenance instructions for proper operation. trim the mounted sample with a diamond saw blade to a thickness of 50 to 100 µm.030 mm thick. gray. If the sample is ≈ 0. Use successively finer abrasives and continue to grind until the surface is highly polished. A thick film may cause the slide to break when the epoxy is removed. Dry thoroughly. If any air bubbles remain. Begin with the coarse abrasive and lap by hand until the sample is relatively thin. As the section cools. remove the final thin film with a razor blade. Allow entrapped air to rise to the top. Wash the section free of abrasive and dry thoroughly. seems to give better impregnation of dense soils. After the epoxy hardens. An ultrasonic bath is recommended. remove them by pressing lightly on the cover glass with a soft eraser. 7. but before the plastic hardens.13 Burnish petrographic slides to a uniform thickness. cut the sample to the appropriate size. the quartz interference colors are of the first order. 7. Clamp with a spring clamp and cure at ~ 50°C for 1 h. 7. remove excess epoxy with a razor blade. 7. Use either a dry-grinding technique or a more penetrating impregnation procedure. Use a figure "8" or a counterclockwise motion for best results. Final Grinding 7.12 Clean the sample free of all abrasive material.21 Very dense soils and soils with clay fractions that have 30% or more montmorillonite require special handling. and pale yellow. Apply a thin layer of epoxide to the slide and to the chip.

skeleton grains. J. Petrographic microscope techniques. Report Describe the thin section as outlined in procedure 3E1b. R. It is an ideal tool to investigate genesis of soil or pedological features. Wilding.P. Monogr. Stoops. 1 143 . Micromorphology is used to identify types and sequences of active processes occurring in soils via identification of argillans. Hold the sample in the Aroclor at ≈ 200°C for 1 to 2 days. Innes. 11.. An excellent book on examination of mineral weathering in thin sections is Delvigne (1998) and the Soil Science Society of America has a collection of images on a CD that illustrates many features of microfabrics (SSSA. and D. 1986). 8. 1986. Calculations None 9. 2003). Proc. Remove impregnated soil material. Research Soil Scientist. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Agron. (1985). 1993).G. This technique is also termed microfabric analysis and entails descriptive terminology that has been developed over the past 50 years. 1993). 34:483-485. 2nd ed.. 1986. Petrographic sample preparation for micro-structural analysis. 198-204. Research Soil Scientist (retired) and Michael A. and L. Lincoln. NSSC. 10. No. 1965). fabric types.R. Fox et al. Cady.(1993). wrote the procedure for description and interpretation of soil micromorphology as seen in thin sections. 9. In A. References Anon.Wilson. Fitzpatrick (1984. Madison. Murphy (1986). Soil Sci. Soc. W. WI. Vol. Physical and mineralogical methods.) Methods of soil analysis. Thus. ASA and SSSA. The level of resolution increases from field examination to optical microscopic examination and finally to submicroscopic techniques (electron microscopy). 1970. and prepare thin sections by dry-grinding.P. NE. and Stoops (2003). Drees.1. Thin section preparation using an epoxy impregnation for petrographic and electron microprobe analysis.Submerge the xylene-saturated soil material in molten Aroclor 5460. Examination of thin sections with a polarizing light microscope can be considered an extension of field morphological studies. Pluth. Methodological descriptions for producing thin sections can be found in Cady et al. but this sequence of techniques increasingly sacrifices field of view (Cady et al. weathering intensity. Fitzpatrick (1984). allow to cool. Am. NRCS. (1986). Dennis Nettleton. pedon morphological description) and laboratory data (Cady. and Fox and Parent (1993). Part 1. Buehler Digest.. p. Bullock et al. Micromorphology1 (3E) Thin Sections (3E1) Interpretation (3E1b) Application Background: Micromorphology may be defined as the study of soils or regolith samples in their natural undisturbed arrangement using microscopic techniques (Cady. L. 24. 1987. the results of micromorphological studies are most useful when they are combined with other field (landscape description. The science and terminology of microfabric analysis was initially documented by Kubiena (1938) and important publications documenting terminology since have included Brewer (1964). Klute (ed.J.

silt. characterized and sometimes identified. Everything should be viewed in several positions of the stage or during slow rotation with crossed polarized light. whereas the thin sections should be used mainly for information about component arrangement. With the exception of halloysite.Initially. Although grain studies are important in soil genesis studies. If enough plate-shaped particles are oriented together in a body that is large enough to see. concretions. However. Light that vibrates parallel to the c axis travels faster than in other directions. Completely dispersed.15 bar) (Rode. Clay develops in oriented bodies. which can be used as models to analyze and describe clay properties. and other optical and morphological properties are more important. Structures in translucent specimens become more clearly visible if plain light is used. The optical properties. and clay. A wellprepared section is 20. Even though the crystals are monoclinic. Clay in a soil is seldom all random and isotropic. The speed of light that travels in the direction of the c axis and vibrates parallel to the a axis is almost the same as that light that vibrates parallel to the b axis.to 30-µm thick. the refractive indices are very close. With a three-dimensional perspective in mind as well as an awareness of section thickness. in grain studies. Recognition of these components in thin section are easier because interior structures are exposed. A grain that appears needle-shaped may be a needle or the edge of a flat plate. Sand and silt grains in thin sections are identified by standard methods presented in petrography texts. The shapes of mineral grains and structural features are viewed in one plane. and the interference effects in crossed polarized light are small when observed along the c axis. Therefore. the investigator should scan the overall features of a thin section and determine those features that require emphasis. A circular unit is probably part of a sphere. the arrangement of components is destroyed or eliminated by sample preparation procedures that separate the sand. 1969) so that visible pores in thin section are mostly drained at water contents below field capacity. birefringence can be observed. and the c axis is so nearly perpendicular to the other axes. bridges. secondary pseudomorphs. crystal structure. and the condensers are stopped down. Even though the clay particles are submicroscopic. the minerals are pseudohexagonal. Recognition of aggregates. The general analytical approach is the same for grain studies (procedure 7B1) as it is for thin sections. Hence. coatings. and the c axis is almost perpendicular to this plane. the refractive index is used only as a relative indicator. In the United States. Furthermore. Different kinds of illumination should be used with each magnification. the 1:1 and 2:1 lattice clays can be distinguished. emphasis in micromorphology has been on clay arrangement. Grains smaller in thickness are stacked and cannot be viewed as individual grains. either during formation or as a result of pressure or translocation. Strong convergent light with crossed polarizers elucidates structures in dense or weakly birefringent material that may appear opaque or isotropic. the silicate clay minerals in soils are platy. in thin sections. Clay occurs not only in the form of aggregates but also in massive interstitial fillings.g. and general habit of clay are analogous to those of the micas. the refractive index is lower. pores smaller than 20 to 30 µm cannot be seen clearly. An elliptical pore may be an angular slice through a tube. a concern with minerals that occur in small quantities or an attempt to quantify mineralogical analysis is seldom necessary. e. and general groundmass. If the edge of the crystal or aggregate of 144 . repeated viewing of similar features that appear to be cut at different angles is the best way to accustom oneself to a volume rather than a planar interpretation of shape.. and weathered grains is more important in thin section studies than in sand and silt petrography. A pore size of 20-µm diameter equates to a soil moisture tension of 15 kPa (0. The separate particle-size fractions should be used for the identification and mineralogical analyses that are important to a study. they can be described. The a and b crystallographic axes are within the plane of the plate. and the true shapes must be inferred. A thin section is a two-dimensional slice through a three-dimensional body. as the distribution of stems along the a and b axes is so nearly the same. This initial scanning may include all the thin sections from a soil profile or all those related to a particular problem. Similarly. randomly arranged clay of less than 1 µm exhibits no birefringence and appears isotropic in crossed polarized light.

1) have high birefringence and show bright. slickenside faces in a Vertisol or in clayey layers. and its location on present or former pore walls. it shows some birefringence. stress orientation cannot be observed. and often flecked with minute opaque grains. In many residual materials.. it should not show birefringence because of its tubular habit. In the clay-size range. Residual clay has been in place since its formation by weathering. 3). The effect is that of a network in a plaid pattern. a dark band is present wherever the composite c axis and the composite a and b axes are parallel to the vibration planes of the polarizers. silt-size flakes and other small aggregates are common. In transported materials. Amorphous coatings of 145 . Translocated clay may have a different composition than matrix clay. which appear in different positions as the stage is turned. Platy particles also are oriented inside the blocks. Stressoriented clay may be near rigid bodies. Stress can also orient mica flakes and any other small platy grains. Other substances such as goethite. These substances can be identified by their mineralogical properties. have no orientation. This material is dark brown to black. The 2:1 lattice minerals (Fig. more often. This clay is more homogeneous and is usually finer than the matrix clay. quartz grains. however. they have parallel extinction. e. and manifests birefringence and extinction.crystals is viewed along the a-b plane between crossed polarizers. isotropic or faintly birefringent. Although it may have been transported within fragments of weathered material. the orientation pattern is reticulate. these dark bands sweep through the clay aggregate. which is caused by impurities or by refraction of light at the interfaces between particles. kaolinite occurs as book-like and accordion-like aggregates of silt and sand size. carbonate minerals (Fig. Clay rearrangement may result from differentially applied stress that produces shear (Fig. in plain light. In crossed polarized light. often intersecting at regular angles. vermicular or accordion-like kaolin books. vermiculite. and creep can produce stress orientation. the optical effects can be observed. The regular. indicating that these translocated clay bodies are oriented aggregates. continuity. and the orientation process of the clay body. When the stage is rotated. If these bodies are curved.g. In plain light. with or without admixed Fe and Al. indicating deposition in successive increments. are common.g. Even though halloysite can form oriented aggregates. Kaolinite has low birefringence and has refractive indices slightly higher than quartz. There may be numerous sets of these slippage planes. Platy particles become oriented by slippage along a plane. interference colors if the edges of aggregates are viewed. intact arrangement of these materials is usually diagnostic of residual material. mass movement. and interference colors are manifested in other positions. Halloysite may show very faint. distinctions among smectite. especially in spodic horizons. or along root channels. slump. If a clay concentration is organized so that most of the plates are parallel. interference colors for kaolinite are gray to pale yellow. If these bodies are straight. and chlorite in thin section are seldom possible. This clay may be random. consisting of bright lines showing aggregate birefringence. especially if its origin is another horizon. The degree and quality of optical effects depend on the purity. Otherwise. Location features that distinguish translocated clay from residual clay are its occurrence in separate bodies. Translocated clay displays lamination. Stressoriented clay is often strongly developed on ped faces. channel linings. intermediateorder. e. clay is arranged either in forms that are pseudomorphs of rock minerals or in definite bodies of crystal aggregates.g.. and gypsum may form pore linings and ped coatings. In many soils. stress orientation can be inferred. mica. it remains in place relative to the fabric of these fragments. Amorphous coatings of organic matter. gibbsite. If the faces on structural units are smooth and do not have separate coatings. Root pressure. usually with distinct boundaries. or ped faces. e. 2). In residual soils that are derived from coarse-grained igneous rocks. these clay minerals are stained and mixed with iron oxide and organic matter. clay in the thin section may be homogeneous and featureless. These clay minerals are usually mixed in the soil and seldom occur pure.. In the average thin section. patternless birefringence. and thus be isotropic. two straight extinction positions are viewed.

S. Peds are the basic units in soils that contain organized structural units and are composed of skeletal grains. 1985..g. shape. the larger units support one another. and Stoops. granulation. The system may be used to describe the distribution of primary particles.S. size.. The coarser particles may be silt. There are no restrictions on material type. or orientation (Brewer. Bullock et al. 1983). Related Distribution Patterns: The five "coarse-fine related distribution patterns" of Stoops and Jongerius (1975) are in common usage. sand. Eswaran (1983) characterized the <25-µm2 size domains of monomineralic soils using a scanning electron microscope (SEM). The nomenclature of these distribution patterns. Micromorphological descriptions often contain terminology from different sources to describe properties of the fabric. having no definite boundary. and drained pore to filled pore (DP/FP) ratios of some related distribution patterns of a number of U.. e. are not oriented relative to each other. In general. and the interstitial spaces are partially filled with finer material. and pedological features. linear extensibilities (LE). 1964 and 1976. lithic fragments (coarse monic) or clays (fine monic). pebbles.g. silt. The monic type (granic type of Brewer et al. the coarser units are linked by bridges of finer material but are not surrounded by this material.. In the enaulic type. humic micro-aggregates. 1975. the SSL increasingly uses them in Soil Survey Investigations Reports (SSIR's) and in soil project correspondence. The class may be divided into types based on the spacing of the coarser units. the descriptive terms for the s-matrix are those as defined by Brewer (1976). soils. Figure 5 shows some plasma fabrics and their clay.organic matter occur as the bridging and coating material in B horizons of sandy Spodosols and as thin coatings or stains on pore and ped faces in other soils. or sand. Figure 4 shows the average textures. However. In the end member of the sequence. In the chitonic type (chlamydic type of Brewer et al. whereas the finer material may be clay. These features are smaller than some domains described by Brewer (1976). e. The domains in allophanic soils are composed of globular aggregates. The enaulic fabric consists of material finer than is found in either the gefuric or chitonic type but is not so fine as is found in the porphyric type. the large fabric units occur in a dense groundmass of smaller units. and s-matrices. 2003). 1983. In the gefuric type.. absolute size. the porphyric type. The halloysitic soils differ in that the halloysite tubes 146 .. the coarser units are surrounded by coatings of finer material. The soil plasma includes all the colloidal size material as well as relatively soluble material not bound in skeleton grains. as well as compound units. and linear extensibility averages of a number of U. are intended to be broadly defined. the asepic and sepic types. i. Plasma concentrated or crystallized into pedological features is not included in the description of plasmic fabrics.. these small features provide the detail expected of the interparticle relationships present in the larger separations. orientation. 2. as described by Stoops and Jongerius (1975). 1976). and there is an absence of interstitial pores. Sepic fabrics are those with anisotropic domains with various orientation patterns visible under cross-polarized light. Skeleton grains of a soil material are individual grains larger than colloidal size. especially extinction phenomena. quartz grains. As these terms have become more widely adopted in the literature. Plasma Fabrics: Brewer (1976) divided soil materials into three groups for descriptive purposes: peds. 1983) consists of fabric units of only one size group. e.. Brewer et al. The smatrix plasma fabrics are divided into two groups. or gravel. or origin. Procedure Description of Microfabrics Terms have been defined for distribution patterns of the components of soil thin sections (Brewer. pedological features. soils. sand. The s-matrix is the material within which pedological features occur.e. silt + clay.g.. Stoops and Jongerius. the plasma separations. The description of plasmic fabrics is based on the interpretations of optical properties under crossed-polarized light. plasma. Asepic fabrics are those with anisotropic plasma in which the domains. 1983). This type is equivalent to the earlier porphyroskelic class of Brewer (1964) or to the current porphyric class (Brewer et al.

Silasepic fabrics have a wider range of particle sizes than argillasepic types. in which case. In kaolinitic soils. silica. 9). Skeleton grains that adhere to the cutanic surface are called skeletans.g. Overall. and definitions of its respective types (Brewer. The fabric is skelsepic when the plasma separations occur at the skeleton grain-matrix contact (Fig. 8). halite. quartzans. The domains in micaceous soils retain the face-to-face packing that is common in micas and may retain some of the book-like forms as well. or gibbsans. Lattisepic fabrics are similar to masepic fabrics except that the acicular and prolate domains occur in lattice-like patterns. Brewer (1964) recognizes seven kinds. most of which are widely adopted. Sesquans that are specific for goethite. a careful observer may view silt-size domains or plasma bodies that give the matrix an overall flecked extinction pattern (Fig. or voids. 1964) are three dimensional pedological units (e. Argillasepic fabrics are dominated by anisotropic clay minerals and have a random orientation pattern of clay-size domains. 1964) have been widely adopted by soil scientists. e. ferri-argillans have iron oxides as a significant part of their composition. composition. and chalcedony are called gypsans. carbonate. The remaining three sepic plasmic fabrics are most common in fine-textured soils. respectively. or gibbsite are called goethans.g. usually of soluble materials. quartz. Undulic plasmic fabrics have practically isotropic extinction patterns at low magnification. the domains. hematans.. silans. Argillans are composed dominantly of clay minerals. plasma separations. Cutan is defined by Brewer as a modification of the texture. unless iron hydrous oxide has disrupted the platelets. all of the plasma has a complex striated orientation pattern... The domains in montmorillonitic soils are bent to conform to the shape of skeletan grains. or fabric at natural surfaces in soil materials due to the concentration of particular soil constituents or as in-place modification of the plasma (Fig. However. the plasma separations occur as elongated zones within the s-matrix and apparently are not associated with void walls or skeleton grains (Fig. the packing is essentially face-to-face and. Cutan locations are surfaces of grains. Three other kinds of plasmic fabrics are characteristic of particular minerals or kinds of soils. The mineralogical nature of cutans is characterized. and the domains are indistinct even at high magnification. ferri-argillans. peds. Generally. Isotic plasmic fabrics have isotropic plasma.) They are usually prolate to equant. striated plasma domains within a flecked plasma matrix (Fig. Pedological Features. argillans. and organo-argillans have significant color addition by inclusion of organic matter. calcans. channels. Mosepic fabrics consist of plasma domains with striated orientation that may adjoin each other or be separated by small plasma areas with flecked orientation that are not oriented relative to each other (Fig. Asepic plasmic fabrics are subdivided into two groups. asepic fabrics have flecked extension patterns. respectively. 7). and chalcedans. and internal fabric. even at highest magnifications with high light intensity. (The name is derived from the Latin term glaebula. Glaebules: Glaebules (Brewer. meaning a small lump or aggregate of earth.generally may be seen as protrusions from globular forms. In masepic fabrics. The crystic plasmic fabrics have anisotropic plasma with recognizable crystals. 10). i. Sesquan is a general term used for a cutan of sesquioxides or hydroxides. upon drying. cutans of gypsum. hematite. Fe oxide or carbonate nodules) within the s-matrix whose morphology is incompatible with the composition of the present matrix material. 11). halans. have striated extinction patterns. In omnisepic fabrics.e. Internally. 6). Cutans: The term. The sepic plasmic fabrics have recognizable domains with various patterns of orientation. the platelets may still be packed face-to-face in subparallel stacks. The fabric is vosepic when the plasma separations with striated orientation are associated with channel or pore (void) walls. the cutans are subdivided on the basis of their location. calcitans. argillasepic and silasepic types. Similarly. structure. Pedological Features. However. Insepic fabrics consist of isolated. A glaebule is recognized as a unit either because of a greater concentration of a 147 . calcite. or organo-argillans. cutan. the fabric is very dense and compact. The striations have parallel orientations to zone length. the domains frequently are present as booklets that are packed face-to-face.

In soils that are slightly more developed than those with gefuric patterns. 17) . 14) (relatively large spaces that are not formed by packing of skeleton grains. Pedodes are pedological features with hollow interiors. sharp external boundaries. Monic fabrics also can form by fracturing and flaking of organic coatings in the upper B horizons of the Spodosols (Flach. (6) joint planes (plane-shaped. 13) (empty spaces between peds or other compound individuals). and organic matter (Chadwick and Nettleton. (4) vesicles (Fig.g. or because of the presence of distinct boundaries of a constituent within the enclosing s-matrix. and the amorphous silica in some kinds of duripans. and include soil fabrics formed in sand dunes. Those voids with diameters of 20 µm to > 2 mm can be studied and measured in thin section. concretions. with the units being aggregates) to matrigranodic (enaulic) to porphyric. Voids: Voids are the empty spaces within the s-fabric. nodules. 1960) and by freezing and thawing (Brewer and Pawluk. iron. In sandy soils. Papules are pedogenic features composed of clay minerals with continuous and/or laminar fabric. 12) are pedological features with undifferentiated internal fabric. Nodules (Fig.. e. and (9) channels (mostly cylindrical-shaped. modifiers commonly are added when fabric descriptions are complete enough to understand the means of formation. The average properties of some related distributions we have described are given in Figure 4. and pedodes. empty spaces that are larger than packing voids).S. 16). the basic descriptive terms for soil fabrics do not imply any specific genesis of the feature. These are common in argillic and spodic horizons and in duripans. 1990). chitonic related distribution patterns form. and commonly prolate to equant. 3). i. aluminum. Concretions are pedological features with concentrically laminated structures about a center. 15) (relatively large empty spaces with smooth. The enaulic related distribution patterns are more common in soil material in which the cement bonds to itself more strongly than to skeleton grains. (5) chambers (empty spaces with smooth. the cement or plasma is material that adheres to skeleton grains. Gefuric patterns are common in weakly developed argillic and spodic horizons and in duripans. However. whereas an illuviation cutan is formed by movement of material in solution or suspension and later deposited (Brewer. ionic-bonded calcite and gypsum tend to bond to themselves more strongly than to skeleton grains (Fig. Usually.e. empty spaces that traverse the s-matrix in a highly irregular pattern of short flat or curved planes). sandy sediments deposited by streams and rivers. Pedological Features. (8) craze planes (plane-shaped. iron. Jim (1986) showed that with an increase in the activity and proportion of the clay fraction. or in-place plasma modification. Brewer (1976) classifies these voids as follows: (1) simple packing voids (empty spaces due to random packing of single skeleton grains). Interpretations Related Distribution Patterns: Usually. the related distribution patterns alter from dominantly matrigranic (monic. regular outlines). Similarly our data for some U. (2) compound packing voids (Fig. the organic matter. (3) vughs (Fig. often lined with crystals. stress cutan. Several kinds of finer material (plasma) can bridge the coarser particles (skeleton grains) to form gefuric related distribution patterns. In an experimental study of soil microfabrics by anisotropic stresses of confined swelling and shrinking. Glaebules include papules.constituent. shearing. empty spaces that traverse the s-matrix in a regular pattern). empty spaces that traverse the s-matrix in an irregular pattern). is the result of differential forces. and aluminum complexes in some kinds of spodic horizons. soils show that the relative pore volumes at 30 kPa for some soil coarse-fine distributions increase from enaulic through open porphyric (Fig. Silicate clays can bridge skeleton grains in some argillic horizons. somewhat rounded shapes.. beach deposits. Fauna can produce monic fabrics that are mostly fecal pellets. or difference from the s-matrix fabric. These cements have covalent bonds and commonly include silica (Fig. Some monic fabrics are inherited. 148 . regular outlines that connect to other voids). and gruss. (7) skew planes (plane-shaped. 1964). 1975). Bridges as well as complete coatings of skeleton grains are present.

. especially in argillic and petrocalcic horizons. or 149 . There are at least two types of origins for orientation of plasma on sands. One is a result of clay illuviation. the plasma islands or papules are pseudomorphs of some weatherable mineral.. whereas in other insepic fabrics. In an experimental study of soil microfabrics by anisotropic stresses of confined swelling and shrinking. lattisepic. sandstone. a progression from insepic to mosepic to masepic plasmic fabrics. Organic matter or iron stains. the plasmic fabric sequence is insepic. In porphyric related patterns. 1983). usually <30 percent but may have as much as 70 percent (Brewer et al. In soils that form in the same climate. 1983). omnisepic. Holzhey et al. organics. the silt to clay ratio is used to identify the kind of sequences by which the porphyric pattern forms (Brewer et al. LE also remains low. Even though root growth is adequate to increase the percentage of oriented clay near the root-soil interface (Blevins et al. In some insepic plasmic fabrics. and are also associated with some sedimentary deposits (Brewer et al.thereby producing open porphyric related distribution patterns (Chadwick and Nettleton. Even if there is high clay content. Argillasepic fabrics are important fabrics in many fine-textured B horizons. Plasmic Fabrics: The asepic plasmic fabrics differ in composition mainly in silt to clay ratios. Silasepic plasmic fabrics have low clay contents and have more silt than clay. the horizons with asepic plasmic fabrics have low effective linear extensibilities (LE) either because the clays are low-swelling types or because the soils do not dry enough to undergo the full range of laboratory-measured LE. Mosepic plasmic fabrics commonly have more clay than insepic fabrics do because they contain more islands of plasma. and ortstein. 1990). Porphyric related patterns form from the normal packing of grains in materials with a high proportion of fine material. The porphyric patterns are common in loessial soils... 1970). The silasepic fabrics are common in porphyric related distribution patterns in A and B horizons of Solonetz. mosepic. Solodized Solonetz and Solodic Soils. and the interstices tend to be filled with minimal formation of coatings. 1974). the papules are clay skin fragments or are eolian sand-size clay aggregates (Butler. there may or may not be skeleton grains of primary minerals. 1983). the kind of sepic plasmic fabrics form a sequence relative to increasing linear extensibility (Nettleton et al. the pseudomorphs do not disperse well in particle-size distribution analysis (PSDA). resulting in a flecked distribution pattern mask the birefringence of the plasma. Using X-ray diffraction (Clark. vosepic fabrics are present in soil horizons in which the main fabric type is masepic or skelsepic. By definition. Jim (1986) shows that with an increase in the activity and content of the clay fraction. In precursors of the porphyric related distribution patterns. there is an increase in the long and narrow plasma separations. Red Podzolic Soils. 1976). In some samples. These patterns can be the end member of several kinds of sequences (Brewer et al. In increasing order of shrink-swell stress. 1974). lithic fragments of shale. observations of deformation experiments indicate that the degree of clay orientation increases with an increase in applied stress. The related distribution patterns associated with this fabric commonly are monic. However.. Shrink-swell forces have not been sufficient or have not operated long enough to have homogenized the islands of plasma into the soil matrix. the material consists of silt and clay. i. 1983). 1969. and masepic. Argillasepic fabrics have the higher clay contents. this type would not be included with skelsepic fabric.e.. gefuric.. organic material forms pellets in void spaces between skeleton grains in some spodic horizons. 1983). Insepic plasmic fabrics are very common in finer-grained porphyric B horizons of a wide range of soil groups (Brewer et al. The vosepic plasmic fabric rarely occurs as the only fabric in a soil horizon. 1970) and scanning electron microscopy (Edil and Krizek. Soloths. or other rocks. in mosepic plasmic fabrics. Soil horizons with insepic fabrics generally have a LE of <4 percent. Silasepic plasma fabrics are common in A and B horizons of loessial soils in association other kinds of plasma separations. Even though organic matter has covalent bonds and usually surrounds grains. duripans. pedorelicts. In the porphyric related patterns. root growth does not appear adequate to form vosepic or other highly stressed plasmic fabrics. Vosepic plasmic fabrics occur in soil horizons that have undergone stress either due to shrink-swell forces or to tillage.. Lateritic Podzolic Soils. Usually..

The determination of whether or not a papule is an illuvial feature is important for classification purposes. soils in aridic. illuvial origin of the feature is relatively certain (Nettleton et al. In some humid environments. As soils in humid environments do not dry to the same degree as those in the desert. as well as pedodes. argillans and papules may be present even where the LE is >4 percent. by illuviation. papules and clay skins rarely are found. lattisepic. increased unconfined compressive strength. Unlike soil pedorelicts or rock fabrics (lithorelicts).. there is restricted soil permeability. xeric. Arcuate forms and laminar internal fabrics are evidence that the feature is illuvial.. the argillans and papules are as much as 30 percent of the soil material (Brewer et al. A study of soil voids may be useful in predicting the clay activity and shrink-swell behavior of soils. as well as of parent material. lattisepic. 1990) or by the introduction of eolian sands and silts that are composed of clays (Butler.. especially basalt. 1976). 1983).. in texture-contrast soils (soils with argillic horizons) is usually <5 percent of the soil volume (Brewer et al. Clays in these horizons do not disperse well in PSDA. These are the true skelsepic fabrics. Shrink-swell forces have been involved in their formation as shown by relatively few papules or clay skins remaining. and kaolinite and halloysite are the important clay minerals. The comparison of size and shape of papules and minerals. its internal fabric. the isolation of clay skins by the channel and void migration within the soil matrix (Nettleton et al. In some sandy soils that are low in silt. nodules. In an experimental study of soil microfabrics by anisotropic stresses of confined swelling and shrinking. Jim (1986) shows that with an increase in the activity and 150 . depending on the degree of cementation. The measured illuviated clay rarely accounts for the difference in clay content between the A and B horizons. Some of the clay may originate from weathering in place and some from a destruction of argillans and papules.e. The origin of the papule as eolian may be determined by studying its size and shape. Crystic plasmic fabrics are common in B horizons of soils formed in dryland areas. but the threshold amount is dependent on clay mineral type and on degree of dryness common to the environment. If argillans and papules are present in argillic horizons in dryland soils. The other origin is commonly the porphyric related distribution patterns with LE's that are >4 percent for dryland soils. Microlaminae may suggest an origin as sediment. Cutans and Pedogenic features: Most argillans (Fig. the clay skins may survive because only part of the linear extensibility is effective. 1968. the soil LE is usually <4 percent (Nettleton et al. but these plasma separations also are stained deeply by iron. 1969). Some papules and clay skins commonly are present. If the feature partially surrounds an oval body of silt. 1968). and limited particle dispersion. but high 1500-kPa (15 bar) water contents suggest that the horizons belong in clayey families. In soil horizons with large areas of interlocking crystals.. The content of strongly oriented clay (usually argillans plus papules). Masepic. but areas of skelsepic and vosepic areas commonly are present. or ustic soil moisture regimes.enaulic. Papules may originate by the weathering of primary minerals. 1983).. 1976). Isotic plasmic fabrics are common in spodic horizons and in Andisols. and omnisepic plasmic fabrics.. may help to determine if the papules are pseudomorphs of one of the primary minerals. 1983). Internal fabric resemblances and residual parts of the primary mineral within the papules help to determine if a papule is a pseudomorph. Undulic plasmic fabrics seem to be associated with basic parent materials. or glaebules rich in soluble plasma. 1974. at least in part. Clay contents are usually >35 percent. and with moderate to strong weathering (Brewer et al. and the number and degree of its alterations relative to other particles. i. probably form by accretion (Brewer. The water-holding capacities of these soil horizons are relatively high. Nettleton et al. Some unweathered volcanic ash may be present.. are accretionary and usually form in place. In masepic. The clays in these horizons are amorphous and disperse poorly in PSDA. and there are vosepic areas. The fabric commonly is stained deeply by iron minerals. Most concretions. 11) are formed. and omnisepic plasmic fabrics are evidence of stress >4 percent in dryland soils. Brewer and Blackmore.

NY. Inc. The failure of most vesicles to connect to other voids and the low strength of the crust in which vesicles occur help to explain the low infiltration rates and the high sediment yields that commonly are found on these soils. or by other unknown causes. Soil physics. Skau. 1964. Furthermore. 1974. John Wiley & Sons. and L.. The very regular outline of vesicles is of interest (Nettleton and Peterson. 271). plant root systems. J. and no constant void size distribution exists (Brewer.. Once formed. even if reduced to a 20-µm thickness. 1983). Am. Blackburn and Skau (1974) and Rostagno (1989) conclude that the infiltration rates are the lowest and the sediment yields are the highest on sites that have vesicular surface horizons. 1976). Robert E. or by certain geological processes (Brewer and Sleeman. 18) are produced in relatively uniform fine-textured soils by a relatively regular system of cracking upon drying (Brewer. In thin section studies of voids in sands and sandy soils. 1964. the void shapes change from compound packing voids to planar voids and vughs.. The unaccommodated peds of the compound packing voids may be formed by faunal excreta. R. 1971). pores are distributed at random. 151 . Because of their size. Craze planes often occur in Chernozems (Mollisols). Holowaychuk.. NY. Vughs usually occur in soil materials with a wide range in size of particles. possibly as a result of the high humic acid content (Brewer. and kind of branching pattern.. aggregates become flattened at contacts. 1976). 11).. shrink-swell action. 1976).L. and arrangement of skeleton grains determine the nature of simple packing voids. Soil Sci. Laboratory studies verify this phenomenon (Springer. Brewer. Brewer. and others form by faunal activity or the normal packing of plasma and skeleton grains. cross-sectional shape. pore size distribution is undefined. there are several invalidated assumptions that commonly are made in relating porosity to permeability (Nielsen et al. Blackburn. especially the >30µm. but the origin of compound packing voids is not so straightforward. Micromorphology of soil fabric at tree root-soil interface. NY. NY. there is a drastic decrease in void volume. A possible objective of micromorphological studies may be the measurement of porosity and the prediction not only of soil water content at various suctions but also of hydraulic conductivity.D. including silicate clays. if these pores pass through the section at an angle of <45°. resulting in more angular and eventually fused compound units. Huntington. with suppl. 1958). 1956.content of the clay fraction. Proc.M. 1956 p. If high silt soils are allowed to dry before each irrigation. The assumptions that especially relate to soil fabric are that no pores are sealed off. 34:460-465Brewer. Soc. and C. Fabric and mineral analysis of soils.P. References Baver. John Wiley & Sons Inc. Cringer Publ.. John Wiley & Sons Inc. 27:476-480. may make the examination of the <20-µm diameter pores impossible. in those soils whose volumes change with changes in water content. Fabric and mineral analysis of soils. 3. 1970. W. 1976). However. R. Fabric and mineral analysis of soils. As a result of studies of infiltration rates and sediment production in rangeland in central and eastern Nevada. Co. The size. material. With an increase in stress from shrink-swell forces. the vesicle size increases with the number of irrigations (Miller. Joint planes (Fig. L. N. the vesicles that are near the surface are the result of air entrapment by rainfall following dry dusty periods. 3rd ed.. there is a close correlation between microscopic and suction methods (Swanson and Peterson. Furthermore. Range Manage. Reprint of 1964 ed. This means that many voids that are involved in unsaturated water flow in soils will not be visible in thin section (Baver. 1972 p. 1976. R. Skew planes are produced in more heterogeneous materials or by irregular drying (Brewer. Lapham (1932) states that in Sierozems (Aridisols). 1963). Some vughs form by the weathering and removal of carbonate. shape. and pores are generally uniform in size. channels probably form by faunal activity. A more serious difficulty may be that a thin section. man's activities. R.H. these joint planes tend to open in the same place during successive drying cycles. Blevins. Wilding. Infiltration rates and sediment production of selected plant communities in Nevada. 1942).

Sols bruns acides in the northeastern United States. Part 1. Ontario. 269:250-266.E. M. of Canada. V.. 1965. FitzPatrick. 1990. Micropedology. S. and W. optically oriented clay. 9:185-218. The fabric of Australian soils.F. p. Geoderma. NY. R. NY. 473-485. cementation and aggregate stability. E.) Soil sampling and methods of Analysis. Chadwick. Stoops. W. New York. 55:301-319. J. Ltd. K. In A. Fedoroff.. Yeck.L. xeric.H. Fox. Geomorph. Cornell. Sleeman. Am. Pedology 33:41-54. Working-meeting on Soil Micromorphology. 1974. 439476. Parent. 1986. Jongerius. 1938. Physical and mineralogical properties. and A.) Methods of soil analysis. Soil Sci.R. 1976. Physical and mineralogical properties. p.A. Brewer.D.Y.E. Atlas of micromorphology of mineral alteration and weathering. 1974.. Wilding. Ph. C. Assoc. and F. P.R. 1963. N. Sweeney. In L. Soil micromorphology: a basic and applied science. Germany. for soil thin section description. Pedotubules: their definition.. Bd. Part 1. Ames. J. J. 14:237248. 1998. Soil microscopy and micromorphology. and J.K. White.E. p. Collegiate Press. and R.R. Carter (ed. Nettleton. and relationships to associated soils.D. Foster. Fox. p. Soil Sci. Agron. Black. 152 . Relationships between subplasticity rating. Sci. J.R. Chapman and Hall. Experimental study of soil microfabrics induced by anistropic stresses of confined swelling and shrinking.A.E.D. Drees. Micromorphology methodology for organic soils. T. and S.B. Limestone Press. Lapham.J. J. Bullock. 1985. Morphology and micromorphology. Dickson. J. and torric soil environments of the United States. p. and A. Berlin. Guertin. Elsevier Sci. classification and interpretation.. Micromorphology of soils. Sleeman. of 4th Int. and R. J. Pawlak. J. CSIRO: Melbourne/Academic Press. 1976.) Developments in Soil Sci.) Soils: an Australian viewpoint. Assoc. 2nd ed. Canadian Miner Special Pub. London. Mermut.. Waine Res. T. FitzPatrick. Proc.A. 1st ed. E.Brewer. Jim. 1984. W. 9:604-631. CSIRO (ed. Genesis and morphology of desert soils. 1993. and A. 1983. England. Krizek. Ensminger.A.) Methods of soil analysis. Flach. 19. 3.P.) Soil Microscopy. Kingston.. Clark (eds.C. Nettleton. 683-709.. Soil Surv. 1975. Soil Res. Clark. Brewer. 1932. A contribution towards the better specification of parna and some other aeolian clays in Australia. N. R.L. Micromorphologic evidence of adhesive and cohesive forces in soil cementation. and L. Publ. Influence of fabric and soil suction on the mechanical behavior of a kaolinitic clay.A.D.) Soil sampling and methods of Analysis. 13:34-52. and L.. London. Delvigne. J. morphology. R. C. Microfabric of some argillic horizons in udic. O.. 747-760. Boca Raton.G. In M. Cady. Thesis. Cady. In C. Micromorphology methodology for inorganic soils. Evans. Klute (ed. Investigations of some soils developed in hummocks of the Canadian sub-artic and southern-arctic regions. R. 15:323-341. D. Suppl. Protz. Bull. 37:91-112.R. Publ. 15:66-78.. I. Butler.K. H.. Holzhey. 1986. Carter (ed. Lewis Publishers.E.W.A. Petrograhic microscope techniques. Ontario. IA.G. R. L. Rutherford (ed. In Division of soils. Edil. including statistics of measurement and sampling. 1993. In M. Brewer. B. 20:106-116. E. and others.R. Agron. Miner. Z.S.. Am. Eswaran. R.R. Douglas (ed. Blackmore. Lewis Publishers. Handb. Walverhampton. Petrographic microscope techniques. 1960.A. C. John Wiley and Sons. B. G. In G. Genesis..D.. Geoderma. 1993. Mechanical formation of preferred orientation in clays. Unpubl. Aust. 1983. C. Canada. Can. L.. Tursina. Characterization of domains with the scanning electron microscope. 207-212. 1970. Boca Raton. Kubiena. and R.

and fragipan genesis.. Argillic horizons without clay skins.B. Soc. Soil Sci.J. 38. 1942. Jerusalem.L. A. Aridisols.D. C.) Proc.. Argentina. Infiltration and sediment production as affected by soil surface conditions in a shrubland of Patagonia. p. Soil Science Society of America.D.. 1972. In L. of 4th Int. 1986. Geoderma. A reference collection for soil micromorphology.. C. Hall (eds. Soc. Agron. 1. WI. 1968. McCracken.E. 53:173-183. N. Kimble and W. Academic Publishers. 42:383-385. W.. Nettleton (eds. R. Stoops. Soil Sci. Two North Carolina Coastal Plain catenas. Brasher. Soc. J. Nielsen. 1969. Characterization.. Micromorphology. Cary. Brasher. II. 33:121-125.. Soil Sci. Daniels. Am. Proc. Soil Sci. Swanson. W.E. Soil water. Elsevier. J. Smeck. composition. 1983. Grossman. Rode. Pedogenesis and soil taxonomy. Am.D. Soil Sci.D. and D. J.W. for Scientific Translations. Nettleton.D.R. Great Britain. In J.M. Thin section preparation of soils and sediments. New Mexico.Miller. Moisture properties of soils and movement of soil moisture. WI. 1969. 13:189-200. and B.M.W. Jongerius. CD Rom.D. Am.W. Springer. Vol. and A. Flach.) Israel Prog.F. Concept of argillic horizons in Aridisols-taxonomic implications. 1971. The soil orders. G. Soil Correlation Meeting (ISCOM).. and G.R. Nevada. Nettleton. Desert pavement and vesicular layer of some soils of the desert of the Lahontan Basin.A. W. Proposal for micromorphological classification in soil materials. Part A: Papers. Proc. Jackson. Wilding. D. R. p. K. W. R. 165-215. 22:63-66. NY.B. Am. Am. 1989. 35:635637. Nettleton. Formation of vesicular structure in soil. and California. Soc. classification. p. and B. Evans (eds). 1993. Arizona. Theory of soil moisture. Nettleton.R.). (In English. and J. Peterson. 1987.P. October 3-17. Madison. A classification of the related distribution of coarse and fine particles. translated from Russian. 167-176.P. 153 . I. Peterson. Murphy. II. 32:582-587.E. 1975. C. Range Manage. and R. The use of micrometric and other methods for the evaluation of soil structure. 1990. 1958. D. M. Proc. Rostagno.F. and F. ASA and SSSA.B. Madison. Soc.D. and utilization of Aridisols in Texas.

Pedon 40A001. Fremont Co.Figure 1. making the plasma anisotropic (visible under crossed polarized light. (Series name not designated. (White House pedon. Pedon 98P0456. Figure 2.. Horizons with high percentage of clay of expandable aluminosilicate claysized minerals become aligned through shrink-swell processes. Cochise Co. Note the high birefringence due to the orientation of the grain in thin section..0 mm. Bt2 horizon under crossed polarized light). 154 . This process results in a loss of argillans along ped faces in many soils. AZ. This alignment results in preferred orientation of clay particles. Frame width = 0. BCtk horizon under crossed polarized light). Frame width = 1.9 mm. WY. Large biotite grain undergoing expansion from weathering.

( Cax pedon.g.5mm. 155 . Pedon 97P0420. 1976). Figure 4. CA. Their formation illustrates attraction to and deposition of carbonates on mineral surfaces (e... Frame width of each idealized kind of fabric is 0.9 mm. These carbonate coatings are referred to as calcitans (Brewer. Kinds of related distribution patterns and a listing of their physical properties. Calcium carbonate around skeletal (sand-sized) grains in a coarse-textured matrix. Co. quartz or feldspar grains) accessible to percolating water. The lower size limit of coarse material in the C/Fpatterns was set at about 50 µm for most of the slides. San Bernardino.Figure 3. Frame width = 0. Bkg2 horizon under crossed polarized light).

Figure 6.3 mm. Silasepic plasma fabric. 156 . Kinds of plasma fabrics and a listing of their physical properties. (Southridge pedon. IA.Figure 5. Allamakee Co.. 87P0075 Ap horizon under crossed polarized light).5 mm. Frame width = 1. Frame width of each idealized kind of fabric is 0.

Macon Co. MO. 87P0771.Figure 7. Macon Co. BE horizon under crossed polarized light). Frame width = 1. (Mexico pedon. Mosepic plasma fabric. 157 . (Leonard pedon.3 mm. Frame width = 1. 2Btg3 horizon under crossed polarized light)..3 mm. Insepic plasma fabric. 87P0770.. Figure 8. MO.

. 40A2847. San Diego Co. Frame width = 1. Masepic plasma fabric. Bt horizon under crossed polarized light).3 mm. Skelsepic plasma fabric. Bt horizon under crossed polarized light). CA. (Gloria pedon.Figure 9. Monterey Co. (Redding pedon. CA. Figure 10. Frame width = 1. 40A2845..3 mm. . 158 .

Figure 11. 2Cd1 horizon under plane polarized light) .. 00P0001. New York Co. 97P0547. Frame width = 1. Umatilla Co. 159 . (Tower pedon. Oriented illuvial clay (argillans) surrounding skeletal grains.. Bw1 horizon under plane polarized light).5 mm. Figure 12.1 mm (Paxon pedon. Fe oxide nodule from an Andisol in Blue Mountains of eastern Oregon. Frame width = 2. OR. NY.

Gunnison Co. while clay (plasma) in the s-matrix is partially anisotropic due to stress orientation (shrinkswell processes). Void that has smooth edges and is elongated. This void type is described by Brewer (1976) as a vugh. E&Bt horizon under cross polarized light). (Troutville pedon. 160 . (Endlich pedon. 99P0002..Figure 13. CO. Compound packing voids. Frame width = 1. surrounded by illuvial clay (argillans).0 mm. 99P0001.0 mm. Clay lining channels is anisotropic due to orientation during deposition. Frame width = 1. Figure 14. Bt1 horizon under crossed polarized light).

The walls consisting of “smooth.. UT. 81P0610.S. Relative pore volumes at 30 kPa for soil fabric coarse-fine distributions for some U. surface crust of a Typic Haplargid. These vesicles were formed in the thin. soils. 161 . A1 horizon under crossed polarized light). Frame width = 3. Figure 16.Figure 15. simple curves” indicates that this void is a vesicle. Juab Co.2 mm (Dera pedon.

Fabric has an opal and chalcedony laminar cap. OR. Figure 18. (Series name not designated. Fremont County. The absorption of silica onto established silica phases leads to formation of nodules. Pedon 87P0513.0 mm. Frame width = 2. The matrix above and below is composed of durinodes (non-crystalline silica) surrounded by moderately-oriented silicate clays.. (Frisite pedon. Frame width = 1. 162 . A horizon under cross polarized light). Clay can provide the initial absorption surface for silica in soil solution. 98P0453. 2Bkqm horizon under plane polarized light).Figure 17. Horizon with duripan exhibiting silica cementation. WY. Joint planes (platy structure) formed in the surface horizon of a soil.5 mm. Jefferson Co.

stainless steel. Crush sample so as to pass the 2-mm sieve with a minimum reduction in size. Crush the NF sample by hand or with mortar and pestle. Safety If ovens are used. Reagents 6. Coleman.01-g sensitivity and 500-g capacity 5. e.3 Sieves.4 Oven. 3. 163 . 2. Soil Survey field offices. brass.1 Use natural fabric (NF) samples in pint containers. Dissolve 35. use Calgon.to 0. Rubbermaid or equivalent.1 Bowls. A correction should be made for the sand > 0. thereby reducing the percentage of aggregates that are retained on the 0.3. Interferences Air bubbles in the sieve can create tension in the water.g. 2. with lifting tab 6.3. Assemble a 2-mm sieve on top of a 1mm sieve. Follow standard laboratory safety precautions. 1800 mL 5. Aggregate stability is a function of whether the cohesive forces between particles can withstand the applied disruptive force. 5.2 1 mm.5-mm sieve after sample has been submerged in RO water overnight followed by agitation of sample. water softener. 110°C 5.1 0. square-hole 5. 203-mm diameter.5 mm resistant to dispersion in sodium hexametaphosphate. 50-mm height 5. Variation in the moisture content of airdry soils can affect results. Equipment 5.5 mm.5-mm Aggregates Retained (3F1a1a) 1. Model 8553-462. 7. Disaggregration of soil mass into aggregates requires the application of a disrupting force.3. Summary of Method This method (3F1a1a) measures the retention of air-dry aggregates (2 to 1 mm) on a 0.35.7 g of sodium hexametaphosphate (Na4P2O7) and 7. ±0.2 Electronic balance. This procedure was developed for use by the Natural Resources Conservation Service.Wet Aggregate Stability (3F) Wet-Sieving (3F1) Air-dry. Application An aggregate is a group of primary particles that cohere to each other more strongly than to other surrounding soil particles (Soil Science Society of America. tillage and organic-matter additions. 57-mm diameter x 15-mm deep. hot surfaces can be a hazard.5 Camping plate. 203-mm diameter. 50-mm height 5. stainless steel. no.6 Aluminum foil dish. 1997). Sieve entire NF sample. Procedure 7. 50-mm height 5. 4. 5. brass.3 2 mm. and erosion by wind and water (Nimmo and Perkins. 152-mm diameter. This method provides a measure of aggregate stability following a disruption of initially air-dry aggregates by abrupt submergence followed by wet sieving. 125-mm diameter. Alternatively. 2 to 1 mm. Peak 1. The measurement can serve as a predictor of infiltration and soil erosion potential.2 Sodium hexametaphosphate solution.5-mm sieve.1 Reverse osmosis (RO) water 6. The analysis of soil aggregation can be used to evaluate or predict the effects of various agricultural techniques.94 g of sodium carbonate (Na2CO3) in 1 L of RO water. 2002).

Alternatively. and dry for 2 to 2.11 Thoroughly wash sieve and plate with RO water. Place sieve on Coleman plate.5-mm sieve with sample in sodium hexametaphosphate (or Calgon) solution so that the solution line is at a 35-mm height above the base of screen. Alternatively.5 mm. Aggregates should not touch. and sample. Report Report aggregate stability as a percentage of aggregates (2. the plate retains the soil that drops through the sieve. Record weight. 7.05-g sample of the 2. and sample.to 0. If no sand (>0. place in oven. On the upward strokes. Remove air bubbles with a syringe.2 Place the material that is retained on 1-mm sieve in pint container and discard the remaining material.7 Remove sieve from water bowl. 7. 7.5 mm) is left on sieve.to 0.5-mm sieve SW = Weight of 2. drain sieve but do not raise so high that air enters to beneath the sieve.to 1-mm material in aluminum foil dishes. Discard sample and brush sieve and plate. 8. Gently triturate the dispersing solution with the fingers to remove soft <0. During drying process.. Calculations Aggregates (%) = [(WR .4 Place 0. plate.SW)/(3. plate. place 3 g of Calgon in plastic bowl and stir until dissolved. Record weight.5 mm material adhering to the > 0.5 mm) is present.to 1mm sample.5 Distribute the 3.6 Agitate the sample by raising and lowering the sieve in the water bowl 20 times in 40 s. 7. discard sample from sieve and plate by brushing.00 – Sw)] x 100 where: WR = Total weight of aggregates retained on 0.5 h at 110°C. especially those sieves with sodium hexametaphosphate solution.5 h at 110°C.5-mm sieve in plastic bowl and fill bowl so that the water level is at a 20-mm height above the base of screen. Remove sieve from sodium hexametaphosphate (or Calgon) solution and rinse with RO water until all sodium hexametaphosphate (or Calgon) solution has passed through sieve. Sample is those aggregates retained on 0.8 Remove the sample from the oven. Record weight. Weigh sieve and plate.5-mm) retained after wet sieving. 7.5-mm fraction is >50% of the 2. and only the sand (>0. Record weight. and dry in oven for 2 to 2.10 Remove sample from oven.5-mm sieve. 7. Weigh a 3. 7. discard sample on plate and disperse that retained on the sieve with sodium hexametaphosphate solution. Allow sample to sit overnight.3 Sieve the material again with 1-mm sieve to remove dust and other small particles.9 Calculate the Sw from the particle-size data (procedure 3A1). If there is sand (>0. Place the 0.7. place on Coleman plate.00-g sample (2 to 1 mm) on the 0.5-mm sand 9. Weigh sieve.00 ± 0. Weigh sieve and plate. calculate the Sw from the particle-size data (procedure 3A1). Do not report determinations if the 2.to 0. 7. 164 .5-mm sieve. 7.5 mm) and no particle-size data. Weigh the sieve.

01-g sensitivity 5. WI.2 Oven.3 Gas pycnometer. calculating soil volume or mass. 4. 2. 2003). or other soil properties affected by volume displacement of rock fragments (Flint and Childs. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.S. and for mathematically correcting bulk soil samples containing significant amounts of rock fragments so as to determine fine-soil density. 3. 2002). ASA and SSSA. Madison. Helium gas is the most commonly recommended gas since its small atomic dimensions assures penetration into crevices and pores approaching one Angstrom (10-10m) in dimension. 1984. >2 mm (3G1a2) 1. 165 . Particle density is required for sedimentation analysis. Quantachrome Instruments. Soil Sci. 5. 1997. Topp (eds. Boynton Beach. Equipment 5. Application Density is defined as mass per unit volume. Instrument should be calibrated when environmental conditions change. 11. water content. References Nimmo. Part 4.10. 2002. Am.R. Physical methods. Particle Density (3G) Pycnometer Gas Displacement (3G1) Oven-dry. Reagents 6. In J. Book Series No. <2 mm (3G1a1) Oven-dry. 1990).1 Electronic balance. Dane and G.. Displacement gas will evaporate water molecules and create additional partial pressure (Flint and Flint. FL 6. Penta-pycnometer. Perkins. 110°C 5. Summary of Method This method (3G1) determines particle density by the pycnometer gas displacement procedure. Madison. Soil Science Society of America. Interferences Sample should be dry. Procedure 7. Temperature should be relatively constant since the method uses the ideal gas equation of state.1 Oven-dry the soil sample at 110°C overnight.C. WI. and K. Soc. Aggegate stabililty and size distribution. J. 317-328. Childs and Flint. p. 5.1 Helium gas 7. This is accomplished by employing Archimedes’ principle of fluid displacement to determine the volume. Follow standard laboratory safety practices. 2002). Safety No significant hazards are associated with this procedure. Am. The displaced fluid is a gas that can penetrate the finest pores..H. and its behavior as an ideal gas is also desirable. Particle density refers to the density of the solid particles collectively (Flint and Flint. thereby assuring maximum accuracy (Quantachrome Instruments. Soil Sci. Glossary of soil science terms. ±0.).

01 g.C. 7. Nelson. WI. p.01g.8 Place the sample cells into the sample cell holder. and W.7.. Determining soil content and expressing properties of gypsiferous soils. and L.6 Select the largest sample cell size of 135. Particle density. L. Boynton Beach.9 Define each cell with sample cell size. 7. 7.C. The sample should fill at least half of the sample cell volume. 7. 1978. FL 166 .4 Validate the calibration by determining the volume of the calibration sphere. References Flint. J.14 Calculate the particle density. 7.13 Record the average volume for each sample.12 Start the sample run. Part 4. 10.D.5 If volumes are outside specification range.10 Set the instrument to multi run and enter the number of runs between 3 and 5. and sample identification number. or 10 cc.E. 2003. In J. 7. 2002. ASA and SSSA.) Methods of soil analysis. 5. 11.H.7 Weigh the sample cell to the nearest 0. R.3 Set the regulator pressure to slightly over 20 PSIG. Record the weight. Am. 7. 7. Dane and G. 42:659-661. 7.2 Allow the instrument to warm up for least 30 min prior to use. recalibrate the instrument per instruction manual. 50. 7. Soc. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. The difference is the sample weight. 7. weight. Properly seal the cell holder with the cover.11 Set the purge mode to 3 pulse cycles.. Physical methods.E. Nettleton. 229-240. A. Quantachrome Corporation.01 unit on either the <2-mm or >2-mm particle-size fraction. Report Report particle density (g cm-3) to the nearest 0. Penta-pycnometer instruction manual. Klameth. Flint. Quantachrome Corporation. 8. Soil Sci. Calculations Particle density (g cm-3) = Sample weight (g)/Sample volume 9. Topp (eds. Place sample in the sample cell and reweigh to the nearest 0. Madison. Book Series No. Soil Sci. 7.L. Am.

Soil and rock.08. and have a reasonably high equivalent weight in order to minimize the consequences of errors in weighing (Day and Underwood. Refer to procedure 4F1 for the definition of LL. The PL is the percent water content of a soil at the boundary between the plastic and brittle states. plastic limit. Commonly a solution is standardized by a titration in which it reacts with a weighed portion of a primary standard. it is customary to prepare solutions of an acid and base of approximately the desired concentration and then to standardize one of the solutions against a primary standard. Annual book of ASTM standards. stable (easy to dry. Application The process by which the concentration of a solution is accurately ascertained is known as standardization (Dean.1 to 0. <0. Refer to ASTM method D 4318 (American Society for Testing and Materials. 2004). the PI is the difference in the water content between the LL and the plastic limit (PL). The boundary is the water content at which a soil can no longer be deformed by rolling into 3. ASTM. SOIL AND WATER CHEMICAL EXTRACTIONS AND ANALYSES (4) Acid Standardization (4A) 1. a primary standard should be in a state of known high purity (typically <0. 1995). For acid-base titrations.4-mm basis (40-mesh) (procedure 3H1).2-mm (1/8-in) threads without crumbling. PA. Section 4. The LL is reported as percent water on a <0. 2004). 1980). not very hydroscopic. Vol.4 mm (3H2b1) The PI is the range of water content over which a soil behaves plastically. The solution thus standardized can be used a secondary standard to obtain the normality of the other solution. Atterberg Limits (3H) Plasticity Index (3H2) Air-Dry. Philadelphia. and plasticity index for soils.4 mm (3H2a1) Field-Moist.4 mm (3H1b1) Liquid Limit (LL) is the percent water content of a soil at the arbitrarily defined boundary between the liquid and plastic states. References American Society for Testing and Materials. 2004. geosynthesis.2% impurities). Numerically. In addition. The reaction between the titrant and the substance selected as a primary standard should fulfill the requirements for titrimetric analysis. D 4318. Some widely used primary standards are as follows: 167 . or lose weight upon exposure to air). Refer to ASTM method D 4318 (American Society for Testing and Materials.4 mm (3H1a1) Field-Moist.Atterberg Limits (3H) Liquid Limit (LL) (3H1) Air-Dry. This water content is defined as the water content at which a pat of soil placed in a standard cup and cut by a groove of standard dimensions will flow together at the base of the groove for a distance of 13 mm (1/2 in) when subjected to 25 shocks from the cup being dropped 10 mm in a standard LL apparatus operated at a rate of 2 shocks s-1. 04. <0. <0. The PL is reported as percent water on a <0. dimension stone.4-mm basis (procedure 3H2). Construction. Standard tests for liquid limit. <0.

Dissolve 0. Wiping the electrode dry with a cloth.(KH(IO3)2). Na2CO3) in reverse osmosis deionized (RODI) water. Molecular weight = 100. Phenolphthalein bitatrate indicator. Thoroughly wash hands after handling reagents. Prepare 10 of these Na2CO3 solutions plus 8 blanks and titrate with the acid to be standardized (e. Use gloves to weigh the primary standard in weighing vessel. Molecular weight = 204. storing. Potassium biphthalate . or weighing the reagent. 5.g. Summary of Method Dissolve a known amount of the primary standard (e. Potassium bicarbonate .3 Weighing vessel. If all else fails.224.(KHC4H4O6). H2SO4). 3.599. Slow electrode response may cause the end point to be overshot. or similar material may cause electrode polarization.5 g in 50% ethanol and titrate to phenolphthalein end point. Cleaning the electrode with detergent solution may decrease the response time. Weak acid.116. Bromthymol blue indicator. change the electrode. 4.(KHCO3).10-mg sensitivity 5. Molecular weight = 105. Refer to Table 1 for a list of some common acids and bases.4 Desiccator 168 . Contamination of the primary standard may occur when drying. 110οC 5. laboratory tissue. Review Material Safety Data Sheets (MSDS) for reagents. excluding CO2. Strong acid.(KHC8H4O4). Use sodium bicarbonate and water to neutralize and dilute spilled acids.(HgO) Molecular weight = 216. Molecular weight = 188. Bromcresol green indicator. Bromthymol blue end biodate point.(C6H5CO2H).2 Oven. 40 x 50mm 5. Dissolve about 0. Potassium bitatrate . Dispense concentrated acids in a fume hood. first tint of green end point.(Na2CO3).123.912. Methyl red indicator.5 g with 15 g of KBr in 25 mL of reverse osmosis deionized (RODI) water. Calculate the normality of the acid from the mean blank and titers. first green end point. Phenolphthalein indicator.g. HCl. Weak acid. Low solubility. ±0.Benzoic acid . Molding problem. Report the normality and standard deviation for the acid standardization.1 Electronic balance. Molecular weight = 122. Mercuric oxide .360. Dissolve in water. Potassium biodate .988 Bromocresol green indicator.. Interferences Clean the glass electrode by rinsing with distilled water. Follow the manufacturer’s safety precautions when using the automatic titrator.(Na2B4O7·10H2O).. Borax . 2. Molecular weight = 381. Equipment 5. Dry primary standards and store in a dessicator to prevent hydration. Safety Wear protective clothing and eye protection when preparing reagents. Sodium carbonate . Be prepared to use safety showers and eyewash stations if necessary. Molecular weight = 389.178.

00. Metrohm Ltd. return to Section 7. 7.6 Combination pH-reference electrode. ASTM Type I grade of reagent water 6.SW10 and to eight empty beakers for blanks (B1.5 Prepare nine more Na2CO3 solutions (SW2 …SW10) by this same procedure (Sections 7. 7. Let cool in a desiccator to room temperature (≈ 30 min). 7. 7. 7. proceed to Section 7. Inc.1 to the nearest 0.4). Add 0. Procedure 7.4.. Metrohm Ltd.15 . Brinkmann Instruments.2 Refer to Acid Standardization Form.4.5.8 Set-up the automatic titrator to set end point titration mode.2 and begin again. borosilicate.1 Re-weigh the weighing vessel plus Na2CO3 designated in Section 7.00.1mg (SW1). 5.. Metrohm Ltd... but if not.1 to the nearest 0.18) 6.00. 250 mL.5 Automatic titrator. sample changer.8 Titration beakers. and dispenser.2 pH buffers (4.4b is within 0. Inc. 6.5. Reagents 6. with control unit.1mg (VW1b).2 pH High 169 . 7.. 7. The "Set" pH parameters are listed as follows: Parameter Measured value Titration rate Stop volume Stop End Point Stop Potential Sensitivity Value pH normal 100.3 Sodium carbonate... and 9.0. 9.. Calibrate the pH electrode with 4.. 99. 7. 7.4. Brinkman Instruments. anhydrous.4 Verify the weighed SW1 as follows: 7. and printer 5..5 mg of the weighed SW1 determined in Section 7.8) and gently swirl to facilitate dissolution of the salt.4 Calcium sulfate (anhydrous) or equivalent desiccant 7.1mg (VW1a).0 mL 9 4.2 Calculate SWC1 as follows: VW1a – VW1b = SWC1.1 Reverse osmosis deionized (RODI) water.1 Place a weighing vessel containing ≈ 10 g of the Na2CO3 in an oven at 110οC overnight. Recalibrate electrode if R2 <0..3 Tare a 250-mL titration beaker on the electronic balance. Brinkman Instruments Inc. Record the weight of the Na2CO3 to the nearest 0.7 Prepare the titration system according to the manufacture’s instructions. Inc.3. Metrohm Ltd.950.8% pure 6.00. 7.. 7.7 Computer. Weigh the weighing vessel plus the Na2CO3 designated in Section 7.3 If SWC1 calculated in Section 7.6 Add 100 mL of RODI water to each of the SW1.18 pH buffers.2 7. with Titrino Workcell software.55 g Na2CO3 to the beaker.. Brinkmann Instruments. 5.

.0188698 mole HCl/g Na2CO3) / (TCS1. 10. If NStd > 0.... Inc...8698)/ TCS1.....10 x 0.10 = TS1..10 – Bm where: TCS1...L...A.. 1995.... J.. Analytical chemistry handbook. and date of standardization..10 = [(SW1. record Nmean to four decimals to left of decimal.10 = Normality calculated from titre (number of equivalents of solute per liter) SW1..5 until 10 (n = 10) are achieved.10 = Corrected sample titre (mL) TS1. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.Fixed End Point Signal Drift Equilibration time 4.3 N1... standard deviation... Dean. Quantitative analysis. 1980.. McGraw Hill..2 TCS1...9 Titrate each of the SW1.8 and record the titres.1 Bmean = Bsum/n where: B = Blank mean (mL) Bsum = Sum of blank titres (mL) n = Number of blanks (n = 8) 8.. NJ.. Inc....10 x 18. discard no more than two suspicious values and return again to Sections 7. Underwood. Prentice-Hall.....10 where: N1....2 to 8. References Day.... Report Report the mean normality of acid (Nmean). If the NStd is < 0... Englewood Cliffs. NY.6 pH 25 5s 7.. Jr.A.5 Calculate standard deviation (Std) for Nmean.0005. 10. 8.SW10 and B1.10 = Sample titre (mL) Bm = Blank mean (mL) 8...10 = Na2CO3 weight (g) 8. 170 . New York.... Calculations 8.. A.0005.........4 Nmean = Nsum/n where: Nmean = Normality mean Nsum = Sum of normalities n = Number of samples (n = 10) 8.10 x 10-3 L ml-1)] = (SW1.. 9.. R.. and.

50 1.74 61.13 104 10 1.53 2.02 1008 71 1.0 1.2 Nitric acid 63.167 1.4 5.92 36.1 0.25 339 30 1.75 111 10 1.0 Moles per Liter 17.155 1.67 9.57 5.8 252 28 0.74 32.02 Ammonia water 17.75 7.1 1020 85 1.045 0.898 Potassium 56.02 127.57 11.05 0.6 2.1 18.42 938 67 1.10 Sodium hydroxide 40 19.70 1. Name Molecular Weight 60.1 46.STANDARDIZATION OF ACIDS Table 1.05 60.5 27.65 9.1 1.54 Phosphoric acid 98 14.0 1766 96 1.3 15.27 Acetic acid Glacial acetic acid Butyric acid Formic acid Hydriodic acid Hydrobromic acid Hydrochloric acid Hydrocyanic acid Hydrofluoric acid Hydrofluosilic acid Hypophosphorus acid 625 50 1.52 hydroxide 1.05 88.01 144.8 2.05 1.9 25 0.18 1.65 1172 70 1.04 Lactic acid 90.06 1.20 1.04 110 10 1.96 1.03 20.5 11.1 28.2 923 60 1.5 757 50 1.7 1445 85 1.996 1.84 Sulfurous acid 82.38 1.51 0.2 6 1.99 14.9 Grams per Liter 1045 376 912 1080 264 969 705 110 720 552 424 105 676 19.70 Sulfuric acid 98. Common commercial strengths of acids and bases.3 23.1 13.11 ______________________________________________________________________________________ 171 .9 80.27 10.09 Sodium carbonate 106.1 66.40 837 61 1.82 11.86 8.0 14.37 Perchloric acid 100.5 36 95 90 25 57 47 10 48 40 36 10 97 2 55 50 30 Specific Gravity 1.89 6.94 109 10 1.4 6.1 763 50 1.9 642 578 382 Percent by Weight 99.50 1.14 1.697 0.47 5.

10 NStd 172 .Acid Standardization Acid:_____________ Date:_______ Technician: _________ Sample Titer TS1 Blanks B1 B2 SW2 TS2 B3 B4 SW3 TS3 B5 B6 SW4 SW5 SW5 TS5 TS4 B7 B8 Bsum Bmean SW6 TS6 TCS6 TCS5 TCS4 TCS3 TCS2 CorrectedS ample Titer TCS1 Vessel Weight #1 Beginning Weight Ending Weight #2 Beginning Weight Ending Weight #3 Beginning Weight Ending Weight #4 Beginning Weight Ending Weight #5 Beginning Weight Ending Weight #6 Beginning Weight Ending Weight #7 Beginning Weight Ending Weight #8 Beginning Weight Ending Weight #9 Beginning Weight Ending Weight #10 Beginning Weight Ending Weight VW1a VW1b VW2a VW2b VW3a VW3b VW4a VW4b VW5a VW5b VW6a VW6b VW7a VW7b VW8a VW8b VW9a VW9b VW10a VW10b Sample Weight SW1 SW7 TS7 TCS7 SW8 TS8 TCS8 SW9 TS9 TCS9 SW10 TS10 TCS10 N1….

CEC is a measure of the total quantity of negative charges per unit weight of the material and is commonly expressed in units of milliequivalents per 100 g of soil (meq 100 g-1) or centimoles per kg of soil (cmol(+) kg-1).2) 100 to 150 60 to 100 40 to 50 20 to 40 10 to 40 2 to 16 5 to 10 0 These very broad CEC ranges are intended only as general guidelines.0 to greater than 100 cmol(+) kg-1 soil. dependent upon negative charges of soil components arising from permanently charged or pH-dependent sites on organic matter and mineral colloid surfaces.. Common CEC values for some soil components (NSSL. CEC is a reversible reaction in soil solution. 1982).. Some soils with abundant goethite and gibbsite. dielectric constant.. with the anion molecular retention capacity of these soils usually much smaller than the CEC (Tisdale et al. The mechanisms for these negative charges are isomorphic substitution within layered silicate minerals. electrolyte level. Soil mineral and organic colloidal particles have negative valence charges that hold dissociable cations. 1988). as do some oxic horizons or subsoils of Oxisols (Soil Survey Staff. and thus are "colloidal electrolytes" (Jackson. 1982). Isomorphic substitution produces permanent charge. The method of determination is routinely reported with CEC data.g. broken bonds at mineral edges and external surfaces. The CEC is a measure of the quantity of readily exchangeable cations that neutralize negative charges in the soil (Rhoades. the cation exchange capacity (CEC) is generally considered to be more important than anion exchange (AEC). 1975) are as follows: Soil Component Organic Matter “Amorphous” Clay Vermiculite Montmorillonite Halloysite 4H2O Illlite Chlorite Kaolinite Halloysite 2H20 Sesquioxides cmol(+) kg-1 200 to 400 160 (at pH 8.SOIL AND WATER CHEMICAL EXTRACTIONS AND ANALYSES (4) Ion Exchange and Extractable Cations (4B) Ion exchange is a reversible process by which one cation or anion held on the solid phase is exchanged with another cation or anion in the liquid phase. 1985). The CEC can range from less than 1. The other charge mechanisms produce variable charge which is dependent on the soil solution phase as affected by soil pH. The SSL reports cmol(+) kg-1 on <2-mm base. The term equivalent is defined as "1 gram atomic weight of hydrogen or the amount of any other ion that will combine with or displace this amount of hydrogen". the term milliequivalent may be defined as "1 milligram of hydrogen or the amount of any other ion that will combine with or displace it" (Tisdale et al. e. As a result of the variable charge in soils. and if two solid phases are in contact. Since the equivalent weight of hydrogen is about 1 gram.. and preferential adsorption of certain ions on particle surfaces (Rhoades. the CEC of 173 . 1958). and nature of anions (Rhoades. ion exchange may also take place between two surfaces (Tisdale et al. the CEC is a property dependent on the method and conditions of determination.0 (net charge of zero) or a small positive charge (Foth and Ellis. valence of counter-ions. 1999). 1982). The milliequivalent weight of a substance is one thousandth of its atomic weight. 1985). may have a CEC to AEC ratio approaching 1. More narrow groupings of CEC values are possible as data are continually collected and correlated. 1985). In most agricultural soils. dissociation of acidic functional groups in organic compounds.

0). 1982) as follows: (1) cation summation (2) direct displacement (3) displacement after washing (4) radioactive tracer The SSL performs a number of CEC methods. CEC-8.g. Knowledge of the operational definition (procedure. concentration of salt. Displacement after washing is the basis for this procedure. washing the soil free of excess saturated salt.2. 1958). 1996).2 is not reported if significant quantities of soluble salts or carbonates are present in the soil. using several different reagents and pH levels.. and concentration) is necessary before evaluating the CEC measurement (Sumner and Miller.. and the equilibrium pH.0 N KCl to determine the exchangeable Al. 1958). 1977). 1975). 1 N KCl. the extraction is determined at or near the soil pH and extracts only the cations held at active exchange sites at the particular pH of the soil. Mg2+. The CEC-8. ECEC may be determined by extracting one soil sample with neutral normal NH4OAc to determine the exchangeable basic cations (Ca2+. 1947).2 is calculated as follows: CEC-8.. i. CEC-8.2 minus the CEC-7 is considered the pH dependent charge from pH 7. Cation summation is the basis for this procedure. An advantage of using this method is that the extractant is highly buffered so that the extraction is performed at a constant and known pH (pH 7. displacing the index cation (NH4+) adsorbed by the soil.2 > CEC-7 > ECEC.2/clay.2) CEC-8. Neutral NH4OAc extracts the same amounts of Ca2+. although many SSL Primary Characterization Data Sheets predating 1975 show CEC8.organic matter in Mollisols in the western United States ranges from 100 to 300 cmol (+) kg-1 (average 200). The 1 N 174 . and measuring the amount of the index cation (NH4+). The CEC’s most commonly reported by the SSL are CEC-7 (4B1a1a1a1).0 (CEC-7) The CEC-7 is a commonly used method (4B1a1a1a1) and has become a standard reference to which other methods are compared (Peech et al. e. cation. K+ as KCl and therefore extractable bases by NH4OAc is used at the SSL in place of KCl-extractable bases. The more widely adopted methods of CEC determination are classified (Rhoades.. The CEC-8. Cation Exchange Capacity: Sum of Cations (CEC-8. The CEC is determined by saturating the exchange sites with an index cation (NH4+) using a mechanical vacuum extractor (Holmgren et al. As a general rule. only affects the soil pH one unit or less.0 to pH 8. These CEC measurements vary according to the nature of the cation employed. Many procedures have been developed to determine CEC. and effective cation exchange capacity (ECEC) (4B4b2). Since the unbuffered salt solution. CEC at the normal soil pH (Coleman et al. and the CEC of organic matter in Histosols ranges from 125 to 185 cmol (+) kg-1 and increases with decomposition of the organic matter (NSSL Staff. the CEC8. Na+. CEC-7 is an analytically determined value and is usually used in calculating the CEC-7/clay ratios. Mg2+. the NH4+ on the exchange complex is easily determined. pH.2 is calculated (4B4b1) by summing the NH4OAc extractable bases (4B1a1b1-4) plus the BaCl2-TEA extractable acidity (4B2a1a1 or 4B2b1a1). The CEC measurement should not be thought of as highly exact but rather as an equilibrium measurement under the conditions selected (Jackson. which measures the effective cation exchange capacity (ECEC). and K+) and by extracting another sample of the same soil with 1.2 = NH4OAc extractable bases + Extractable acidity Effective Cation Exchange Capacity: NH4OAc Extractable Bases + Aluminum: CEC can be measured by extraction with an unbuffered salt.e. Cation Exchange Capacity: NH4OAc. pH 7.. In addition.2 (4B4b1). Na+.

Sumner. E. the ECEC value should be < CEC measured with a buffered solution at pH 7.L.L. NY. The CEC is determined by saturating the exchange sites with an index cation (NH4+). Cation exchange capacity and exchange coefficients. and precipitation. Page. John Wiley & Sons. known pH (7. 1975. Part 3. 1947).0 (CEC-7).H. Juve. References Coleman. Nelson. <2 mm (4B1a1a1a1a-b1) 1. S.G. and J. A sample is leached using 1 N NH4OAc and a mechanical 175 .0) and that the NH4+ on the exchange complex is easily determined.P. Ellis. Part 2. The ECEC is not reported for soils with soluble salts. Soil Sci. Miller. Agron. the ECEC should be less than the CEC measured with a buffered solution at pH 7. The advantages of using this method are that the extractant is highly buffered so that the extraction is performed at a constant. J.T. Kamprath. Am. G. 1947.KCl-extractable Al approximates exchangeable Al and is a measure of "active" acidity present in soils with a 1:1 pH <5. Reed. For soils with pH <7.0. 149-157. Co. Liming. J. The NH4Cl CEC is ≈ equal to the NH4OAc extractable bases plus the KCl extractable Al for noncalcareous soils.S. and J. W. 25 pp. and S.) Methods of soil analysis.J.. The CEC by NH4Cl provides an estimate of the ECEC of the soil (Peech et al. NH4OAc. Madison. Application The cation exchange capacity (CEC) determined with 1 N NH4OAc buffered at pH 7.0. USDA Circ. 1988. NE Peech.. Soil fertility and fertilizers.. polymerization. A mechanically controlled variable rate leaching device. 1958. Macmillan Publ.. Cation exchange capacity. Summary of Method Displacement after washing is the basis for this procedure. and W. H. Beaton. Madison.F. M. National Soil Survey Laboratory Staff. 1947). 41:1207-1208. Monogr. and D.A.B.R... ASA and SSSA.0.L. Adv. Chemical and microbiological properties. 757.. L. washing the soil free of excess saturated salt. 1985. USDA-SCS. 4th ed.. ECEC (4B4b2a) is calculated by summing the NH4OAc bases (4B1a1b1-4) plus the KCl extractable Al (4B2a1a1) as follows: ECEC = NH4OAc extractable bases + KCl-extractable Al Effective Cation Exchange Capacity: NH4Cl (ECEC) The CEC using a neutral unbuffered salt (NH4Cl) is also an analytically determined value (4B1b1a1a1). M. 1996. WI. ASA and SSSA. 9. 10:475. and measuring the amount of the index cation (NH4+). In A.L. 5. Keeney (eds. Ion Exchange and Extractable Cations (4B) Displacement after Washing. Inc. Methods of soils analysis for soil fertility investigations. Weed. Alexander.E. Tisdale. 1982. displacing the index cation (NH4+) adsorbed by the soil. R.. Agron.R. Rhoades. 1201-1229. p. Lincoln. L. Aluminum is non-exchangeable at pH >5. 2 M KCl Rinse (4B1a1a) Steam Distillation. In D. R. Dean. 2nd ed. is a commonly used method and has become a standard reference to which other methods are compared (Peech et al. 1977. Geschwender. NY. WI.5 due to hydrolysis.5.D. p. For a soil with a pH of <7.C. T. Sparks (ed. Chemical methods.0. RSSIU.) Methods of soil analysis. No.. and R. Holmgren. Miller.D. Soil fertility. This ECEC method is less commonly used at the SSL. pH 7 (4B1a) Automatic Extractor. 2.D.L. Proposed tables for soil survey reports. HCl Titration (4B1a1a1a) Cation Exchange Capacity (CEC-7) (4B1a1a1a1) Air-dry or Field-Moist. and B. Foth.

Dissolve 10 g of sodium hydroxide (NaOH) in 200 mL of RODI water. Add 4.10 Centrifuge. or safety glasses) when preparing reagents. 250 mL 5. goggles.1 Reverse osmosis deionized (RODI) water.P. 0. Safety Wear protective clothing (coats. Tecator. polypropylene. 1 and 2) 5. 95%.2 ID x 1. 1996) 4. 3. ≈ 40 mL) or NH4OH and dilute with RODI water to 18 L.3 Ethanol (CH3CH2OH). Nessler's reagent contains mercury which is toxic. Dispense concentrated acids and bases in a fume hood.2 Ammonium acetate solution (NH4OAc).45 µm.0. Stir until dissolved. U. and tared extraction tubes 5. pH 7 is reported in meq 100 g-1 or (cmol (+) kg-1) soil in procedure 4B1a1a1a1. 1977). ASTM Type I grade of reagent water 6.0 with CH3COOH (typically.2 Mechanical vacuum extractor. 6.68 g of mercuric iodide (HgI2). aprons. 60-mL. Ethanol is flammable. Lincoln. 1 N. Isopropanol rinses have been used for some soils in which ethanol removes adsorbed NH4+. ±1. The NH4+ saturated soil is rinsed with ethanol to remove the NH4+ that was not adsorbed.4 Rubber tubing. Needham Heights. SAMPLETEX. Avoid open flames and sparks. Ethanol removes some adsorbed NH4+ from the exchange sites of some soils. MA 6. Centra. 24-place. Mix and adjust to pH 7. for extraction (0. Proper disposal of the Nessler's reagent and clean-up of equipment in contact with the reagent is necessary. especially concentrated acids and bases. Use the safety showers and eyewash stations to dilute spilled acids and bases. Add 5.S.. NE (Fig.7 Syringe filters. Thoroughly wash hands after handling reagents. Use sodium bicarbonate and water to neutralize and dilute spilled acids. Add 1026 mL of glacial acetic acid (CH3COOH) to 15 L RODI water. Soils that contain large amounts of soluble carbonates can change the extractant pH and/or can contribute to erroneously high cation levels in the extract. Thermo IEC. 5.8 Wash bottles 5. straight neck.4 mm (1/8 ID x 1/16 OD x 1 in) for connecting syringe barrels. 6. Transfer NaOH solution to a 250-mL volumetric flask 176 .4 Nessler's reagent. This leachate is then analyzed by steam distillation and titration to determine the NH4+ adsorbed on the soil exchange complex. pH 7.9 Vials. plastic 5. The soil is then rinsed with 2 M KCl. The CEC by NH4OAc.6 Digestion tubes. 3. The extract is weighed and saved for analyses of the cations.56 g of potassium iodide (KI) to 30 mL RODI water. MAVCO Industries. Follow the manufacturer's safety precautions when using the vacuum extractor and the Kjeltec Auto Analyzers. Perstorp Analytical 5. Interferences Incomplete saturation of the soil with NH4+ and insufficient removal of NH4+ are the greatest interferences to this method. Reagents 6. 5. and gloves) and eye protection (face shields.5 Kjeltec Auto 2300 Sampler System. Add 1224 mL of concentrated ammonium hydroxide (NH4OH). Standard laboratory equipment includes fire blankets and extinguishers for use when necessary. Cool.0-mg sensitivity 5. Equipment 5. sleeve guards. Soils that contain large amounts of vermiculite can irreversibly "fix" NH4+. reservoir.6 OD x 6.1 Electronic balance. Allow to stand one day to equilibrate to room temperature. This method overestimates the “field” CEC of soils with pH <7 (Summer and Miller.3 Tubes.45-µm filter).vacuum extractor (Holmgren et al. GP-8. Whatman 5.

Solution should not contain a precipitate. or stirring may be required to wet organic samples. Turn off the extractor. Removal of Excess Ammonium Acetate 7. Add 1341. Discard the excess properly.2 Place labeled ET on extractor and connect to corresponding tared extraction tube (TETNH4OAc) with rubber tubing. standardized. Refer to procedure for Standardization of Acids.5 Add 40 mL of NH4OAc solution to the RT. 7.1 Weigh 2. with bromcresol green-methyl red indicator (0.9 Extract at the 30-min extraction rate the ethanol solution until 2 mL of this solution remains above the soil level. Chempure 6.6 Next day. Do not let soil dry. Weigh each TETNH4OAc containing the NH4OAc extract to the nearest mg. If sample is fine-grind.9 g of KCl reagent in 8 L RODI water. 7. 7.3 Use wash bottle to rinse inside of ET with NH4OAc. Some samples may be cloudy and need to be filtered prior to analysis on the AA.5 or 1g. 7. Set extractor for an overnight (12h) extraction. 4% (w:v). 7. then store samples at 4°C in plastic tubes. weigh 1 g to the nearest mg. Leave the rubber tubing on the ET. 6. respectively. Dilute 167 mL of concentrated HCl in 20 L of RODI water.8 NaOH. Carefully remove TETNH4OAc. 177 . 1 M.1 N. Procedure Extraction of Bases 7. Do not let soil dry. 7. Allow solution to equilibrate to room temperature. Dilute to volume with RODI water and thoroughly mix.7 Mix the extract in each TETNH4OAc by manually shaking. The solution in the vial is reserved for analyses of extracted cations (procedure 4B1a1b1-4) on the atomic absorption spectrophotometer (AAS). remove RT from top of extractor and place in a clean container.05% methyl red). 0. 7.6 Boric acid. 6. Fill ET to the 20-mL mark with NH4OAc solution (≈ 10 mL). All soil should be wetted and no air bubbles. Use a wash bottle to rinse the sides of the ET with ethanol to remove any remaining NH4OAc or soil particles adhering to the ET. Secure RT to top of ET tube and let stand for 30 min.075 % bromcresol green and 0.and slowly add K-Hg-I solution. 6. swirling. air-dry soil to the nearest mg and place in a labeled extraction tube (ET). Solution can be used immediately. If sample is moist.7 Hydrochloric acid (HCl). 7. Dilute to 9 L with RODI water.4 Secure reservoir tube (RT) to top of ET tube and let stand for 30 min. Extractor will turn off automatically. Fill ET to the 20-mL mark with ethanol. weigh enough soil to achieve ≈ 2. Dilute to 9 L with RODI water. Prepare one quality control check sample per 24 samples. If extracts are not to be determined immediately after collection. All soil should be wetted and no air bubbles. Shaking. 2 M. Fill a labeled plastic vial with extract solution and cap.5 Potassium chloride solution. Add 500 mL of 50% NaOH solution to 8 L of RODI water. Store in brown bottle to protect from light.5 g of <2-mm.8 Re-connect the TETNH4OAc with paired ET. of air-dry soil. Turn off extractor. Extract at 30-min rate the NH4OAc solution until 2 mL of this solution remains above soil level.

Fill ET to the 20-mL mark with KCl solution and let stand for 30.21 When using new reagents. Turn off the extractor.20 Refer to the manufacturer’s manual for operation of the distillation unit. leaving the tubing connected to the ET. 7. 178 . If extracts are not to be determined immediately after collection. Distillation and titration are performed automatically. reagent blanks are distilled in 2 sets of 6. 7. Discard the ethanol properly. Repeat until a negative test is obtained.16 Use a wash bottle to rinse inside of ET with 2 M KCl to remove any remaining ethanol or soil particles adhering to the ET. one set per Kjeltec machine. Turn off the extractor. Do not let soil dry. Extract (≈ 45 min) the ethanol until 2 mL of this solution remains above the soil level.. boric acid. repeat the ethanol wash and retest with Nessler's reagent. Close the safety door. Program: Kjeldahl 1 Receiving solution (boric acid): 30 mL Water: 0 mL Alkali (NaOH): 20 mL Mode: Delay Time: 1 s Distillation: Volume Tube Drain: Yes 7. Do not let soil dry. The following are only very general guidelines for instrument conditions. red to reddish brown precipitate is a positive test. 2 M KCl Rinse 7. Operation.18 Secure RT to top of ET tube. 7. 7.22 Record the normality of standardized acid.17 Extract at the 30-min rate the KCl solution until 2 mL of this solution remains above soil level. Add 40 mL KCl solution to RT and set the extract for 45 min.15 Connect a new labeled extraction tube (ETKCl) with rubber tubing to ET on extractor. 7. 7. e. Test for NH4+ by using Nessler's reagent.23 Connect the tube to the distillation unit.7. Record the titer in mL of titrant.19 Transfer the contents of the ETKCl to a 250-mL digestion tube.14 After the final ethanol wash. collect a few drops of ethanol extract from the ET on a spot plate. the mean reagent blank titer is automatically subtracted from the sample titer.g.11 Re-connect the TETNH4OAc to the ET and add 55 mL of ethanol to the RT. Remove the ET and ETKCl from the extractor. Remove the TETNH4OAc. All soil should be wetted and no air bubbles. Each set of 6 is averaged and recorded on bench worksheet and manually set on each machine. 7. A yellow. 7.10 Add 45 mL of ethanol to the RT. Turn off extractor. Steam Distillation: Setup. Disconnect the TETNH4OAc from the ET and discard the ethanol properly. If the test is positive. and Analysis 7. During the steam distillation. Set the extractor for 45 min. then store samples at 4°C.

No. Sumner. 5.L.T. Dean.1 meq 100 g-1 (cmol (+) kg-1).. L.F. Calculations CEC = [Titer x N x 100 x R]/[Sample Weight (g)] where: CEC = Cation Exchange Capacity (meq 100 g-1) Titer = Titer of sample (mL) N = Normality of HCl titrant 100 = Conversion factor to 100-g basis R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 9.A. and W. 25 pp. A mechanically controlled variable rate leaching device. Alexander. 11. 41:1207-1208. Report Report CEC-7 to the nearest 0. 179 . WI. 1201-1229. ASA and SSSA. L.. Peech.G.8. Juve.S. R.L. M. References Holmgren.) Methods of soil analysis. In D. Miller. Geschwender. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Madison. Soil Sci.C. J. Methods of soil analysis for soil fertility investigations. 1947. 1977. and J. Cation exchange capacity and exchange coefficients.P. p. Part 3.E. 10. G. M. USDA Circ. 757. 1996. Reed. Am.. Chemical methods. Sparks (ed. and R.

Fig. e.. MAVCO Industries.1. 2. SAMPLETEX. NE.Fig.g. Mechanical vacuum extractor. 180 . cation exchange capacity. NH4OAc. Lincoln. pH 7. Mechanical vacuum extractor used at the USDA-NRCS Soil Survey Laboratory for chemical extractions and analyses.

1947). Use the safety showers and eyewash stations to dilute spilled acids and bases. Avoid open flames and sparks. Summary of Method Displacement after washing is the basis for this procedure. Lincoln. The CEC by NH4Cl is reported as meq 100 g-1 or (cmol (+) kg-1) soil in procedure 4B1b1a1a1. Safety Wear protective clothing (coats.4 mm (1/8 ID x 1/16 OD x 1 in) for connecting syringe barrels.6 OD x 6. SAMPLETEX. goggles. Tecator. A sample is leached using 1 N NH4Cl and a mechanical vacuum extractor (Holmgren et al.4 Rubber tubing.5 Kjeltec Auto 2300 Sampler System. The NH4+ saturated soil is rinsed with ethanol to remove the NH4+ that was not adsorbed. e. especially concentrated acids and bases. 24-place. sleeve guards. The extract is weighed and saved for analyses of the cations. polypropylene. 5. Perstorp Analytical 181 . 5.3 Tubes. procedure 4B1a1a1a1) 5.0. 3. HCl Titration (4B1b1a1a) Cation Exchange Capacity (4B1b1a1a1) Air-dry or Field-Moist. 3. <2 mm (4B1b1a1a1a-b1) 1. Interferences Incomplete saturation of the soil with NH4+ and insufficient removal of NH4+ are the greatest interferences to this method. for extraction (0. 2 M KCl Rinse (4B1b1a) Steam Distillation.Ion Exchange and Extractable Cations (4B) Displacement after Washing. The CEC is determined by saturating the exchange sites with an index cation (NH4+). Proper disposal of the Nessler's reagent and clean-up of equipment in contact with the reagent is necessary. Follow the manufacturer's safety precautions when using the vacuum extractor and the Kjeltec Auto Analyzers.. NH4Cl (4B1b) Automatic Extractor. Nessler's reagent contains mercury which is toxic. Ethanol is flammable. and measuring the amount of the index cation (NH4+). reservoir. and gloves) and eye protection (face shields. ±1. Isopropanol rinses have been used for some soils in which ethanol removes adsorbed NH4+. or safety glasses) when preparing reagents. Equipment 5.0-mg sensitivity 5. The NH4Cl CEC is approximately equal to the NH4OAc extractable bases plus the KCl extractable Al for noncalcareous soils. Thoroughly wash hands after handling reagents. Standard laboratory equipment includes fire blankets and extinguishers for use when necessary.2 ID x 1. 2. 1977). Dispense concentrated acids and bases in a fume hood. For a soil with a pH of <7. This leachate is then analyzed by steam distillation and titration to determine the NH4+ adsorbed on the soil exchange complex. Use sodium bicarbonate and water to neutralize and dilute spilled acids. 1 and 2. Soils that contain large amounts of soluble carbonates can change the extractant pH and/or can contribute to erroneously high cation levels in the extract.1 Electronic balance. The soil is then rinsed with 2 M KCl. 60-mL. is an estimate of the “effective” CEC (ECEC) of the soil (Peech et al.0. displacing the index cation (NH4+) adsorbed by the soil. 1 N NH4Cl..g. the ECEC values should be <CEC measured with a buffered solution at pH 7. aprons..45-µm filter). NE (See Fig. MAVCO Industries.2 Mechanical Vacuum Extractor. Application The cation exchange capacity (CEC) determined with a neutral cation unbuffered salt. washing the soil free of excess saturated salt. Ethanol removes some adsorbed NH4+ from the exchange sites of some soils. and tared extraction tubes 5. Soils that contain large amounts of vermiculite can irreversibly "fix" NH4+. 4.

6. 4% (w:v).8 NaOH. of air-dry soil. Do not let soil dry.5 Add 40 mL of NH4Cl solution to the RT. respectively.1 Reverse osmosis deionized (RODI) water.2 Ammonium chloride solution (NH4Cl). Fill ET to the 20-mL mark with NH4Cl solution (≈ 10 mL).8 Wash bottles 5. Dilute to volume with RODI water and thoroughly mix. Shaking. Whatman 5.6 Boric acid. Turn off extractor. air-dry soil to the nearest mg and place in a labeled extraction tube (ET).P.3 Ethanol (CH3CH2OH). 0. 7. Dissolve 535 g of NH4Cl reagent in RODI water and dilute to 10 L. Procedure Extraction of Bases 7.45 µm. Chempure. Store in brown bottle to protect from light.7 Syringe filters.7 Mix the extract in each TETNH4Cl by manually shaking. 1 M. If sample is fine-grind.5 g of <2-mm. 7. swirling.6 Digestion tubes. Add 5. 7.56 g of potassium iodide (KI) to 30 mL RODI water. GP-8. Leave the rubber tubing on the ET. Dilute to 9 L with RODI water. or stirring may be required to wet organic samples.4 Nessler's reagent. Reagents 6.3 Use wash bottle to rinse inside of ET with NH4Cl. Refer to procedure for Standardization of Acids. The solution in the vial is reserved for 182 . Weigh each TETNH4Cl containing the NH4Cl extract to the nearest mg. 1 N. Extract at 30-min rate the NH4Cl solution until 2 mL of this solution remains above soil level. standardized. Set extractor for an overnight (12h) extraction. Allow solution to equilibrate to room temperature. Add 4. If sample is moist. 6. 6. weigh enough soil to achieve ≈ 2. ASTM Type I grade of reagent water 6. 7. straight neck.05% methyl red). Add 500 mL of 50% NaOH solution to 8 L of RODI water. 7. 6. 6.S.9 Vials. Fill a labeled plastic vial with extract solution and cap. MA 6.2 Place labeled ET on extractor and connect to corresponding tared extraction tube (TETNH4Cl) with rubber tubing. 0. 6. remove RT from top of extractor and place in a clean container.10 Centrifuge. Centra. 2 N.1 Weigh 2. Dissolve 10 g of sodium hydroxide (NaOH) in 200 mL of RODI water. Extractor will turn off automatically. Discard the excess properly. Dilute to 9 L with RODI water. Carefully remove TETNH4Cl.7 Hydrochloric acid (HCl). Prepare one quality control check sample per 24 samples. weigh 1 g to the nearest mg. U. with bromcresol green-methyl red indicator (0.5 or 1g. Add 1341. 250 mL 5. Stir until dissolved. All soil should be wetted and no air bubbles.68 g of mercuric iodide (HgI2). Solution can be used immediately. Transfer NaOH solution to a 250-mL volumetric flask and slowly add K-Hg-I solution. Needham Heights. plastic 5.9 g of KCl reagent in 8 L RODI water.1 N.5 Potassium chloride solution. 95%.5. Solution should not contain a precipitate.6 Next day. 7. Dilute 167 mL of concentrated HCl in 20 L of RODI water.4 Secure reservoir tube (RT) to top of ET tube and let stand for 30 min. 7. Thermo IEC.075 % bromcresol green and 0.

repeat the ethanol wash and retest with Nessler's reagent. 7. If extracts are not to be determined immediately after collection. red to reddish brown precipitate is a positive test. Fill ET to the 20-mL mark with KCl solution and let stand for 30 min. If the test is positive.12 After the final ethanol wash. All soil should be wetted and no air bubbles. Steam Distillation: Setup. 7. 183 . Extract (≈ 45 min) the ethanol until 2 mL of this solution remains above the soil level. Discard the ethanol properly. Remove the TETNH4Cl.16 Secure RT to top of ET tube.18 Refer to the manufacturer’s manual for operation of the distillation unit. Test for NH4+ by using Nessler's reagent. A yellow. The following are only very general guidelines for instrument conditions. Do not let soil dry. Some samples may be cloudy and need to be filtered prior to analysis on the AA.14 Use a wash bottle to rinse inside of ET with 2 M KCl to remove any remaining ethanol or soil particles adhering to the ET. Set the extractor for 45 min. Turn off extractor. Secure RT to top of ET and let stand for 30 min. Turn off the extractor. 7. Turn off the extractor.17 Transfer the contents of the ETKCl to a 250-mL digestion tube. Do not let soil dry. 2 M KCl Rinse 7. 7. Removal of Excess Ammonium Chloride 7.13 Connect a new labeled extraction tube (ETKCl) with rubber tubing to ET on extractor.15 Extract at the 30-min extraction rate the KCl solution until 2 mL of this solution remains above soil level. Operation. Fill ET to the 20-mL mark with ethanol. 7. If extracts are not to be determined immediately after collection. Do not let soil dry. Repeat until a negative test is obtained. 7. collect a few drops of ethanol extract from the ET on a spot plate.8 Re-connect the TETNH4Cl with paired ET.analyses of extracted cations (procedure 4B1b1b1-4) on the atomic absorption (AA) spectrophotometer. Disconnect the TETNH4Cl from the ET and discard the ethanol properly.11 Re-connect the TETNH4Cl to the ET and add 55 mL of ethanol to the RT. then store samples at 4°C in plastic tubes. 7. Remove the ET and ETKCl from the extractor. leaving the tubing connected to the ET. Turn off the extractor.9 Extract at 30-min rate the ethanol solution until 2 mL of this solution remains above the soil level. Use a wash bottle to rinse the sides of the ET with ethanol to remove any remaining NH4Cl or soil particles adhering to the ET. and Analysis 7. All soil should be wetted and no air bubbles.10 Add 45 mL of ethanol to the RT. then store samples at 4°C. 7. Add 40 mL KCl solution to RT and set the extract for 45 min.

USDA. During the steam distillation. Circ. Mg2+.19 When using new reagents.C. one set per Kjeltec machine.F. M. References Holmgren.L. Magnesium. 1977.g. Ion Exchange and Extractable Cations (4B) Displacement after Washing. L. and Sodium (4B1a1b1-4) Air-dry or Field-Moist. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Close the safety door.S. The term extractable rather than exchangeable bases is used because 184 . Peech. 7. 11.. and J. <2-mm (4B1a1b1-4a-b1) 1.Program: Kjeldahl 1 Receiving Solution (boric acid): 30 mL Water: 0 mL Alkali (NaOH):20 mL Mode: Delay Time: 1 s Distillation: Volume Tube Drain: Yes 7. Potassium. Distillation and titration are performed automatically. Geschwender. NH4OAc.G.. L. boric acid. Methods of soil analysis for soil fertility investigations.. the mean reagent blank titer is automatically subtracted from the sample titer. Agric. 8.1 meq 100 g-1 (cmol (+) kg-1). and Na+) from the NH4OAc extraction (procedure 4B1a1) are generally assumed to be those exchangeable bases on the cation exchange sites of the soil.20 Record the normality of standardized acid. Alexander. G. reagent blanks are distilled in 2 sets of 6. A mechanically controlled variable rate leaching device.T. Juve. Each set of 6 is averaged and recorded on bench worksheet and manually set on each machine. 41:1207-1208. 10. Application The extractable bases (Ca2+.A. R. 7. Am. 25 pp. Calculations CEC = [Titer x N x 100 x R]/[Sample Weight (g)] where: CEC = Cation Exchange Capacity (meq 100 g-1) Titer = Titer of sample (mL) N = Normality of HCl titrant 100 = Conversion factor to 100-g basis R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 9. J.21 Connect the tube to the distillation unit. K+. Dean. Soil Sci. Reed. Report Report neutral salts CEC to the nearest 0. Record the titer in mL of titrant. and R. 757. e. 1947. pH 7 (4B1a) Automatic Extractor (4B1a1) Atomic Absorption Spectrophotometer (4B1a1b) Calcium.

NV 5.6 Ammonium acetate solution (NH4OAc). Do not use borosilicate tubes because of potential leaching of analytes.9 Peristaltic pump 6. Interferences There are four types of interferences (matrix.any additional source of soluble bases influences the results. ASTM Type I grade of reagent water 6. and Na+. Ca2+. Equipment 5.2 Atomic absorption spectrophotometer (AAS).2 Hydrochloric acid (HCl). CT. gas tight.4 Computer. serpentine (high Mg2+). with syringes 10000 and 1000 µL. MicroLab 500.. The analyte is measured by absorption of the light from a hollow cathode lamp. Restrict the use of concentrated HCl to a fume hood.4 NH4OH. 5. Perkin-Elmer Corp. and ionization) in the analyses of these cations. 6. reagent-grade. e. Many metal salts are extremely toxic and may be fatal if ingested.3 Autosampler. AAnalyst. 3. spectral. Standard laboratory equipment includes fire blankets and extinguishers for use when necessary. Norwalk.5 Glacial acetic acid. or natric material (high Na+). double-beam optical system. 2. with AA WinLab software. Follow standard laboratory procedures when handling compressed gases. free CaCO3 or gypsum. exercise special care. respectively. Avoid open flames and sparks. Deviation from this usual order signals that some factor or factors. and printer 5. AS-90. Add 1026 mL of glacial acetic acid (CH3COOH) to 15 L RODI water. 1982).0. concentrated 12 N 6. CT 5. Add 1224 mL of concentrated ammonium 185 . for sample dilution and sample changer 5. Norwalk. Carefully mix 1 part of concentrated HCl to 1 part RODI water. Summary of Method The NH4OAc extract from procedure 4B1a1 is diluted with an ionization suppressant (La2O3).7 Plastic test tubes. 15-mL.5 Single-stage regulator.1 Reverse osmosis deionized (RODI) water. 4. When preparing reagents. have altered the soil chemistry. An automatic sample changer is used to aspirate a series of samples. Follow the manufacturer's safety precautions when using the AAS. The abundance of these cations usually occurs in the sequence of Ca2+ > Mg2+ > K+ > Na+. 1:1 HCl:RODI. Mg2+.. depending upon the particular analyte selected..1 Electronic balance. chemical. Norwalk. The analytes are measured by an atomic absorption spectrophotometer (AAS). The NH4OAc extracted cations.5% 6.. 16 mm x 100. Safety Wear protective clothing and safety glasses.. The most doubtful cation extractions with this method are Ca2+ in the presence of free CaCO3 or gypsum and K+ in soils that are dominated by mica or vermiculite (Thomas.g. are reported in meq 100 g-1 soil or (cmol (+) kg-1) in procedures 4B1a1b1-4. The AAS converts absorption to analyte concentration.3 HCl. Data are automatically recorded by a microcomputer and printer. acetylene 5. 300. Hamilton Co. K+. Gas cylinders should be chained or bolted in an upright position. polyethylene 5. pH 7. ±1. These interferences vary in importance.8 Containers. Reagents 6. Reno.6 Digital diluter/dispenser. specific gravity 0.0-mg sensitivity 5. 1 N. 6 N. CT 5. Perkin-Elmer Corp. 99. Perkin-Elmer Corp. Thoroughly wash hands after handling these metal salts. Acetylene gas is highly flammable.90 6.

0 mg L-1 K. 0.5 mL Ca PSSS.11.12. High. 0.5 mL Mg PSSS. Invert to thoroughly mix. 0. 0.0 mL K PSSS. Allow to equilibrate to room temperature before use. and 200 mg L-1 Na 6. Store in polyethylene containers.0 mL Mg PSSS. Dilute to volume with RODI. While stirring.25 mg L-1 K. The NH4OAc solution is used for extraction of cations (procedure 4B1a1).5 mg L-1 Mg.0 mg L-1 Na 6. 6. Mix and adjust to pH 7. carefully add 272 mL of concentrated NH4OH.4 MCSS Very Low Standard: 1.0 using CH3COOH or NH4OH.025 mg L-1 Mg. 6. Dilute to final volume of 2-L with RODI water. Cooling the solution is necessary. 1000 mg L-1: Ca. 15 mg L-1 Mg.2 Medium Standard WSMSS: 60 mL Ca PSSS.0 with CH3COOH (typically. Very Low. Store in the refrigerator.0 N. Allow to stand one day to equilibrate to room temperature. Medium. 10 mg L-1 K. Prepare fresh weekly. and 50.5 Blank WSMSS = 0 mL of Ca. and 10. 6. Store in polyethylene container.0 mL K PSSS. 0.0 mL K PSSS.000 mg L-1.12. Wet 152. Dilute to 2 L with RODI water.5 mg L-1 Na 6.5 mg L-1 Mg.0 mg L-1 K.11.12.0. and Blank. and Na 186 .0 mL Na PSSS = 60 mg L-1 Ca.3 Low Standard WSMSS: 30 mL Ca PSSS. Low. ≈ 40 mL) or NH4OH and dilute with RODI water to 18 L. and 20 mg L-1 Na 6. Mg. Mg. high purity.0 mg L-1 Ca. Filter solution.5 Blank = 0 mg L-1 Ca. High. 0. 40 mg L-1 K.11. 20. 5. 6. 2000 mg L-1.25 mg L-1 Ca. 20 mg L-1 K. Prepare WSMSS as follows: 6.2 MCSS Medium Standard: 6. and 10 mg L-1 Na 6.5 mg L-1 K.75 mg L-1 Mg. Store in polyethylene container. Dilute to 2 L with RODI water.hydroxide (NH4OH). K.4 Low/Low Standard WSMSS: 12. K PSSS. Allow to stand one day to equilibrate to room temperature. and 5. 0. and 0. and 100 mg L-1 Na 6.0 mL Na PSSS = 180 mg L-1 Ca.11 Working stock mixed standards solution (WSMSS). and 100. 65. Mg PSSS. and Na. 0. K. 7. Dilute 1 part WSMSS with 19 parts of WLISS (1:20) dilution with resulting concentrations for MCSS as follows: 6. Cool.125 mL K PSSS. Mix 228 mL of glacial acetic acid in 1200 mL of RODI water. K.12.5 mL of SLISS with 1800 mL of RODI water (1:10).7 NH4OAc solution. 0. Low.0 mL Na PSSS = 25 mg L-1 Ca. 0. 5.0 mg L-1 Ca. 2.3 MCSS Low Standard: 3. 1. 6. 10 mg L-1 Mg.9 Working lanthanum ionization suppressant solution (WLISS).4 g lanthanum oxide (La2O3) with 100 mL RODI water. and 5. and Na PSSS. 2. and 10.0 mg L-1 Na 6. Mg. Dilute 61.25 mL Mg PSSS. and Blank. pH 7. In five 500-mL volumetric flasks.8 Stock lanthanum ionization suppressant solution (SLISS).1 High Standard WSMSS: 90 mL Ca PSSS. add 250 mL of 2 N NH4 OAc and the following designated amounts of Ca PSSS. Very Low.0 mL Na PSSS = 120 mg L-1 Ca. Slowly and cautiously add 500 mL of 6 N HCl to dissolve the La2O3. and Na PSSS.11. and 1.11. 2. 5 mg L-1 Mg.1 MCSS High Standard: 9.0 mg L-1 Ca. 10. 6.0 mg L-1 Na 6.25 mg L-1 Mg.10 Primary stock standards solutions (PSSS).125 K.12. Medium.12 Mixed calibration standard solutions (MCSS).5 mL Mg PSSS. Mix and adjust pH 7. Cool.

0 7.0 Mg 0. Burner Wavelength Slit Fuel/Oxidant (mg L-1) & angle (nm) (mm) (C2H2/Air) ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ Ca 9.6.5/10.5/10. the instrument is re-calibrated and QC re-analyzed. These analyte concentrations are converted to meq 100 g-1 as follows: Soil Analyte Concentration (meq 100 g-1) = [A x [(B1 . with 1 N NH4OAc followed by 1:20 dilution with WLISS. K. Calculations The instrument readings for analyte concentration are in mg L-1.0 10 cm @ 30° 589. if R2 <0. Very Low.01 unit.3 Refer to the manufacturer's manual for operation of the AAS. See reagents for preparation of the MCSS (High. The data system will then associate the concentrations with the instrument responses for each MCSS.5/10.1 The 10-mL syringe is for diluent (WLISS). Rejection criteria for MCSS. Procedure Dilution of Calibration Standards and Sample Extracts 7. 7.6%.4 Use the computer and printer to set instrument parameters and to collect and record instrument readings.8 Record analyte readings to 0.5 Calibrate the instrument by using the MCSS (High. Blank). AAS Calibration and Analysis 7.2 0. 7.B2)/B3] x C x R x 100]/[1000 x E x F] where: A = Analyte (Ca.5 0. 7. Set the digital diluter at a 1:20 dilution.2 Dispense the diluted sample solutions into test tubes which have been placed in the sample holders of the sample changer.6 If sample exceeds calibration standard. Acetylene gas.7 1. Dilute 1 part NH4OAc sample extract with 19 parts of WLISS (1:20 dilution). Low. If reading is not within 10%. etc. purity 99. Blank).5/10. Mg.0 0. The 1-mL syringe is for the MCSS and NH4OAc extracts (procedure 4B1a1). the sample is diluted 1:5.0 10 cm @ 0° 766. 8.99.0124 g cm-3) 187 Analyte . Na) concentration in extract (mg L-1) B1 = Weight of extraction syringe and extract (g) B2 = Weight of tared extraction syringe (g) B3 = Density of 1 N NH4OAc at 20°C (1. The following are only very general guidelines for instrument conditions for the various analytes. Low..13 6. 7. Very Low.75 10 cm @ 0° 285.0 10 cm @ 0° 422. AAS Set-up and Operation 7. Medium.7 Perform one quality control (QC) (Low Standard MCSS) every 12 samples. 1:100. 7.2 1.0 K 2. 1:20.14 Compressed air with water and oil traps.0 Na 10. Medium.7 1. Conc.7 0.7 1.

Report Report the extractable Ca2+. Deviation from this usual order signals that some factor or factors. Keeney (eds. 1982). or natric material (high Na+). In A. are reported in meq 100 g-1 soil or (cmol (+) kg-1) in procedures 4B1b1b1-4. 10. References Thomas.R. and Na+. ASA and SSSA. Agron. The AAS converts absorption to analyte concentration.H. and K+ to the nearest 0. 3.. have altered the soil chemistry.C = Dilution. 1982. Ca2+. Miller. Mg2+. free CaCO3 or gypsum. An automatic sample changer is used to aspirate a series of samples. The analytes are measured by an atomic absorption spectrophotometer (AAS). and D. 9. 159-165. Mg2+. respectively.L. WI. These interferences vary in importance. <2-mm (4B1b1b1-4a-b1) 1. Na+. The most doubtful cation extractions with this method are Ca2+ in the presence of free CaCO3 or gypsum and K+ in soils that are dominated by mica or vermiculite (Thomas.15 mg meq-1 Na+1 = 22. Exchangeable cations. Madison. The analyte is measured by absorption of the light from a hollow cathode lamp. Summary of Method The NH4Cl extract from procedure 4B1b1 is diluted with an ionization suppressant (La2O3). depending upon the 188 . Interferences There are four types of interferences (matrix.1 meq 100 g-1 (cmol (+) -1 kg ). p. Chemical and microbiological properties. K+. The abundance of these cations usually occurs in the sequence of Ca2+ > Mg2+ > K+ > Na+. G. Part 2. and ionization) in the analyses of these cations. Potassium. NH4Cl (4B1b) Automatic Extractor (4B1ba) Atomic Absorption Spectrophotometer (4B1b1b) Calcium. if performed 100 = Conversion factor (100-g basis) R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = mL L-1 E = Soil sample weight (g) F = Equivalent weight (mg meq-1) where: Ca+2 = 20. 2.g. Application The extractable bases (Ca2+. spectral. e.) Methods of soil analysis. and K+) from the NH4Cl extraction (procedure 4B1b1) are generally assumed to be those exchangeable bases on the cation exchange sites of the soil.10 mg meq-1 9. chemical.W. and Sodium (4B1b1b1-4) Air-dry or Field-Moist. The NH4Cl extracted cations. Data are automatically recorded by a microcomputer and printer. Mg2+. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Na+.99 mg meq-1 K+1 = 39. 11.04 mg meq-1 Mg+2 = 12. Magnesium. 2nd ed. Page. R. Monogr. Ion Exchange and Extractable Cations (4B) Displacement after Washing. serpentine (high Mg2+).

0 mL Mg PSSS. Dissolve 535 g of NH4Cl reagent in RODI water and dilute to 10 L. Store in polyethylene containers.0 mL K PSSS.5 Single-stage regulator.9 Peristaltic pump 6.7 Primary stock standards solutions (PSSS). Perkin-Elmer Corp. Follow standard laboratory procedures when handling compressed gases. and 100 mg L-1 Na 189 . Safety Wear protective clothing and safety glasses. Filter solution.4 g lanthanum oxide (La2O3) with 100 mL RODI water. with syringes 10000 and 1000 µL. 6. Equipment 5.7 Plastic test tubes. Cooling the solution is necessary. 40 mg L-1 K. CT 5. Reagents 6.2 High Standard WSMSS: 90 mL Ca PSSS. Medium. 1:1 HCl:RODI. Thoroughly wash hands after handling these metal salts. K PSSS.0 mL K PSSS. 5. and 200 mg L-1 Na Medium Standard WSMSS: 60 mL Ca PSSS. Avoid open flames and sparks. Allow to equilibrate to room temperature before use.1 Electronic balance. Store in polyethylene container. Acetylene gas is highly flammable. and 100.2 Atomic absorption spectrophotometer (AAS). high purity. and printer 5. Perkin-Elmer Corp.3 HCl.particular analyte selected. Invert to thoroughly mix.0-mg sensitivity 5. 1000 mg L-1: Ca. Norwalk. Low. and Na. 1 N. 300. gas tight.3 Autosampler. High. add 250 mL of 2 N NH4Cl and the following designated amounts of Ca PSSS. Dilute to 2 L with RODI water.8 Working stock mixed standards solution (WSMSS). 4. Norwalk. Prepare WSMSS as follows: 6. 65. ASTM Type I grade of reagent water 6. K. 10 mg L-1 Mg. 6. AAnalyst.0 mL Na PSSS = 120 mg L-1 Ca. with AA WinLab software. Do not use borosilicate tubes because of potential leaching of analytes. Dilute to volume with RODI.5 Stock lanthanum ionization suppressant solution (SLISS). 10. Restrict the use of concentrated HCl to a fume hood.8. In five 500-mL volumetric flasks. CT 5. Many metal salts are extremely toxic and may be fatal if ingested. 7.0 mL Na PSSS = 180 mg L-1 Ca. and Na PSSS. 15-mL. Prepare fresh weekly.5 mL Mg PSSS. and 50. Mg. Store in the refrigerator. and Blank. NV 5. Very Low.. Norwalk. 2000 mg L-1. 16 mm x 100. concentrated 12 N 6.6 Working lanthanum ionization suppressant solution (WLISS). Standard laboratory equipment includes fire blankets and extinguishers for use when necessary. Perkin-Elmer Corp. Reno.1 6. 6 N. acetylene 5. 5... Store in polyethylene container. 6.1 Reverse osmosis deionized (RODI) water. polyethylene 5. 6.2 Hydrochloric acid (HCl).4 Ammonium chloride solution (NH4Cl). for sample dilution and sample changer 5.8.4 Computer. MicroLab 500. Carefully mix 1 part of concentrated HCl to 1 part RODI water.. ±1. AS-90.8 Containers. Gas cylinders should be chained or bolted in an upright position.6 Digital diluter/dispenser. CT. Follow the manufacturer's safety precautions when using the AAS. 15 mg L-1 Mg. 20. 6.000 mg L-1. When preparing reagents.5 mL of SLISS with 1800 mL of RODI water (1:10). Dilute to final volume of 2-L with RODI water. Slowly and cautiously add 500 mL of 6 N HCl to dissolve the La2O3. exercise special care. 20 mg L-1 K. double-beam optical system. Hamilton Co. Mg PSSS. Wet 152. Dilute 61.

K.5/10. 1.6.5 mg L-1 Mg. 0.3 6.0 mL Na PSSS = 25 mg L-1 Ca. Analyte 190 . 6.0 mg L-1 Ca.0 mg L-1 Na MCSS Very Low Standard: 1.125 mL K PSSS. 7. and 1.1 6.10 Compressed air with water and oil traps. Very Low.75 mg L-1 Mg.75 10 cm @ 0° 285.5 0.0 Na 10.0 0.5 6.0 Mg 0.0 mL Na PSSS = 60 mg L-1 Ca. Dilute 1 part NH4Cl sample extract with 19 parts of WLISS (1:20 dilution).5 mg L-1 Mg.0 mg L-1 K.0 10 cm @ 0° 422. 5 mg L-1 Mg. 0.125 K. 0.5 mL Mg PSSS. and Na 6. Low. Procedure Dilution of Calibration Standards and Sample Extracts 7. 0.5 mg L-1 K. 0. and Blank. 0.0 10 cm @ 30° 589.4 6. and 5. and 10. Burner Wavelength Slit Fuel/Oxidant & angle (nm) (mm) (C2H2/Air) (mg L-1) ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ Ca 9.3 6. Medium.8. Conc.9.025 mg L-1 Mg. 10 mg L-1 K. Low.2 0.3 Refer to the manufacturer's manual for operation of the AAS. 2.9 Low Standard WSMSS: 30 mL Ca PSSS. 7. Blank). and 5.0 mL K PSSS.25 mg L-1 K.2 6. 0.8. 5. and 10 mg L-1 Na Blank WSMSS = 0 mL of Ca. and 0. Medium.5/10.2 1.11 Acetylene gas. See reagents for preparation of the MCSS (High.5/10.0 mg L-1 Na MCSS Low Standard: 3.5 mg L-1 Na Blank = 0 mg L-1 Ca.9. The 1-mL syringe is for the MCSS and NH4Cl extracts (procedure 4B1b). Mg.7 0.1 The 10-mL syringe is for diluent (WLISS).0 mg L-1 Ca. Dilute 1 part WSMSS with 19 parts of WLISS (1:20) dilution with resulting concentrations for MCSS as follows: MCSS High Standard: 9. High. The following are only very general guidelines for instrument conditions for the various analytes.0 mg L-1 Ca. Mg.0 mg L-1 Na MCSS Medium Standard: 6.0 7.7 1.7 1.7 1. and Na PSSS Mixed calibration standard solutions (MCSS). Set the digital diluter at a 1:20 dilution.5 mL Ca PSSS. Very Low.25 mg L-1 Ca.4 Use the computer and printer to set instrument parameters and to collect and record instrument readings.4 6.9.9.25 mL Mg PSSS. and 20 mg L-1 Na Low/Low Standard WSMSS: 12. 0.25 mg L-1 Mg.0 10 cm @ 0° 766. purity 99.0 mg L-1 K. and 10. K.9.6%. 2. AAS Set-up and Operation 7.8.0 K 2.5/10.2 Dispense the diluted sample solutions into test tubes which have been placed in the sample holders of the sample changer. 0.5 6. 0.

Rejection criteria for MCSS. K+. Na) concentration in extract (mg L-1) B1 = Weight of extraction syringe and extract (g) B2 = Weight of tared extraction syringe (g) B3 = Density of 1 N NH4Cl at 20°C (1. These analyte concentrations are converted to meq 100 g-1 as follows: Soil Analyte Concentration (meq 100 g-1) = [A x [(B1 . 1:100. the instrument is re-calibrated and QC re-analyzed.1 meq 100 g-1 (cmol (+) -1 kg ). with 1 N NH4Cl followed by 1:20 dilution with WLISS. the sample is diluted 1:5.7 Perform one quality control (QC) (Low Standard MCSS) every 12 samples.AAS Calibration and Analysis 7. Mg. K. Part 2. 7. 159-165.10 mg meq-1 9. 1:20. ASA and SSSA. 7. WI. 11. 9. References Thomas. etc. In A.99. Miller. Report Report the extractable Ca2+. and D.8 Record analyte readings to 0. Very Low.01 unit. Monogr. 191 .15 mg meq-1 Na+1 = 22. 1982. Page. and Na+ to the nearest 0.B2)/B3] x C x R x 100]/[1000 x E x F] where: A = Analyte (Ca.. Exchangeable cations.W. p. Mg2+. Keeney (eds. 10. Agron. if R2 <0. Calculations The instrument readings for analyte concentration are in mg L-1. 2nd ed. Medium. 7. if performed 100 = Conversion factor (100-g basis) R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = mL L-1 E = Soil sample weight (g) F = Equivalent weight (mg meq-1) where: Ca+2 = 20.5 Calibrate the instrument by using the MCSS (High. Chemical and microbiological properties.0166 g cm-3) C = Dilution. 8. R.L. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. The data system will then associate the concentrations with the instrument responses for each MCSS.R.99 mg meq-1 K+1 = 39.) Methods of soil analysis.6 If sample exceeds calibration standard.H. Madison. Low. G. Blank). If reading is not within 10%.04 mg meq-1 Mg+2 = 12.

Although other pH values are valid for some types of soils.BaCl2-Triethanolamine. 1977). Metrohm Ltd. Metrohm Ltd. Use the safety showers and eyewash stations to dilute spilled acids and bases. Interferences No significant interferences are known to exist with this method. plastic. with control unit.. and gloves) and eye protection (face shields. 24 place.45-µm filter 5.2 Extraction (4B2) Automatic Extractor (4B2a) Automatic Titrator (4B2a1) Back Titration with HCl (4B2a1a) Extractable Acidity (4B2a1a1) Air-Dry or Field-Moist. 5. <2 mm (4B2a1a1a-b1) 1. Extractable acidity may be measured at any pH. Inc.4 Titration beakers.. especially concentrated acids and bases.. 2. sleeve guards. goggles. the buffer capacity of the BaCl2-TEA solution may be exceeded. pH 8.9 Tubes. Brinkmann Instruments. A pH of 8. Metrohm Ltd.7 Computer. 60-mL. and dispenser. 3. Thoroughly wash hands after handling reagents. SAMPLETEX. plastic. aprons. Metrohm Ltd. (1/8 ID x 1/16 OD x 1 in) for connecting syringe barrels 192 .2 also closely corresponds to the pH of complete neutralization of soil hydroxy-Al compounds.8 Titration beakers. with Titrino Workcell software.2. pH 8. 5..5 Automatic titrator. 3. However. and a variety of methods have been used to measure it. Brinkmann Instruments Inc..2 because it approximates the calculated pH of a soil containing free CaCO3 in equilibrium with the normal CO2 content (0.6 Combination pH-reference electrode. NE 5. Safety Wear protective clothing (coats. The Soil Conservation Service adopted a pH of 8. Metrohom Ltd.2 ID x 6.4 mm.2 method (4B2a1a1) may not always accurately reflect the nature of soils as they occur in the environment.. and the BaCl2-TEA. or safety glasses) when preparing reagents. Lincoln. Extractable acidity is reported in meq 100 g-1 soil or (cmol (+) kg-1). Use sodium bicarbonate and water to neutralize and dilute spilled acids. 4.2 and includes all the acidity generated by replacement of the H and Al from permanent and pH dependent exchange sites. Inc.0-mg sensitivity 5. The difference between a blank and the extract is the extractable acidity.2 Mechanical vacuum extractor. 250-mL. MAVCO Industries. Equipment 5. Inc.10 Rubber tubing. Dispense concentrated acids in a fume hood. Brinkmann Instruments.3 Pipettes or dispenser. polypropylene. Brinkmann Instruments. with 0. adjustable volume to 20 mL 5. for some very acid soils. ±1.. and printer 5.1 Electronic balance. Brinkmann Instruments Inc.4 OD x 25. sample changer. Application The extractable acidity is the acidity released from the soil by a barium chloridetriethanolamine (BaCl2-TEA) solution buffered at pH 8. 5. for extraction. Sample is allowed to stand overnight and extracted using a mechanical vacuum extractor (Holmgren et al. 5.03%) of the atmosphere. 250-mL. Summary of Method A soil sample is leached with a BaCl2-TEA solution buffered at pH 8. this method has become a standard reference to which other methods are compared. The extract is back-titrated with HCl. 5.

6 Replacement solution. 7. Mix two solutions and bring to nearly 16-L volume with RODI water. During the addition.5 g of air-dry soil. 7.5. Prepare at least one reagent blank (no sample in syringe) and one quality control check sample per 24 samples. 7. Titration of BaCl2-TEA Extract 7. Dissolve 977 g of BaCl2·2H2O in 8 L of RODI water.2 Place labeled ET on extractor and connect to corresponding extraction tube (ETAcidity) with rubber tubing. 7.0-cm height above the sample.2]. 7. Dissolve 977 g of BaCl2·2H2O in 8 L of RODI water.6 Use a dispenser to add 20. Extract at 30-min rate until all the solution has been drawn through the sample. The solution is ready to be titrated. Dilute 193 mL of concentrated HCl to 16-L volume with RODI water. Extract the sample at 30min rate.13 N.00 mL of BaCl2-TEA solution to the ET1.18.5 N BaCl2.7 Add a second 20. Leave rubber tubing on the ET1. If sample is moist. Procedure Extraction of Acidity 7.00-mL aliquot of replacement solution to ET1. Reagents 6.6. 7. Extract solution to a 0.00 and 4. 0. 0. 12 N 6. wash the sides of the tube and wet the sample.4 Let ET1 tube stand overnight. 6. Adjust to pH 8.5 g of <2-mm or fine-grind. pH 8. Set-up the automatic titrator to set end point titration mode.8 Carefully remove ETAcidity.10 Add 100 mL of RO water to the beaker.4 HCl. Add 80 mL of buffer solution and dilute 16-L volume with RODI water.to 1. 7. swirling.11 Refer to manufacturer's manual for operation of the automatic titrator. air-dry soil to the nearest mg and place in a labeled extraction (ET1).2 N Triethanolamine (TEA).5 Set the extractor for a 30-min extraction rate. Bring to 16-L volume with RODI water. weigh enough soil to achieve ≈ 2.1 Reverse osmosis deionized (RODI) water 6. Dissolve 477 g of TEA in 4 L of RODI water.5 Buffer solution [0.00 pH buffers.00 mL of replacement solution to ET1. concentrated.2 with ≈ 33 mL of concentrated HCl or barium hydroxide.2 Reverse osmosis (RO) water 6. For organic soils. standardized. 7. 7.12 Calibrate automatic titrator with with 9.3 Hydrochloric acid (HCl).3 Use a dispenser to add 20. pulling the solution almost completely through the sample. 7. 7. 7.9 Transfer the BaCl2-TEA extract from the ETAcidity to a 250-mL polyethylene titration beaker.1 Weigh 2. or stirring may be required to wet the sample. Do not allow the sample to become dry. Turn off the extractor. shaking. The "Set" pH parameters are listed as follows: 193 . 6.

3 units lower than the average pH of the blanks.01 mL.4 mV s-1 25°C 75 mL 7.. The Soil Conservation Service adopted a pH of 8. re-run using a 0.14 Record the titer to the nearest 0. Soil Sci.2 because it approximates the calculated pH of a soil containing free CaCO3 in equilibrium with the normal CO2 content (0. References Holmgren. and R. Calculations Extractable acidity (meq 100 g-1) = {[(B – T) x N x R]/C} x 100 where: B = Average reagent blank titer (mL) T = Sample titer (mL) N = Normality of HCl C = Sample Weight (g) 100 = Conversion factor (100-g basis) R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 9.S. J. Am. and the 194 . Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 11. Record the normality of the HCl solution. Report Report extractable acidity to the nearest 0. Average the titer of the reagent blanks and record. Geschwender.5 units 0. 10. and a variety of methods have been used to measure it.4 mV s-1 10 s 0.2 Extraction (4B2) Centrifuge (4B2b) Automatic Titrator (4B2b1) Back Titration with HCl (4B2b1a) Extractable Acidity (4B2b1a1) Air-Dry or Field-Moist. 41:1207-1208. 8. A pH of 8.2 also closely corresponds to the pH of complete neutralization of soil hydroxy-Al compounds. Application The extractable acidity is the acidity released from the soil by a barium chloridetriethanolamine (BaCl2-TEA) solution buffered at pH 8.13 If pre-titration pH is 0. 1977.25 g sample 7.Parameter Ep1 Dyn change pH Drift Time delay Drift Temp Stop Volume Value pH 4.03%) of the atmosphere. R.L. Juve. Extractable acidity may be measured at any pH.G.2 and includes all the acidity generated by replacement of the H and Al from permanent and pH dependent exchange sites.C. BaCl2-Triethanolamine. A mechanically controlled variable rate leaching device. <2 mm (4B2b1a1a-b1) 1.60 1.1 meq 100 g-1 (cmol (+) kg-1). G. Although other pH values are valid for some types of soils. pH 8.

4. The extract is back-titrated with HCl. standardized. 3. 6.4 Buffer solution (0. Dilute 193 mL of concentrated HCl to 16-L volume with RODI water. sleeve guards. Sample is allowed to stand overnight. Equipment 5. Brinkmann Instruments. with control unit. Bring to 16-L volume with RODI water. 5. Summary of Method A soil sample is leached with a BaCl2-TEA solution buffered at pH 8. 50-mL. Metrohm Ltd. weigh enough soil to achieve ≈ 5 g of air-dry soil. Mix two solutions and bring to nearly 16-L volume with RODI water. Brinkmann Instruments Inc. 0.3 HCl.2.. Analog. 250-mL. mini. 5. and centrifuged. Reagents 6. Prepare at least two reagent blanks (no sample in tube) and one quality control check sample per 21 samples.0-mg sensitivity 5.2 N Triethanolamine (TEA). Metrohm Ltd. Brinkmann Instruments. If sample is moist. ±1.2 method (4B2b1a1) may not always accurately reflect the nature of soils as they occur in the environment. Add 80 mL of buffer solution and dilute to 16-L volume with RODI water. 12 N 6. and dispenser. shaken. 7. 5.1 Weigh 5 g of <2-mm or fine-grind. MA 5. Thoroughly wash hands after handling reagents.2 Hydrochloric acid (HCl). Thermo IEC. VRW Scientific Products 5.3 Vortexer.5 Centrifuge. aprons. Brinkmann Instruments.9 Computer.2 Pipettes or dispenser.5 Replacement solution. sample changer.8 Combination pH-reference electrode.. pH 8. with Titrino Workcell software. air-dry soil to the nearest mg and place in a centrifuge tube. polyethylene 5.2 with ≈ 33 mL of concentrated HCl or barium hydroxide. Dissolve 977 g of BaCl2·2H2O in 8 L of RODI water. this method has become a standard reference to which other methods are compared.. Extractable acidity is reported in meq 100 g-1 soil or (cmol (+) kg-1). Metrohm Ltd. GP-8. Needham Heights. Adjust to pH 8. Inc. 5. plastic.. Dissolve 477 g of TEA in 4 L of RODI water. especially concentrated acids and bases. Interferences No significant interferences are known to exist with this method. Procedure Extraction of Acidity 7. The difference between a blank and the extract is the extractable acidity.13 N. Safety Wear protective clothing (coats. Centra.BaCl2-TEA. Dispense concentrated acids in a fume hood. adjustable volume to 40 mL 5. goggles. Inc.6 Titration beakers.5 N BaCl2. Use sodium bicarbonate and water to neutralize and dilute spilled acids. pH 8.1 Electronic balance. the buffer capacity of the BaCl2-TEA solution may be exceeded. Dissolve 977 g of BaCl2·2H2O in 8 L of RODI water.2). for some very acid soils.1 Reverse osmosis deionized (RODI) water 6. and printer 6. However. Metrohom Ltd. 6. 0. 2. and gloves) and eye protection (face shields. Use the safety showers and eyewash stations to dilute spilled acids and bases. concentrated. Inc.4 Centrifuge tubes. or safety glasses) when preparing reagents.7 Automatic titrator. 195 ..

5-g sample. 7.4 – 7.11 Refer to the manufacturer’s manual for operation of the automatic titrator.00 and 4. 7. 7.3 Place tube rack on its side and gently shake to stratify the mixture lengthwise along the tube.12 Calibrate the titrator meter with 9.01 mL. 7.8 Repeat Sections 7. 7.4 mV s-1 25°C 75 mL 7.18. Allow to stand overnight on its side.00 pH buffers.2 Add 40.4 – 7.5. Calculations Extractable acidity (meq 100 g-1) = {[(B – T) x N x R]/C} x 100 where: B = Average reagent blank titer (mL) T = Sample titer (mL) N = Normality of HCl C = Sample Weight (g) 100 = Conversion factor (100-g basis) R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 196 .60 1. 7.5 Decant extract into numbered titration beakers. 7. Titration of BaCl2-TEA Extract 7.4 mV s-1 10 s 0.00 mL of BaCl2-TEA solution to sample. 7. 7. The “Set” pH parameters are listed as follows: Parameter Ep1 Dyn change pH Drift Time delay Drift Temp Stop Volume Value pH 4.13 If pre-titration pH is 0.14 Record the titer to the nearest 0. Record the normality of the HCl solution. Total volume in titration beaker should be ≈ 120 mL. Cap the tube and shake to ensure all soil is wetted. Manually shake. Set-up the automatic titrator to sent end point mode.4 Centrifuge sample at 2000 rpm for 5 min.9 Repeat Sections 7. Average the titer of the reagent blanks and record.5 units 0. Place tube in a rack.7.3 units lower than the average pH of the blanks.10 Place titration beakers on automatic sample changer.7. 8. re-run using a 0. 7.7 Cap tube and use a vortexer to loosen soil. 7.6 Add 40 mL of replacement solution to sample.

9. Report Report extractable acidity to the nearest 0.1 meq 100 g-1 (cmol (+) kg-1). 10. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 11. References Holmgren, G.G.S., R.L. Juve, and R.C. Geschwender. 1977. A mechanically controlled variable rate leaching device. Soil Sci. Am. J. 41:1207-1208.

1 N KCl Extraction (4B3) Automatic Extractor (4B3a) Inductively Coupled Plasma Atomic Emission Spectrophotometer (4B3a1) Radial Mode (4B3a1a) Al and Mn (4B3a1a1-2) Air-Dry or Field-Moist, <2 mm (4B3a1a1-2a-b1)
1. Application The Al extracted by 1 N KCl approximates exchangeable Al and is a measure of the "active" acidity present in soils with a 1:1 water pH <5.5. Above pH 5.5, precipitation of Al occurs during analysis. This method does not measure the acidity component of hydronium ions (H3O+). If Al is present in measurable amounts, the hydronium is a minor component of the active acidity. Because the 1 N KCl extractant is an unbuffered salt and usually affects the soil pH one unit or less, the extraction is determined at or near the soil pH. The KCl extractable Al is related to the immediate lime requirement and existing CEC of the soil. The "potential" acidity is better measured by the BaCl2-TEA method (procedure 4B2a1a1) (Thomas, 1982). The use of NH4Cl in place of KCl is useful where a single exttractant for exchangeable bases and Al is preferred since NH4+ is as effective as K at displacing Al (Lee et al., 1985: Bertsch and Bloom, 1996). The Mn extracted by 1 N KCl approximates exchangeable Mn. Mn is an essential trace metal for plant nutrition. Soil analysis for Mn is of interest from both deficiency and toxicity perspectives (Gambrell, 1996). 2. Summary of Method In this procedure (4B3a1a1-2), a soil sample is leached with 1 N KCl using the mechanical vacuum extractor (Holmgren et al., 1977). The extract is weighed. The KCl extracted solution is diluted with 0.5 N HCl. The analytes are measured by inductively coupled plasma atomic emission spectrophotometer (ICP-AES). The Mn and Al are reported in mg kg-1 and cmol(+) kg-1, respectively, in the soil. 3. Interferences There are four types of interferences (matrix, spectral, chemical, and ionization) in the ICP-AES analyses of these cations. These interferences vary in importance, depending upon the particular analyte selected. The soil:extractant ratio must remain constant. A soil:extractant ratio of 1:10 (w:v) for batch procedures is most commonly used. Using a leaching technique, a 1:20 (w:v) ratio gives comparable results. If the sample size is changed, the amount of extractable Al is changed. No other significant interferences have been identified for this procedure. 4. Safety Wear protective clothing and eye protection. When preparing reagents, exercise special care. Follow standard laboratory practices when handling compressed gases. Gas cylinders should be chained or bolted in an upright position. Follow the manufacturer's safety precautions when using the ICP-AES.

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5. Equipment 5.1 Electronic balance, ±1.0-mg sensitivity 5.2 Mechanical vacuum extractor, 24-place, SAMPLETEX, MAVCO Industries, Lincoln, NE (See Fig.1 - 2, procedure 4B1a1a1a1) 5.3 Tubes, 60-mL, polypropylene, for extraction (0.45-µm filter), reservoir, and tared extraction tubes 5.4 Rubber tubing, 3.2 ID x 1.6 OD x 6.4 mm (1/8 ID x 1/16 OD x 1 in) for connecting syringe barrels. 5.5 Dispenser, 10 mL 5.6 Inductively coupled plasma atomic emission spectrophotometer (ICP-AES), Perkin-Elmer Optima 4300 Dual View (DV), Perkin-Elmer Corp., Norwalk, CT. 5.7 Scott spray chamber with end cap and gem cone x-flow nebulizer 5.8 Torch coupler at -3 position 5.9 RF generator, floor mounted power unit, 45 MHz free running, Perkin-Elmer Corp.,Norwalk, CT. 5.10 Computer, with WinLab software ver. 4.1, Perkin-Elmer Corp., Norwalk, CT, and printer 5.11 Recirculating chiller, Neslab, CFT Series 5.12 Autosampler, AS-93, Perkin-Elmer Corp., Norwalk, CT. 5.13 Single-stage regulator, high-purity, high-flow, argon 5.14 Pipettes, electronic digital, 10000 and 1000 µL, with tips 10000 and 1000 µL 5.15 Test tubes, 15-mL, 16 mm x 100, for sample dilution and sample changer 5.16 Containers, polyethylene 5.17 Vortexer, mini, MV1, VWR Scientific Products 5.18 Disposable tubes, glass, 10 mL 6. Reagents 6.1 Reverse osmosis deionized (RODI) water, ASTM Type I grade of reagent water 6.2 Potassium chloride solution (KCl), 1.0 N. Dissolve 1341.9 g of KCl reagent in 16 L RODI water. Allow solution to equilibrate to room temperature. Dilute to 18 L with RODI water. Use 1.0 N KCl for Al and Mn extraction. 6.3 Potassium chloride solution (KCl), 2.0 N. Dissolve 298.2 g of KCl reagent in 1.5 L RODI water. Allow solution to equilibrate to room temperature. Dilute to 2 L with RODI water. Use 2.0 N KCl for standards. 6.4 HCl, 0.5 N. In a 1-L volumetric, add 41.67 mL concentrated HCl 12 N to RODI water and dilute to volume with RODI water. 6.5 Primary Stock Standard Solution (PSSS), high purity, 1000 mg L-1: Al and Mn. 6.6 Mixed calibration standards solution (MCSS) for Al and Mn as follows: 6.6.1 MCSS High: In 1-L volumetric flask, mix 40 mL Al PSSS, 5 mL Mn PSSS, 14.91 g KCl, and 33.3 mL concentrated HCl and dilute to volume with RODI water. Invert to thoroughly mix. Final concentration = 40 and 5 mg L-1 Al and Mn, respectively. Store in polyethylene containers. Prepare fresh weekly. Store in the refrigerator. Allow to equilibrate to room temperature before use. 6.6.2 MCSS Medium: In 1-L volumetric flask, mix 20 mL Al PSSS, 2 mL Mn PSSS, 14.91 g KCl, and 33.3 mL concentrated HCl and dilute to volume with RODI water. Invert to thoroughly mix. Final concentration = 20 and 2 mg L-1 Al and Mn, respectively. Store in polyethylene containers. Prepare fresh weekly. Store in the refrigerator. Allow to equilibrate to room temperature before use. 6.6.3 MCSS Low: In 1-L volumetric flask, mix 10 mL Al PSSS, 1mL Mn PSSS, 14.91 g KCl and 33.3 mL concentrated HCl and dilute to volume with RODI water. Invert to thoroughly mix. Final concentration = 10 and 1 mg L-1 Al and Mn, respectively. Store in

198

polyethylene containers. Prepare fresh weekly. Store in the refrigerator. Allow to equilibrate to room temperature before use. 6.6.4 MCSS Blank: In 1-L volumetric flask, mix 500 RODI water, 33.3 mL concentrated HCl, and 14.91 g KCl and dilute to volume with RODI water. Invert to thoroughly mix. Store in polyethylene containers. Prepare fresh weekly. Store in the refrigerator. Allow to equilibrate to room temperature before use. 6.7 Argon gas, purity 99.9% 7. Procedure

Extraction of Al and Mn 7.1 Weigh 2.5 g of <2-mm, air-dry soil to the nearest mg and place in a labeled extraction tube (ET). If sample is fine-grind, weigh 1.25 g to the nearest mg. If sample is moist, weigh enough soil to achieve ≈ 2.5 or 1.25 g, respectively, of air-dry soil. Prepare one quality control sample per 24 samples. 7.2 Place labeled ET on extractor and connect to corresponding tared extraction tube (TETKCl) with rubber tubing. 7.3 Use a dispenser and add 10 mL of 1 N KCl to the ET. All soil should be wetted and no air bubbles. Shaking, swirling, or stirring may be required to wet organic samples. 7.4 Secure reservoir tube (RT) to top of ET tube and let stand for 30 min. Extract at 30-min rate the KCl soultion until 2 mL of this solution remains above soil level. Turn off extractor. Do not let soil dry. 7.5 Add 45 mL of KCl solution to the RT if sample weight is 2.5 g. Add 17.5 mL of KCl solution to the RT if sample weight is 1.25 g. Set extractor for 45-min extraction. Extractor will turn off automatically. 7.6 Remove RT from top of extractor. Carefully remove TETKCl. Leave the rubber tubing on the ET. Weigh each TETKCl containing the KCl extract to the nearest mg. 7.7 Mix the extract in each TETKCl by manually shaking. Fill a disposable tube with extract solution and discard the excess properly. This solution is reserved for extractable Al and Mn analyses. If extracts are not be determined immediately after collection, then store samples at 4°C. Dilution of Extracts 7.8 Dilute samples (1:5 dilution). Dilute 1 part KCl sample extract with 4 parts 0.5 N HCl. Use Vortexer to mix sample. 7.9 Place the diluted sample solutions into test tubes and place in the sample holder of the sample changer. ICP-AES Set-up and Operation 7.10 Refer to the manufacturer's manual for operation of the ICP-AES. The following parameters are only very general guidelines for instrument conditions for the analytes.

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Parameter View Wavelength Al Wavelength Mn Background Correction Gas Flow Torch Gas Auxiliary Gas Flow Nebulizer Flow Power Peristaltic Pump Sample Flow Rate Flush Rate Relaxation Time Pump Tubing Type

Value Radial 396.153 257.610 “ON” 2-Point 15.0 L min-1 0.5 L min-1 0.80 L min-1 1450 W 1.25 mL min-1 35 s 15 s Solvflex black/black, 2-stop, 0.030 ID for sample Solvflex red/red, 2-stop, 0.045 ID for rinse

ICP-AES Calibration and Analysis 7.11 Calibrate the instrument by using the MCSS. The data system will then associate the concentrations with the instrument responses for each MCSS. Rejection criteria for MCSS, if R2 <0.99. 7.12 If sample exceeds calibration standard, the sample is diluted 1:10 with 1 N KCl followed by 1:5 0.5 HCl. 7.13 Perform one quality control (QC) (Low MCSS) every 12 samples. If reading is not within 10%, the instrument is re-calibrated and QC re-analyzed. 7.14 Record analyte readings to 0.01 mg L-1. 8. Calculations The instrument readings are the analyte concentration (mg L-1 Al and Mn). Use these values to calculate the analyte concentration in meq 100 g-1 and mg kg-1 for Al and Mn, respectively. 8.1 Al (meq 100 g-1) = [A x [(B1 - B2)/B3] x C1 x C2 x R x 100]/[1000 x E x F] where: A = Al concentration in extract (mg L-1) B1 = Weight of extraction syringe and extract (g) B2 = Weight of tared extraction syringe (g) B3 = Density of 1 N KCl at 20°C (1.0412 g mL-1) C1 = Dilution, required (1:5) C2 = Dilution, if performed 100 = Conversion factor (100-g basis) R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = mL L-1 E = Soil sample weight (g) F = Equivalent weight (Al3+ = 8.99 mg meq-1) 8.2 Mn (mg kg-1) = [A x [(B1 - B2)/B3] x C1 x C2 x R x 1000]/[1000 x E]

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where: A = Mn concentration in extract (mg L-1) B1 = Weight of extraction syringe and extract (g) B2 = Weight of tared extraction syringe (g) B3 = Density of 1 N KCl at 20°C (1.0412 g mL-1) C1 = Dilution ratio, required (1:5) C2 = Dilution ratio, if needed R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = Conversion factor in numerator to kg-basis 1000 = Factor in denominator (mL L-1) E = Soil sample weight (g) 9. Report Report KCl extractable Al to the nearest 0.1 meq 100 g-1 (cmol(+) kg-1) and Mn to the nearest mg kg-1. 10. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 11. References Gambrell, R. P. 1996. Manganese. p. 665-682. In D.L. Sparks (ed.) Methods of soil Analysis . Part 3. Chemical Methods. . Soil Sci. Am. Book Series No. 5. ASA and SSA, Madison WI. Holmgren, George G.S., R.L. Juve, and R.C. Geschwender. 1977. A mechanically controlled variable rate leaching device. Soil Sci. Soc. Am. J. 41:1207-1208. Bertsch, P.M., and P.R. Bloom. 1996. Aluminum. p. 517-530. In D.L. Sparks (ed.) Methods of soil analysis. Part 3. Chemical methods. No. 5. ASA and SSSA, Madison, WI. Lee, R., B.W. Bache, M.J. Wilson, and G.S. Sharp. 1985. Aluminum release in relation to the determination of cation exchange capacity of some podzolized New Zealand soils. J. Soil Sci. 36:239-253. Thomas, G.W. 1982. Exchangeable cations. p. 159-165. In A. Klute (ed.) Methods of soil analysis. Part 2. Chemical and microbiological properties. 2nd ed. Agron. Monogr. 9. ASA and SSSA, Madison, WI.

Ratios and Estimates Related to Ion Exchange and Extractable Cations (4B4) Sum of Extractable Bases (4B4a) Sum of Extractable Bases by NH4OAc, pH 7 (4B4a1) Sum of Extractable Bases by NH4OAc, pH 7, Calculated (4B4a1a)
Sum the NH4OAc, pH 7 extractable bases (Ca2+, Mg2+, K+, and Na+) (4B4a1a) obtained by procedure 4B1a1 and analyzed in procedures 4B1a1b1-4, respectively. This value is reported as meq 100 g-1 (cmol (+) kg-1).

Ratios and Estimates Related to Ion Exchange and Extractable Cations (4B4) Sum of Extractable Bases (4B4a) Sum of Extractable Bases by NH4Cl (4B4a2) Sum of Extractable Bases by NH4Cl, Calculated (4B4a2a)
Sum the NH4Cl extractable bases (Ca2+, Mg2+, K+, and Na+) (4B4a2a) obtained by procedure 4B1b1 and analyzed in procedures 4B1b1b1-4, respectively. This value is reported as meq 100 g-1 (cmol (+) kg-1).
201

Ratios and Estimates Related to Ion Exchange and Extractable Cations (4B4) Cation Exchange Capacity (CEC) (4B4b) CEC-8.2 (Sum of Cations) (4B4b1) CEC-8.2, Calculated (4B4b1a) CEC-8.2, Not Calculated (4B4b1b)
Calculate the CEC-8.2 (4B4b1a) by adding the sum of the NH4OAc extractable bases (4B4a1) plus the BaCl2-TEA extractable acidity (4B2a1a1 or 4B2b1a1). This value is reported as meq 100 g-1 (cmol (+) kg-1). Cation summation is the basis for this procedure. The CEC-8.2 minus the CEC-7 is considered the pH dependent charge from pH 7.0 to pH 8.2. The CEC-8.2 is not calculated (4B4b1b) if significant quantities of soluble salts or carbonates are present in the soil. CEC-8.2 is calculated as follows: CEC-8.2 = NH4OAc Bases + BaCl2-TEA Acidity

Ratios and Estimates Related to Ion Exchange and Extractable Cations (4B4) Cation Exchange Capacity (CEC) (4B4b) Effective Cation Exchange Capacity (ECEC) (4B4b2) Sum of NH4OAc Extractable Bases + 1 N KCl Extractable Aluminum, Calculated (4B4b2a) Sum of NH4OAc Extractable Bases + 1 N KCl Extractable Aluminum, Not Calculated (4B4b2b)
Calculate the ECEC (4B4b2a) by adding the sum of the NH4OAc extractable bases (4B4a1) plus the 1 N KCl extractable Al (4B3a1a1). This value is reported as meq 100 g-1 (cmol (+) kg-1). The ECEC is not calculated (4B4b2b) if significant quantities of soluble salts or carbonates are present in the soil. ECEC by NH4OAc extractable bases and 1 N KCl Al is calculated as follows: ECEC = NH4OAc Bases + 1 N KCl Al

Ratios and Estimates Related to Ion Exchange and Extractable Cations (4B4) Base Saturation (4B4c) Base Saturation by NH4OAc, pH 7 (CEC-7) (4B4c1) Base Saturation by CEC-7, Calculated (4B4c1a) Base Saturation by CEC-7, Set to 100% (4B4c1b)
Calculate the base saturation (4B4c1a) by dividing by the sum of NH4OAc extractatable (4B4a1) bases by CEC-7 (4B1a1a1a1) and multiplying by 100. This value is reported as meq 100 g-1 (cmol (+) kg-1). If a soil has significant quantities of soluble salts or carbonates, this value is set to 100% (4B4c1b). In soil taxonomy, base saturation determined by CEC-7 is used in mollic, umbric, and eutro-dystro criteria (Soil Survey Staff, 1999). Calculate base saturation by CEC-7 as follows: Base Saturation (%) = (NH4OAc Bases/CEC-7) x 100

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References Soil Survey Staff. 1999. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys, USDA-NRCS Agric. Handb. 436. 2nd ed. U.S. Govt. Print. Office, Washington, DC.

Ratios and Estimates Related to Ion Exchange and Extractable Cations (4B4) Base Saturation (4B4c) Base Saturation by NH4Cl (4B4c2) Base Saturation by NH4Cl, Calculated (4B4c2a) Base Saturation by NH4Cl, Set to 100% (4B4c2b)
Calculate the base saturation (4B4c2a) by dividing the sum of the NH4Cl extractatable (4B4a2) bases by CEC by NH4Cl (4B1b1a1a1) and multiplying by 100. This value is reported as meq 100 g-1 or cmol (+) kg-1. In soil taxonomy, base saturation determined by the sum of cations (CEC-8.2) is used in most alfic-ultic criteria (Soil Survey Staff, 1999). If a soil has significant quantities of soluble salts or carbonates, this value is set to 100% (4B4c2b). Calculate base saturation by CEC-7 as follows: Base Saturation (%) = (NH4Cl Bases/CEC by NH4Cl) x 100

Ratios and Estimates Related to Ion Exchange and Extractable Cations (4B4) Base Saturation (4B4c) Base Saturation by CEC-8.2 (Sum of Cations) (4B4c3) Base Saturation by CEC-8.2, Calculated (4B4c3a) Base Saturation by CEC-8.2, Not Calculated (4B4c3b)
Calculate the base saturation (4B4c3a) by dividing the sum of the NH4OAc extractable bases (4B4a1) by CEC-8.2 (4B4b1a) and multiplying by 100. This value is reported as meq 100 g-1 or cmol (+) kg-1. If a soil has signficant quantities of soluble salts or carbonates, this value is not calculated (4B4c3b). Calculate base saturation by CEC-8.2 (Sum of Cations) as follows: Base Saturation (%) = [NH4OAc Bases/(NH4OAc Bases + BaCl2-TEA Acidity)] x 100 References Soil Survey Staff. 1999. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys, USDA-NRCS Agric. Handb. 436. 2nd ed. U.S. Govt. Print. Office, Washington, DC.

Ratios and Estimates Related to Ion Exhange and Extractable Cations (4B4) Base Saturation (4B4c) Base Saturation by Effective Cation Exchange Capacity (ECEC) (4B4c4) Base Saturation by Sum of NH4OAc Extractable Bases + 1 N KCl Extractable Aluminum, Calculated (4B4c4a) Base Saturation by Sum of NH4OAc Extractable Bases + 1 N KCl Extractable Aluminum, Not Calculated (4B4c4b)
Calculate the base saturation (4B4c4a) by dividing the sum of NH4OAc extractable bases (4B4a1) by the ECEC (4B4b2a) and multiplying by 100. If a soil has signficant quantities of soluble salts or carbonates, this value is not calculated (4B4c4b). Calculate base saturation by ECEC as follows:

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Base Saturation (%) = (NH4OAc Bases/NH4OAc Bases + 1 N KCl Al) x 100

Ratios and Estimates Related to Ion Exchange and Extractable Cations (4B4) Aluminum Saturation (4B4d) Aluminum Saturation by Effective Cation Exchange Capacity (ECEC) (4B4d1) Aluminum Saturation by Sum of NH4OAc Extractable Bases + 1 N KCl Extractable Aluminum, Calculated (4B4d1a) Aluminum Saturation by Sum of NH4OAc Extractable Bases + 1 N KCl Extractable Aluminum, Not Calculated (4B4d1b)
Calculate the Al saturation (4B4d1a) by dividing the 1 N KCl extractable Al (4B3a1a1) by ECEC (4B4b2a) and multiplying by 100. If a soil has signficant quantities of soluble salts or carbonates, this value is not calculated (4B4d1b). Calculate Al saturation as follows: Al Saturation (%) = [1 N KCl Al/(NH4OAc Bases + 1 N KCl Al)]

Ratios and Estimates Related to Ion Exchange and Extractable Cations (4B4) Activity (4B4e) 1500-kPa Water/CEC-7
Divide the 1500-kPa water retention (procedure 3C2a) by CEC by NH4OAc, pH 7 (procedure 4B1a1a1a1). This ratio is reported as a dimensionless value. In the past, the ratios of CEC:clay have been reported as meq g-1. For more detailed information on the application of this ratio, refer to Soil Survey Staff (1995, 1999).

Reaction (4C) Soil Suspensions (4C1) Electrode (4C1a) Standard Glass Body Combination (4C1a1) Digital pH/Ion Meter (4C1a1a)
Soil pH is one of the most frequently performed determinations, and one of the most indicative measurements of soil chemical properties (McLean, 1982). Soil pH tells more about a soil than merely indicating whether it is acidic or basic but also the availability of essential nutrients and toxicity of other elements can be estimated because of their known relationship with pH (Thomas, 1996). Soil pH is affected by many factors, e.g., nature and type of inorganic and organic matter; amount and type of exchangeable cations and anions; soil:solution ratio; salt or electrolyte content; and CO2 content (McLean, 1982). The acidity, neutrality, or basicity of a soil influences the solubility of various compounds; the relative ion bonding to exchange sites; and microbial activities. Depending on the predominant clay type, the pH may be used as a relative indicator of base saturation (Mehlich, 1934). Soil pH is also a critical factor in the availability of most essential elements for plants. The SSL performs several pH determinations. These methods include but are not limited to as follows: NaF (1 N pH 7.5 to 7.8) (4C1a1a1); saturated paste pH (4C1a1a2); oxidized pH (4C1a1a3); 1:1 water and 1:2 CaCl2 (final solution: 0.01 M CaCl2) (4C1a2a1-2, respectively); 1 N KCl, procedure 4C1a2a3; and organic materials, CaCl2 (final solution ≈ 0.01 M CaCl2) (4C1a1a4). An increase in the soil:water ratio or the presence of salts generally results in a decrease in the soil pH. The soluble salt content of the soil can be overcome by using dilute salt
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solutions, e.g., CaCl2 or KCl, instead of distilled water. The use of dilute salt solutions is a popular method for masking seasonal variation in soil pH. The pH readings are usually less with dilute salt solutions than with distilled water but may be equal to or greater in highly weathered tropical soils, i.e., soils with a high anion exchange capacity. When the pH values of various soils are compared, determination by the same method is important (Foth and Ellis, 1988). The 1 N KCl is an index of soil acidity and is more popular in those regions with extremely acid soils and in which KCl is used as an extractant of exchangeable Al. The KCl pH indicates the pH at which Al is extracted. Similar to the 1:2 CaCl2 pH, the 1 N KCl pH readings also tend to be uniform regardless of time of year. The saturated paste pH is popular in regions with soils with soluble salts. The water content varies with soil water storage characteristics. The saturated paste pH may be more indicative of the saturated, irrigated soil pH than is the soil pH measurement at a constant soil:water ratio. The saturated paste pH is also that pH at which the saturation extract is removed for salt analysis, and hence, is the pH and the dilution at which the sodium adsorption ratio (SAR) is computed (procedure 4E4b). The 1 N NaF pH may be used as an indicator that amorphous material dominates the soil exchange complex. The oxidized pH may be used to assess the activities of soil microorganisms. In soil taxonomy, the CaCl2 pH is used to distinguish two family reaction classes in Histosols (Soil Survey Staff, 1999). References Foth, H.D., and B.G. Ellis. 1988. Soil fertility. John Wiley and Sons. New York, NY. McLean, E.O. 1982. Soil pH and lime requirement. p. 199-224. In A.L Page, R.H. Miller, and D.R. Keeney (eds.) Methods of soil analysis. Part 2. Chemical and microbiological properties. 2nd ed. Agron. Monogr. 9. ASA and SSSA, Madison, WI. Mehlich, A. 1943. The significance of percentage of base saturation and pH in relation to soil differences. Soil Sci. Soc. Am. Proc. 7:167-174. Soil Survey Staff. 1999. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys, USDA-NRCS Agric. Handb. 436. 2nd ed. U.S. Govt. Print. Office, Washington, DC. Thomas, G.W. 1996. Soil pH and soil acidity. p. 475-490. In D.L. Sparks (ed.) Methods of soil analysis. Part 3. Chemical methods. No. 5. ASA and SSSA, Madison, WI.

Reaction (4C) Soil Suspensions (4C1) Electrode (4C1a) Standard Glass Body Combination (4C1a1) Digital pH/Ion Meter (4C1a1a) 1 N NaF, pH 7.5 – 7.8 (4C1a1a1) Air-Dry or Field-Moist, <2 mm (4C1a1a1a-b1)
1. Application The action of NaF upon noncrystalline (amorphous) soil material releases hydroxide ions (OH-) to the soil solution and increases the pH of the solution. The amount of amorphous material in the soil controls the release of OH- and the subsequent increase in pH (Fields and Perrott, 1966). The following reactions illustrate this action and form the basis of this procedure. Al(OH)3 + 3 F- >> AlF3 + 3 OHSi(OH)4 + 4 F- >> SiF4 + 4 OH-

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Most soils contain components that react with NaF and release OH-. However, a NaF pH >9.4 is a strong indicator that amorphous material dominates the soil exchange complex. Amorphous material is usually an early product of weathering of pyroclastic materials in a humid climate. Amorphous material appears to form in spodic horizons in the absence of pyroclastics. 2. Summary of Method A 1-g sample is mixed with 50 mL of 1 N NaF and stirred for 2 min. While the sample is being stirred, the pH is read at exactly 2 min in the upper 1/3 of the suspension (4C1a1a1). 3. Interferences The difference in the sediment and supernatant pH is called the suspension effect (McLean, 1982). To maintain uniformity in pH determination, measure the pH just above the soil sediment. Clays may clog the KCl junction and slow the electrode response. Clean the electrode by rinsing with distilled water and patting it dry with tissue. Wiping the electrode dry with a cloth, laboratory tissue, or similar material may cause electrode polarization. Use high purity (99%) NaF. Soils with a 1:1 water pH >8.2 do not give a reliable NaF pH. Free carbonates in a soil result in a high NaF pH. In general, soils with a 1:1 water pH <7.0 are not affected. 4. Safety The NaF is poisonous. Avoid eye contact and ingestion. Skin penetration and irritation are moderately hazardous. Do not eat or drink while using NaF. Thoroughly wash hands after use. Wear protective clothing, e.g., coats, aprons, and gloves, and eye protection, e.g., safety glasses or goggles, when using NaF. Use the fume hood when using NaF. Follow standard laboratory safety practices. 5. Equipment 5.1 Electronic balance, ±1.0-mg sensitivity 5.2 Paper cup, 120 mL (4 fl. oz.), disposable, Solo Cup Co., No. 404 5.3 Titration beakers, polyethylene, 250 mL 5.4 Automatic titrator, Metrohm Titroprocessors, Control Units, Sample Changers, and Dosimats, Metrohm Ltd., Brinkmann Instruments, Inc. 5.5 Combination pH-reference electrode, Metrohm, Brinkmann Instruments, Inc. 6. Reagents 6.1 Reverse osmosis (RO) water, ASTM Type III grade of reagent water 6.2 Borax pH buffers, pH 4.00, pH 7.00, and pH 9.18, for electrode calibration, Beckman, Fullerton, CA. 6.3 Phenolphthalein 6.4 Sodium fluoride (NaF), 99% purity, EM Science 6.5 Sodium fluoride (NaF), 1.0 N solution. In a plastic bottle, add 400 g NaF in 8 L of distilled water. Let stand for 3 days. On the third day, after excess NaF has settled, measure 50 mL of the solution and read pH. The pH should be between 7.5 and 7.8. Add 3 to 5 drops 0.25% phenolphthalein and titrate to pink end point (pH 8.2 to 8.3). If pH is outside the 7.5 and 7.8 range, then adjust pH with either HF or NaOH. If solution has a pH >8.2 or if the titratable acidity is >0.25 meq L-1, use another source of NaF. 7. Procedure 7.1 Weigh 1 g of <2-mm or fine-grind, air-dry soil to the nearest 1 mg and place in a 120-mL (4-oz) paper cup. If sample is moist, weigh enough soil to achieve ≈ 1 g of air-dry soil. 7.2 Calibrate the titrator with pH 4.00, 7.00, and 9.18 buffer solutions.
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7.3 Sample stirring, waiting interval for readings, addition of NaF solution, pH readings, and rinsing of electrode are controlled by computer. 7.4 The general sequence used by the automated system is as follows: 7.4.1 The sample is lifted so that the pH electrode is positioned above the soil sediment. Stirring begins immediately and is maintained during each sample cycle. 7.4.2 A 50-mL solution is added to sample. 7.4.3 After 2 min, NaF pH is read. Record pH to the nearest 0.01 unit. 7.4.4 The sample is lowered, and the electrode and stirrer are rinsed with RO water. 7.4.5 The next sample is positioned for analysis. 7.4.6 The cycle is repeated until all samples have been analyzed. 7.5 Discard the solution and cup in safe containers. The paper cup with the NaF solution leaks in about 15 min. 8. Calculations No calculations are required for this procedure. 9. Report Report NaF pH to the nearest 0.1 pH unit. 10. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 11. References Fields, M., and K.W. Perrott. 1966. The nature of allophane in soils. Part 3. Rapid field and laboratory test for allophane. N.Z. J. Sci. 9:623-629. McLean, E.O. 1982. Soil pH and lime requirement. p. 199-224. In A.L. Page, R.H. Miller, and D.R. Keeney (eds.) Methods of soil analysis. Part 2. Chemical and microbiological properties. 2nd ed. Agron. Monogr. 9. ASA and SSSA, Madison,

Reaction (4C) Soil Suspensions (4C1) Electrode (4C1a) Standard Glass Body Combination (4C1a1) Digital pH/Ion Meter (4C1a1a) Saturated Paste pH (4C1a1a2) Air-Dry, <2 mm (4C1a1a2a1)
1. Application When making interpretations about the soil, the saturated paste pH is usually compared to the 1:1 water pH and the 1:2 CaCl2 pH. The usual pH sequence is as follows: 1:1 water pH > 1:2 CaCl2 pH > saturated paste pH. If saturated paste pH is > 1:2 CaCl2 pH, the soil is not saline. If the saturated paste pH > 1:1 water pH, the soil may be Na saturated and does not have free carbonates. Because of the interrelations that exist among the various soil chemical determinations, the saturated paste pH value may be used as a means of cross-checking salinity data for internal
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consistency and reliability (U.S. Salinity Laboratory Staff, 1954). Some rules of thumb that apply to the saturated paste pH are as follows: a. Soluble carbonates are present only if the pH is >9. b. Soluble bicarbonate seldom >3 or 4 meq L-1, if the pH is <7. c. Soluble Ca2+ and Mg2+ seldom >2 meq L-1, if the pH is >9. d. Gypsiferous soils seldom have a pH >8.2. 2. Summary of Method The saturated paste is prepared (4F2), and the pH of paste is measured with a calibrated combination electrode/digital pH meter (4C1a1a2). 3. Interferences The difference in the sediment and supernatant pH is called the suspension effect (McLean, 1982). To maintain uniformity in pH determination, measure the pH just beneath the surface of saturated paste. Clays may clog the KCl junction and slow the electrode response. Clean the electrode by rinsing with RO water and patting it dry with tissue. Wiping the electrode dry with a cloth, laboratory tissue, or similar material may cause electrode polarization. 4. Safety No significant hazards are associated with this procedure. Follow standard laboratory safety practices. 5. Equipment 5.1 Digital pH/ion meter, Accumet Model AR15, Fisher Scientific 5.2 Electrode, standard glass body combination, Accu-flow, Fisher Scientific 6. Reagents 6.1 Reverse osmosis (RO) water, ASTM Type III grade of reagent water 6.2 Borax pH Buffers, pH 4.00, pH 7.00 and pH 9.18, for electrode calibration, Beckman, Fullerton, CA. 7. Procedure 7.1 Prepare a saturated paste (procedure 4F2). 7.2 Calibrate the pH meter with pH 4.00, 7.00 and 9.18 buffer solutions. 7.3 After equipment calibration, gently wash the electrode with RO water. Dry the electrode. Do not wipe the electrode with a tissue as this may cause a static charge on the electrode. 7.4 Gently lower the electrode in the saturated paste until the KCl junction of the electrode is beneath the surface of saturated paste. 7.5 Allow the pH meter to stabilize before recording the pH. Record pH to the nearest 0.01 unit. 7.6 Gently raise the pH electrode from the paste and wash all particles adhering to the electrode with a stream of RO water.

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8. Calculations No calculations are required for this procedure. 9. Report Report saturated paste pH to the nearest 0.1 pH unit. 10. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 11. References McLean, E.O. 1982. Soil pH and lime requirement. p. 199-224. In A.L. Page, R.H. Miller, and D.R. Keeney (eds.) Methods of soil analysis. Part 2. Chemical and microbiological properties. 2nd ed. Agron. Monogr. 9. ASA and SSSA, Madison, WI. U.S. Salinity Laboratory Staff. 1954. L.A. Richards (ed.) Diagnosis and improvement of saline and alkali soils. USDA Handb. 60. U.S. Govt. Print. Office, Washington, DC.

Reaction (4C) Soil Suspensions (4C1) Electrode (4C1a) Standard Glass Body Combination (4C1a1) Digital pH/Ion Meter (4C1a1a) Oxidized pH (4C1a1a3)
1. Application Sulfidic material is waterlogged mineral, organic, or mixed soil material with a pH of 3.5 or higher, containing oxidizable sulfur compounds, and which if incubated as a 1-cm thick layer under moist, aerobic conditions (field capacity) at room temperature, shows a drop in pH of 0.5 or more units to a pH value of 4.0 or less (1:1 by weight in water or in a minimum of water to permit measurement) within 8 wk (Van Breemen, 1982; Soil Survey Staff, 1999). The intent of the method described herein is to determine if known or suspected sulfidic materials will oxidize to form a sulfuric horizon (Soil Survey Staff, 1999). Identification of H2S in a soil by a “rotten-egg” smell or FeS in a saturated soil by its blue-black color indicates that sulfidic materials may be present. If such soils are drained and oxidized, the soil pH could drop to 3.5 or less, making the soil unsuitable for many uses. A field test for FeS is to add 1 N HCl and note the odor of H2S. 2. Summary of Method Transfer enough soil to fill a plastic cup one-half to two-thirds full. Add a little water if needed to make a slurry. Stir the slurry thoroughly to introduce air. Determine pH immediately. Place cup in a closed container with openings (inlet and outlet) providing humidified air. Keep at room temperature. After 24 h, open the container, stir the sample thoroughly, and determine the soil pH. Repeat the procedure for a minimum of 10 days until the pH reaches a steady state of < 0.1 units over a 2-day period. Record daily pH readings (4C1a1a3). 3. Interferences Samples should be shipped in watertight containers completely filled with water from the ambient soil solution to prevent potential oxidation of sulfides and reduction in soil pH. Extended time in stirring of sample and/or in reading the pH may result in the introduction of sufficient O2 into the mixture to change the pH reading. Quickly stirring the mixture and reading the pH reduce this error. Clean the electrode by rinsing with reverse osmosis (RO) water and patting it dry with tissue. Wiping the electrode dry with a cloth, laboratory tissue, or similar material may cause electrode polarization.
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4. Safety No significant hazard has been identified with this procedure. Follow standard laboratory safety precautions. 5. Equipment 5.1 Cups, plastic 5.2 Closed container, with openings (inlet and outlet) providing for humidified airflow. A tube from the inlet of this closed container is connected to the outlet of a stoppered 2.5-L container full of RO water. A pump supplies air to a bubbling stone placed near the bottom of the 2.5-L container (Fig. 1).

Fig. 1. Apparatus for measuring oxidized pH. 5.3 Digital pH/ion meter, Accumet Model AR15, Fisher Scientific 5.4 Electrode, standard glass body combination, Accu-flow, Fisher Scientific 6. Reagents 6.1 Reverse osmosis (RO) water, ASTM Type III grade of reagent water 6.2 Borax pH buffers, pH 4.00 and pH 7.00 for pH meter calibration, Beckman, Fullerton, CA. 7. Procedure 7.1 Calibrate the pH meter with pH 4.00 and pH 7.00 buffer solutions. 7.2 After equipment calibration, gently wash the electrode with RO water. Dry the electrode. Do not wipe the electrode with a tissue as this may cause a static charge on the electrode. 7.3 Transfer enough soil to fill a small plastic cup one-half to two-thirds full. Add a little water if needed to make a slurry. Stir the slurry thoroughly to introduce air. 7.4 Determine immediately the pH of sample by carefully placing the electrode into the soil mixture. Ensure that the KCl junction and sensor membrane are in contact with the mixture. 7.5 Allow the pH meter to stabilize before recording the pH. Record the pH to the nearest 0.01 pH unit. 7.6 After pH determination, immediately place sample in a closed container with openings (inlet and outlet) providing for humidified airflow. A tube from the inlet of this closed container is connected to the outlet of a stoppered 2.5-L container full of RO water. A pump

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9. 2nd. or similar material may cause electrode polarization. Spec.5 mL (2. Genesis. U.5 cm3) of the prepared sample in a 30-mL plastic container and add 4 mL of 0. Report Report the initial pH and the oxidized pH (end pH) to the nearest 0. Wiping the electrode dry with a cloth. morphology.A. 11. and L. Kittrick. yields final concentration of ≈ 0.015 M CaCl2. WI. Application This pH is used in soil taxonomy to distinguish two family reaction classes in Histosols (Soil Survey Staff.01 M CaCl2 in some part of the control section. Final Solution ≈ 0. 1999). ed.7 Stir the sample and record pH daily. 8. 1982. 7. 1999).01 M CaCl2 (4C1a1a4) 1. immediately place sample back in closed container. p.10.) Acid sulfate weathering. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.01 M CaCl2 with most packed. 7. laboratory tissue. Dysic families have a pH <4.e. Note any bubbling. The specific volume of moist material depends on how it is packed. Keep at room temperature (20 to 25°C). Therefore. After pH determination. ASA and SSSA. Since it is not practical in the field to base a determination on a dry sample weight. Am. Madison. 95-108. Print.5 in 0.R. packing of material must be standardized in order to obtain comparable results by different soil scientists (Soil Survey Staff. In J. Soil Soc. Handb. Govt. Mix.supplies air to a bubbling stone placed near the bottom of the 2. i. 10. D. N. No. Reaction (4C) Soil Suspensions (4C1) Electrode (4C1a) Standard Glass Body Combination (4C1a1) Digital pH/Ion Meter (4C1a1a) Organic Materials CaCl2 pH.. DC. Interferences This test of organic soil material can be used in field offices. Uncover and measure pH with pH paper or pH meter (4C1a1a4).5 in 0.8 Record the pH for a minimum of 10 days until the change is <0. 2.S. 436. References Van Breemen. 1999. Publ.1 pH units for two days. cover. Calculations No calculations are required for this procedure. USDA-NRCS Agric. 3. moist organic materials. Washington. Summary of Method Place 2. and classification of acid sulfate soils in Coastal Plains. Euic families have a pH >4. Clean the pH electrode by rinsing with reverse osmosis (RO) water and patting it dry with tissue. Fanning. 211 . Hossner (eds. and allow to equilibrate at least 1 h. moist soil is used. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys.01 M CaCl2 in all parts of the organic materials in the control section.S. Office. Soil Survey Staff.5-L container.1 pH unit.

4 Half-syringe. yields a final concentration of approximately 0.6 Mix.2 Digital pH/ion meter.e. standard glass body combination. Fisher Scientific 5. Close cover and allow to equilibrate approximately 5 min. Report Report the 0.015 M CaCl2. Compare color of active segment (center) with reference segments and with pH scale on box to determine pH.5 Place 2.7 Uncover. mix again. place pH strip on top of sample so that it wets from the bottom. ASTM Type III grade of reagent water 6.00 and 7. Dissolve 1. 5. Beckman. Remove the sample and place on a fresh paper towel.10 g of CaCl2·2H2O in RO water and dilute to 500 mL. and measure pH. 5. Calculations No calculations are required for this procedure. and pH (4C1a1a4). Follow standard laboratory safety precautions. 0.1 pH unit. solubility in pyrophosphate (5B).3 Borax pH buffers. 6 mL.3 Randomly select sample segments for determination of fiber (5C).5 cm3) of the prepared sample in a 30-mL polycon and add 4 mL of 0. Rinse electrode with RO water. Use additional paper towels as external blotters. 7. 7. i. Safety No signifcant hazard has been identifed with this procedure. Equipment 5. Place 50 to 60 mL of a representative sample on a paper towel in a linear mound.8 Alternatively. 7.1 Polycons.5 mL (2. If the soil is dry.0-cm long segments. pH Determination 7. for pH meter calibration. and allow to equilibrate at least 1 h. add water and let stand to saturate.3 Electrode. 9. Fisher Scientific 5. Roll the towel around the sample and express water if necessary. 7.01 M CaCl2 with most packed moist organic materials. Procedure Sample Preparation 7. 30 mL 5. 7.4. Accumet Model AR15. Reagents 6.2 Use scissors to cut sample into 0.01 M CaCl2 pH to the nearest 0. 212 . 7.015 M.4 Use a metal spatula to pack a half-syringe that is adjusted to the 5-mL mark or 2.5.5-mL (2. 7. 8. Cut plastic syringe longitudinally to form a half-cylinder measuring device. Accu-flowt.00.5 Metal spatula 6. immerse electrode. Remove pH strip with tweezers. 6.1 Reverse osmosis (RO) water. cover.to 1.2 Calcium chloride (CaCl2). Use a wash bottle to gently wash soil from bottom of strip. The sample should be firm but saturated with water. CA.1 Prepare soil material. pH 4.5cm3) volume with the moist sample. Fullerton.

02 M CaCl2 (20mL) is added to soil suspension. DC. Closed containers and nonporous materials will not allow equilibration with CO2. 436. 213 . 2nd ed.1 to 1 M) can lower the measured pH from 0. 11. Govt. 1982). < 2mm (4C1a2a2a-b1) 1. U. if doing critical work. The combination of exchange and hydrolysis in salt solutions (0.10.5 in 1:1 water. 1999).0 pH in 0. The sample is stirred for 30 s. USDA-NRCS Agric. and the 1:1 water pH is measured. Measure the pH just above the soil sediment to maintain uniformity. The sample is allowed to stand 1 h with occasional stirring. these pH values are used as a criterion for reaction classes (acid and nonacid) in families of Entisols and Aquepts (Soil Survey Staff.01 M CaCl2 pH (4C1a2a2) Air-Dry or Field Moist. compared to the pH measured in RO water (Foth and Ellis. The CaCl2 soil pH is generally less than the 1:1 water pH. 4.02 M CaCl2 to the soil suspension that was prepared for the water pH. Atmospheric CO2 affects the pH of the soil:water mixture. 2.01 M CaCl2 pH (4C1a2a2) determinations are two commonly performed soil pH measurements. Follow standard laboratory safety practices.01 M CaCl2 pH is measured (4C1a2a2). the sample is stirred. Office. <2 mm (4C1a2a1a-b1) 1:2 0. Rinse the electrode with distilled water and pat dry.0 pH in 0. 1999.01 M CaCl2 (2:1) or ≈ 5. Summary of Method The pH is measured in soil-water (1:1) and soil-salt (1:2 CaCl2) solutions. References Soil Survey Staff. The 0. Safety No significant hazards are associated with the procedure. The acid class is <5.S. 1988). 3. Clean the electrode. Handb. Application The 1:1 water pH (4C1a2a1) and 1:2 0. At the time of pH determination. the partial pressure of CO2 and the equilibrium point must be considered. Wiping the electrode dry with cloth. Clays may clog the KCl junction and slow the electrode response. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. A 20-g soil sample is mixed with 20 mL of reverse osmosis (RO) water (1:1 w:v) with occasional stirring. laboratory tissue or similar material may cause electrode polarization. For convenience. Washington. and the 1:2 0. the final soil-solution ratio is 1:2 0. With the addition of an equal volume of 0. The nonacid class is >5. the pH is initially measured in water and then measured in CaCl2. Print. Reaction (4C) Soil Suspensions (4C1) Electrode (4C1a) Combination pH-Reference Electrode (4C1a2) Automatic Titrator (4C1a2a) 1:1 Water pH (4C1a2a1) Air-Dry or Field-Moist. Interfernces The pH will vary between the supernatant and soil sediment (McLean.5 units. In soil taxonomy.01 M CaCl2. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.5 to 1.01 M CaCl2 (2:1).

5 Load beakers into sample changer.02 M CaCl2 are added to sample. and pH 9..01 unit. 7. 6. Sample Changers. 7.8 The cycle is repeated until all samples have been analyzed.4 Beverage stirring sticks. If sample is moist.2 Borax pH buffers.3 After 1 min.5 Titration beakers.6 Automatic titrator.52 g of CaCl2·2H2O in RO water and dilute to 8 L. 5. 0 to 30 mL. Fullerton.1 Use a calibrated scoop to measure ≈ 20 g of <2-mm or fine-grind. 404 5.. waiting interval for readings.2 Place the sample in a 120-mL (4-oz) paper cup. pH 4. 7. 7.02 M. ASTM Type III grade of reagent water 6. 7. handmade.00 and pH 4. pH readings. Beckman. ≈ 20-g capability 5.4 Place paper cup with sample in 250-mL titration beaker.8.8. The sample is stirred for 30 s. 7. Control Units. 214 .8. 7.).18. for electrode calibration. 120 mL (4 fl. 7. Dissolve 23. Procedue 7. Brinkmann Instruments. use calibrated scoop to achieve ≈ 20 g of air-dry soil.00. 7.18. Metrohm Ltd. addition of CaCl2 solution. 6. air-dry soil.7 The next sample is positioned for analysis. Inc.0210.7 Sample stirring. pH 7. stirring occasionally. 7.8. Equipment 5.8. and the electrode and stirrer are rinsed with RO water. 7.1 The sample is lifted so that the pH electrode is positioned above the soil sediment. Record pH to the nearest 0. 7. allow to stand for 1 h. Metrohm part no. 7.3 Dispense 20 mL of RO water into sample and stir.2 Paper cup.01 unit.00 buffer solutions. Inc. Reagents 6.8 The general sequence used by the automated system is as follows: 7. CA. No. wood 5.5 After 1 min. Metrohm Titroprocessors.100. 7. 6. Solo Cup Co.1 Measuring scoop. 7.3 Dispenser. polyethylene. oz. Brinkmann Instruments.8.3 Calcium chloride (CaCl2). and rinsing of electrode are controlled by computer.4 The 20 mL of 0.2 The sample is stirred for 30 s. the 1:2 CaCl2 pH is read.8. Record pH to the nearest 0.1 Reverse osmosis (RO) water. 250 mL 5.6 The sample is lowered. Repipet or equivalent 5. 1:1 water pH is read.00. 7. disposable. 0.5.7 Combination pH-reference electrode. and Dosimats.8.6 Calibrate the pH meter using the pH 9.

2 Paper cup. McLean. Govt. 11. Soil fertility. 4.R.1 pH unit. 2nd ed. 9. DC. Repipet or equivalent 5. and D. 199-224. oz. almost all the acidity is in the form of Al. 5.) Methods of soil analysis. 3. handmade. Keeney (eds. Monogr. 250 mL 215 . The sample is allowed to stand for 1 h with occasional stirring. Application The 1 N KCl pH is an index of soil acidity. Soil pH and lime requirement. 1982). Ellis.8. Part 2. Page. Madison. Miller.. laboratory tissue. NY. ≈ 20 g 5. Summary of Method A 20-g soil sample is mixed with 20 mL of 1 N KCl. 404 5. Chemical and microbiological properties. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.S.1 Measuring scoop. and after 1 min. 1999. 0 to 20 mL. p. 1982.L. Washington. polyethylene. E. Clays may clog the KCl junction and slow the electrode response. 9. Handb. NY. FSN 7340-00-753-5565 5. Clean the electrode by rinsing with reverse osmosis (RO) water and patting it dry with tissue.4 Beverage stirring sticks. In A.O. USDA-NRCS Agric.01 M CaCl2 pH to the nearest 0. Equipment 5.5 Titration beakers. R.. Reaction (4C) Soil Suspensions (4C1) Electrode (4C1a) Combination pH-Reference Electrode (4C1a2) Automatic Titrator (4C1a2a) 1 N KCl pH (4C1a2a3) Air-Dry or Field-Moist. <2 mm (4C1a2a3a-b1) 1. Calculations No calculations are required for this procedure. John Wiley and Sons.H. the KCl pH is read (4C1a2a3). To maintain uniformity in determination. Report Report the 1:1 water pH and the 1:2 0. Follow standard laboratory safety practices. Interferences The difference in the sediment and supernatant pH is called the suspension effect (McLean. 2nd ed. 436. References Foth. WI. measure the pH just above the soil sediment. and if the pH is very much below 5. U.). and B. No. Solo Cup Co. Soil Survey Staff. 1988. If KCl pH is <5. 10. H.D. wood. Safety No significant hazards are associated with the procedure. 120 mL (4 fl.G. Office. The sample is stirred for 30 s. 2.3 Dispenser. Print. ASA and SSSA. Agron. Wiping the electrode dry with a cloth. disposable. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. or similar material may cause electrode polarization. significant amounts of Al are expected in the solution.

1 Reverse osmosis (RO) water.4 The sample is lowered.00. Precision and Accuracy Precision and accuracy data are available upon request from the SSL. 7. 7. CA. and Dosimats.8. the KCl pH is read. 7. Procedure 7. Sample Changers. and the electrode and stirrer are rinsed with RO water. and rinsing of electrode are controlled by computer. 7.01 unit. If sample is moist. 7.00.18 for electrode calibration. 9. and 9.8.1 pH unit.0 N. 8.6 Calibrate the pH meter using the pH 4. pH reading. pH 4.8.2 The sample is stirred for 30 s. 7.8 The general sequence used by the automated system is as follows: 7.8. 7.6 The cycle is repeated until all samples have been analyzed. 7. Fullerton.5 Load beakers into sample changer table. Record pH to the nearest 0.5.7 Combination pH-reference electrode. Dissolve 74.8.2 Place the sample in a 120-mL (4-oz) paper cup. 7. Report Report KCl pH to the nearest 0.3 After 1 min. use calibrated scoop to achieve ≈ 20 g of air-dry soil. Calculations No calculations are required for this procedure.7 Sample stirring.56 g of KCl in RO water.18 buffer solutions. 1. 7.00. 7. Brinkmann Instruments. 7. 6. 10.00. 5. waiting interval for reading. air-dry soil.3 Potassium chloride (KCl).. Brinkmann Instruments.2 Borax pH buffers. Reagents 6. Inc. 216 .6 Automatic titrator. Metrohm Titroprocessors. Control Units. 7. and 9. Beckman. 6. 7.8.5 The next sample is positioned for analysis. Metrohm Ltd.1 Use a calibrated scoop to measure ≈ 20 g of <2-mm or fine-grind. Inc. 7. Dilute to 1 L. stirring occasionally. allow to stand 1 h. ASTM Type III grade of reagent water 6.1 The sample is lifted so that pH electrode is positioned above the soil sediment.3 Dispense 20 mL of 1 N KCl into sample and stir with wooden beverage stirrer.4 Place paper cup with sample in 250-mL titration beaker.

level and kind of added P (Barrow. Frossard et al. concentration of interfering substances in the solution to be analyzed. References McLean. and environmental studies (Burt et al. and the particular acid system involved in the analytical procedure (Olsen and Sommers. Chang et al. with the popularity of this procedure increasing due to the use of multi-element soil extractants (SERA-IEG 17. 1982.11. 199-224. accuracy. 3 (4D6a1). WI.. and extracts (SERA-IEG 17. 1993). This selection is influenced by many factors. ASA and SSSA. 1984. accommodating water samples. other soil and land management factors (Haynes.. 4H1b1a1a1-11) are described in another section of this manual entitled “Total Analysis”. 2000). 1985. Olsen sodium-bicarbonate (4D5a1). Inorganic N in soils is predominately NO3 and NH4.) Methods of soil analysis. The procedures for total P analysis (4H1a1a1a1-20. Total N includes both organic and inorganic forms.O.. 1999). The SSL determines a number of P analyses. forms. In more recent years. Sharpley et al. 1985).g. 1974. soil testing has been widely used as a basis for determining lime and fertilizer needs (Soil and Plant Analysis Council. 1982). is commonly related to water-quality problems. and as such. p. 1993). The selected colorimetric method for P determination depends on the concentration of solution P. genesis and geomorphology models. and D. and reproducibility (Olsen and Sommers. For more than 30 years. and lend themselves to automated analysis. Miller. and soil P-sorption characteristics (Goldbert and Sposito. e. Most soil P determinations have two phases. Page. as they are sensitive. 2nd ed. Agron.L. 1957) has been instrumental in developing principles and understanding of the nature and behavior of P in soils (Olsen et al. 1987). water soluble (4D2a1a1). 1984.. some of these tests have been employed in more diverse agronomic and environmental uses (SERAIEG. In A. i. 2002).e. 2000). E. The SSL procedure for total N (4H2a2) is described in another section of this manual entitled “Total Analysis”. digest solutions.R. and New Zealand P Retention (4D8a1). objectives of study. To characterize the P in the soil system requires the selection of an appropriate method of determination. Mehlich No.. sample condition or environment. Bray P1 (4D3a1). Monogr.. It is for these reasons that the SSL has expanded its suite of soil test analyses to more completely characterize the inorganic and organic N fractions and to provide a number P analyses for a broad spectrum of soil applications. Van Riemsdijk et al. Knowledge of these factors and their impact upon the fate and transport of soil P has been used in developing soil P interpretations for such broad and diverse application as fertility. Polyzopoulos et al. Madison. Methods development in soil P characterization (Bray and Kurtz. These P analyses include but are not limited to as follows: anion-resin extractable (4D1a1a1a1-2). soil organic matter. Nitrogen is one of the most important plant nutrients and forms some of the most mobile compounds in the soil-crop system. 9. reproducible. R. 1945. preparation of a solution that contains the soil P or fraction thereof and the quantitative determination of P in the solution. taxonomic classification.. Chemical and microbiological properties. Soil pH and lime requirement.. Part 2. Stewart et al. Amounts.. with nitrite seldom found in detectable amounts except in neutral to alkalilne soils receiving NH4 or NH4-producing 217 Soil Test Analyses (4D) . water and the atomosphere (National Research Council. 2000). mostly colorimetrically. 2000)... with the exception of the multi-element extractant Mehlich No. 1974.H. 1982. 1982). 1985. Nitrogen is ubiquitous in the environment as it is continually cycled among plants. Sharpley. Tisdale et al. Results from colorimetric analyses are not always comparable to those from ICP because ICP estimates the total amount of P in solution while the colorimetric procedures measure P that can react with the color developing reagent (SERA-IEG 17. Olsen et al.. 1996 ). citric acid soluble (4D7a1). 3 (4D6a1a1-18). Keeney (eds. 1982). Inductively coupled plasma (ICP) spectrophotometry can also be used for P determination. and distribution of soil P vary with soil-forming factors (Walker. soil properties. soil organisms. Most P analyses of soil solutions have been colorimetric procedures. 1954.

1996). Soil Sci. Phosphorus. S. J. and Mulvaney. and D.L.W.V. with a flow injection automated ion analyzer used to measure the soluble inorganic nitrate (NO3-) (4D9a1a1-2). Commun. 1982. R. Determination of total. S. Ellert. 1974. Morel. Bray. Lewis Publ. Page.C. and Y.A. S. Koisse. DC Olsen. The resulting water soluble dye has a magenta color which is read at 520 nm. 1993). 1993).) Methods of soil analysis. The nitrate is quantitatively reduced to nitrite by passage of the sample through a copperized cadmium column. Fardeau. Dean. References Barrow.W. Am. 1993. J. Soc. 1982. 24:367-377. Burt. Sommers.fertilizers (Maynard and Kalra. A chemical model of phosphate adsorption by soils. B. Campbell. Haynes. p. R. Plant Anal. FL. 1985. Chang.. Phosphorus characterization and correlation with properties of selected benchmark soils of the United States. described in another section of this manual entitled “Soil Biological and Plant Analyses”. J. Carter (ed. 1993. Plant Soil. 1954. p. FL. Madison. U.J. Soil Sci. and L. and available forms of phosphorus in soils. Effect of previous additions of phosphate on phosphate adsorption by soils.P. Miller. 63:289308. Plant Anal. 1993. Cole.G. Washington.L.A. Mulvaney. Jame..H. and C. with the most common being KCl (refer to Maynard and Kalra. E. The nitrite (reduced nitrate plus original nitrite) is then determined by diazotizing with sulfanilamide followed by coupling with N-1naphthylethylenediamine dihydrochloride. 1945. Soil Sci. R. N. Mays. An agenda for agriculture. Soil and water quality. These techniques may be aerobic or anerobic. Acad. p. 341-357. 84:133-144. and J.. Mulvaney. Stewart. H. Nitrate and exchangeable ammonium nitrogen. Tiessen. and L. Kenney (eds. 1996 for review of extractants). The concept of an organic N fraction that is readily mineralized has been used to assess soil N availability in cropland. Boca Raton. Nitrate is water soluble and a number of soil solutions including water have been used as extractants. D. N. Soil Sci. and M. and Y. Soc. Nitrogen – Inorganic forms.. Maynard.. Natl. 33:117-141.B. 1996. Can. 59:39-45. C.S. In In D. In Martin R.L. Fractionation of soil phosphorus. Can an isotopic method allow for the determination of phosphate-fixing capacity of soils? Commun... Agron. Sposito.S. In Martin R. Chemical and microbiological properties.R..H. Polyzopoulos. p. Soc. Madison. organic. The SSL determines inorganic N (nitrate-nitrite) by KCl extraction. S. Govt. C. 1123-1184. ASA and SSSA. Estimation of available phosphorus in soils by extraction with sodium bicarbonate.L. 2nd ed. Am. and M. In addition. WI.) Soil sampling and methods of analysis.. Kurtz. Phosphate sorption by some Alfisols as described by commonly used isotherms. Keramidas. Washington.Z. 5. Watanabe. Soil Sci. Soil Sci. and H.A.R. USDA Circ.D.C. ASA and SSSA. Frossard. 49:81-84. 2002. Chemical methods. 25-38. National Research Council. 1984. and G. In A. There is considerable diversity among laboratories in the extraction and determination of NO3 and NH4 (Maynard and Kalra. V. 403-430. Benham. No. Monogr. 1957. Office. Noncalcareous soils.L. 1993. Feller. DC.A. F. Incubation-leaching techniques have been used to quantify the mineralizable pool of soil organic N. Goldberg. II. WI. 1993. Press.R. and L. Lewis Publ. the SSL also determines mineralizable N after fumigation incubation (6B2a1a1). Committee on long-range soil and water conservation. 9.R. forests. Kalra..H. Part 3.E. The SSL determines mineralizable N (N as NH3) by anaerobic incubation (4D10a1a1). 48:779-783.C. Soil Sci. E. Olsen. Soil Sci. Nitrogen mineralilzation potential in soils. M. Part 2. Soc. 118:82-89.T... R. 218 . Carter (ed. 939. Wilson. Sparks (ed. H. Print. Can..) Methods of soil analysis. 1993.) Soil sampling and methods of analysis. J. Effects of liming on phosphate availability in acid soils. and waste-disposal sites (Campbell et al. Boca Raton. Jackson. Soil Sci.

Am.N. W.. 1 M NaCl (4D1a1a1) UV-Visible Spectrophotometer. Co. which are very sensitive for P. Availability of residual phosphorus in manured soils. Soil Tests (4D) Anion Resion Extraction (4D1) Two-Point Extraction (4D1a) 1-h. 2003). 0.H. resin bags are shaken for 1 h in 1 M NaCl solution. 4:41-60. Van der Linden. Beaton. Soc.) Southern Cooperative Series Bull. 8. Nelson. Soc. Int.N. In G.L.. Stewart. 2003). Dynamics of soil organic phosphorus. Phosphorus released from soil during shaking is adsorbed by resin.W. Trans. 1984. A. 1996. Am. M. Biogeochemistry.J. 3. 49:1010-1015. USDACSREES Regional Committee: Minimizing Agricultural Phosphorus Losses for Protection of the Water Resource. and management. The intensity of blue color varies with the P concentration but is also affected by other factors 219 . T. III. estimation of release characteristics and runoff P for agricultural land (Elrashidi.M. Methods of phosphorus analysis for soils. A 1-mL aliquot is diluted with 4 mL of ascorbic acid molybdate solution. Sharpley. sediments. J. Data are reported as mg P kg-1 soil (4D1a1a1a1-2). J. Boumans.. soil. 4th ed. Phosphorus as an index of soil development. 48 h) against amounts of P released (mg kg-1) showed a linear relationship in 24 U. No. Sharpley. Soc. Summary of Method A 2-g soil sample and 4-g resin bag are shaken with 100 mL of reverse osmosis deionized water for 1 h. J.25. 2. 1. Van Riemsdijk. benchmark soils (Elrashidi et al. Soil Sci. W. Soil Sci. Macmillan Publ. 24-h. Application Anion resins remove P from soils without chemical alterations and only minor pH changes. 4. S.B. Dual-Beam (4D1a1a1a) Phosphorus.W. 1987. Plotting g log of extraction periods (0. et al. <2 mm (4D1a1a1a1-2a-b1) 1. The method describes a two-point measurement (1 and 24 h extraction). Soil fertililty and fertilizers. Soil Sci. a phosphomolybdate complex forms that can be reduced by ascorbic acid. A. describing the whole relationship between the extraction time (1 min to 48 h) and amount of P released (mg kg-1) for soils (Elrashidi et al. 2003).SERA-IEG 17. 1982). 24.50. Congr. Amounts of P released from soil and adsorbed by resins have been used as a measure of available P. an assessment of the availability of residual phosphates. Two extraction periods (1 and 24 h) are sufficient to develop linear equations that predict P release characteristics (PRC). 2000. and H. 1974. A. 10:451-457. SnCl2. Depth of surface soil-runoff interaction as affected by rainfall. and L. NY. J. Soil Sci. Interferences The Mo blue methods. and the buffer capacity of soils (Olsen and Sommers. slopoe. residuals. 1985. 48:545-548.. XXX. The diffusioin-precipitation model tested for three acid sandy soils. Soil suspension is shaken again with another 4-g resin bag for 23 h. New York.. To remove P from resin. Absorbance of the solution is read using a spectrophotometer at 882 nm. 60:1459-1466.S. 2.L.A.M. Tiessen. are based on the principle that in an acid molybdate solution containing orthophosphate ions. 1985. Concentrated HCl is added to sample extracts.. Two points (4D1a1a1a1-2) Air-dry or Field-Moist. Am. Phosphate sorption by soils. J.D. and other reducing agents to a Mo color. Walker. Pierzynski (ed. and waters. Tisdale.

with Cary WinUV software.0 M NaCl. 1982).8 Pipettes. ASTM Type I grade of reagent water 6. Restrict the use of concentrated H2SO4 and HCl to a fume hood. 100. Store in RODI water in refrigerator. 6.4394 g primary standard grade anhydrous potassium dihydrogen phosphate (KH2PO4) that has been dried for 2 h at 110°C in about 800 mL 1. 4. Slowly and carefully add 700 mL of concentrated H2SO4. electronic digital. and substances that influence the oxidation-reduction conditions of the system (Olsen and Sommers.4 Hydrochloric acid (HCl). type II. Add 10 mL of ascorbic acid solution and dilute to 1 L with RODI water.4 Funnel. Varian. arsenates.0 M NaHCO3 solution and washing out excess salt with RODI water. 2500 µL and 10 mL. Dissolve 13. Make fresh weekly. plastic. Allow to cool to room temperature.455 g of antimony potassium tartarate (potassium antimony tartarate hemihydrate [K(SbO)C4H4O6·1/2H2O] in the ammonium molybdate solution. 1-cm light path. ±1. polyethylene. silicates. Dual-View. 50-mm diameter 5. Make fresh daily. UV-Visible.1 Electronic balance. 50 mL 5. 125.0-mg sensitivity 5. plastic 5.2 g of ascorbic acid in RODI water and dilute to 100 mL with RODI water. Equipment 5.3 Bottles. Cary 50 Conc.4 g NaCl in 1000 mL RODI water.6 Cups.8 Working ascorbic acid molybdate solution (WAMS). 220 .5 NaCl solution. 100 oscillations min-1. 150 mm 5. Cool and dilute to 1 L with RODI water. Inc. 250.1 Reverse osmosis deionized (RODI) water. 6. concentrated. Varian Australia Pty Ltd..0 mg P L-1. Dissolve 1. Thoroughly wash hands after handling these metal salts. MI 5. 4.9 Working stock standard P solution (WSSPS). Use sodium bicarbonate and water to neutralize and dilute spilled acids.10 Spectrophotometer. Daigger Scientific 5.5-mL. for making and sewing resin bags 6. In a 1-L volumetric flask. 510-610 µm spherical beads (DOW Chemical Company). Many metal salts are extremely toxic and may be fatal if ingested.2 Anion exchange resin (AER). Allow to stand at least 1 h before using. 60° angle.3 Nitex nylon fabric. 300-µm pores.11 Computer. 1 1⁄2 in strokes. DOWEX Marathon. and gloves) and eye protection (face shields. 12 N.6 Sulfuric-tartarate-molybdate solution (STMS).9 Cuvettes..such as acidity. Prepare fresh daily. trace pure grade 6. and 60 mL 5.2 Mechanical reciprocating shaker. Use safety showers and eyewash stations to dilute spilled acids and bases.. 6.7 Ascorbic acid solution. or safety glasses). 5. with tips 2500 µL and 10 mL 5. and nylon thread. When preparing reagents. dissolve 0. Safety Wear protective clothing (coats.7 Dispenser. converted to bicarbonate form by soaking bags overnight in 1. Reagents 6. Dissolve 60 g of ammonium molybdate tetrahydrate [(NH4)6Mo7O24·4H2O] in 200 mL of boiling RODI water. aprons. Store in a refrigerator. Mix 25 mL of STMS solution with 800 mL of RODI water. 6. Dilute to volume with NaCl solution and invert to mix thoroughly. and printer 6. exercise special care. long stem.5 Filter paper. Ann Arbor. Dissolve 58. Varian Australia Pty Ltd. Store in a dark bottle in the refrigerator. sleeve guards. Eberbach 6000. 6. Whatman 42. goggles. 5. Eberbach Corp. Sefar America. Store in a polyethylene bottle.

air-dry soil to nearest mg on an electronic balance and place in a 250-mL polyethylene bottle. keep soil suspension for the next extraction.5. 7. Transfer sample to shaker.0.6 Transfer bottle to shaker and shake for 1 h at 100 oscillations min-1 at room temperature (20 °C± 2°C). Add 100 mL RODI water to bottle. After shaking. and SSL standard.5 – 7. and 0. blanks.4 Remove P from resin by lifting resin bag out of soil suspension and rinsing with 5 mL RODI water to remove attached soil particles.14.0. Analyze samples within 72 h.0 mL of concentrated HCl to each SPCS. After shaking. Also transfer a 1mL aliquot of the each SPCS to a plastic cup. 0. Store in a refrigerator.10 Standard P calibration solutions (SPCS) or working standards. 7.11 Quality Control Samples: 0.4 1. To seven 100-mL volumetric flasks add as follows: 6.10.5 – 7. remove P from resin as described in Section 7.0 mg P L-1 = 3.7 0.3 Place another 4-g resin bag in the soil suspension and control sample.2 3.0 M NaCl solution and 4.0 mL WSSPS Add 70 mL of 1.1 Weigh 2 g of <2-mm or fine-grind.0 mL WSSPS 6. 6. 4. remove P from resin as described in Section 7.5 Place resin bag in a 125-mL polyethylene bottle containing 50 mL of 1.25. 2.5 0. Add 2 mL concentrated HCl to each bottle.1 mg L-1 solution made from SSPS.10. 7.6. If necessary.0 mL WSSPS 6. 7.10. Filter if soil particles are observed in the extract. Use two replicates for each soil sample in addition to a control treatment where all steps of the extraction process are performed in the absence of soil.0 mg P L-1 = 1. Prepare fresh weekly. 7. Use a clean pipette tip for each sample and SPCS. Procedure 7.3 2. Invert to mix thoroughly. Shake for 1 h at 100 oscillations min-1 at room temperature (20°C ± 2°C).10.0 mg P L-1 = 2.0 mL WSSPS 6. 7.10.0.5 mL WSSPS 6. 7. 7. selected SPCS.0 mL WSSPS 6.0.5 mg P L-1 = 0.0 M NaCl solution. 1. Allow to cool and dilute to mark with 1.6 0.0 mg P L-1.1 4.4 and then proceed with Sections 7.0 mg P L-1 = 0.0 M NaCl solution. Transfer sample to shaker. then store samples at 4°C.25 mg P L-1 = 0.14.10.25 mL WSSPS 6.8 Use the pipette to transfer a 1-mL aliquot of the sample to a plastic cup. Add RODI water to soil suspension.0 mg P L-1 = 4.2 Place 4-g resin bag in the soil suspension and control sample. Allow to equilibrate to room temperature before use. 0.4 and then proceed with Sections 7. Shake for 23 h at 100 oscillations min-1 at room temperature (20°C ± 2°C). 221 .10.7 Transfer extracting solutions to 60-mL polyethylene bottles. If extracts are not to be determined immediately after collection. 3.

10. 2nd ed. Olsen. Agron. and D. and P. Swirl to mix.E. Rejection criteria for SPCS. Phosphorus. if performed R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = Conversion factor to kg-basis E = Sample weight (g) 9. 8.10 Transfer sample extract and SPCS to cuvettes. and Plant Anal. and if SSL standard >± 20% mean.) Methods of soil analysis. 403-430.11 Set the spectrophotometer to read at 882 nm. References Elrashidi. Rejection criteria for batch. 11. Calculations Convert extract P (mg L-1) to soil P (mg kg-1) as follows: Soil P (mg kg -1) =[ (A x B x C x R x 1000)/E] where: A = Sample extract reading (mg L-1) B = Extract volume (L) (0. and L. A technique to estimate release characteristics and runoff phosphorus for agricultural land. 2003. WI. Mays. Commun. Autozero with calibration blank. 7. Complete all readings within 2-h period since blue color may fade after this period. In A.R. ASA and SSSA. Soil Sci. if blanks as samples >0. p. Keeney (eds. Chemical and microbiological properties.12 Calibrate the instrument using the SPCS. The data system will then associate the concentrations with the instrument responses for each SPCS. Report Report data to the nearest 0.. M. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.055) C = Dilution. if R2 <0. Miller. dilute sample extracts with extracting solution and re-analyze. Part 2. Record results to the nearest 0.13 Run samples using calibration curve. S. Sample concentration is calculated from the regression equation.L. 7. Jones. Sommers. 7.7.01: If SPCS as samples >±20%. Page..99. Madison. R.9 Dispense 4 mL of the WAMS to sample aliquot and to each SPCS. 34:1759-1790. M.14 If samples are outside the calibration range.01unit for the sample extract and each SPCS.E.R. 222 . Monogr.D. 9.H. 1982. The color reaction requires a minimum of 20 min before analyst records readings. 7.1 mg P kg-1 soil.A. 7.

0-mg sensitivity 5.4 Filter paper. Application Phosphorus occurs in soil in both the solution and solid phase. The water or dilute salt extracts represent an attempt to approximate the soil solution P concentration. 50-mm diameter 223 . The sample is then centrifuged until solution is free of soil mineral particles. 30 min (4D2a1) UV-Visible Spectrophotometer. aprons. and then filtered until clear extracts are obtained. Many metal salts are extremely toxic and may be fatal if ingested. Whatman No. 1982). Thoroughly wash hands after handling these metal salts.1 Electronic balance. and sediments (National Research Council. Summary of Method A 2. 200 oscillations min-1. Restrict the use of concentrated H2SO4 and HCl to a fume hood. which are very sensitive for P.. As an index of P availability. Eberbach 6000. Equipment 5. 50-mL.Soil Tests (4D) Aqueous Extraction (4D2) Single-Point Extraction (4D2a) 1:10. 60° angle. are based on the principle that in an acid molybdate solution containing orthophosphate ions. 1958). Eberbach Corp. 2. Use safety showers and eyewash stations to dilute spilled acids and bases.5-g sample of <2-mm.01 M CaCl2). a phosphomolybdate complex forms that can be reduced by ascorbic acid. goggles.. and substances that influence the oxidation-reduction conditions of the system (Olsen and Sommers. 1982). polyethylene 5. Interferences The Mo blue methods. silicates. and gloves) and eye protection (face shields. These forms are well documented but questions still remain concerning the exact nature of the constituents and ionic forms found in water. or safety glasses).2 Mechanical reciprocating shaker. sleeve guards. 42. 1982) and (2) to determine the composition of the soil solution so that the chemical environment of the plant roots may be defined in quantitative terms (Adams. dilute salt extracts (e. O. Safety Wear protective clothing (coats. Water soluble P has been defined as P measured in water. When preparing reagents. Data are reported as mg P kg-1 soil (4D2a1a1).g. Absorbance of the solution is read using a spectrophotometer at 882 nm. 3. 5. Even though the water soluble fraction principally consists of inorganic orthophosphate ions. the objectives of this method are (1) to determine the P concentration level in the soil extract that limits plant growth (Olsen and Sommers. These forms influence P availability in relation to root absorption and plant growth. SnCl2. arsentes. soils. and P loadings. ±1. 4. 1993). Ann Arbor. runoff and water quality problems. air-dry soil is mechanically shaken for 30 min in 25-mL of reverse osmosis deionized water. displaced soil solutions. and other reducing agents to a Mo color. or saturation paste extracts (Olsen and Sommers. MI 5. 150 mm 5. exercise special care. Use sodium bicarbonate and water to neutralize and dilute spilled acids. <2 mm (4D2a1a1a-b1) 1. there is evidence that some organic P is also included (Rigler. The intensity of blue color varies with the P concentration but is also affected by other factors such as acidity. long stem. The sum of water soluble P and pH 3 extractable P has also been defined as the available P in runoff (Jackson. 1974). 1968).5 Funnel. 1 1⁄2 in strokes. Dual-Beam (4D2a1a) Phosphorus (4D2a1a1) Air-dry or Field-Moist.3 Centrifuge tubes.

Thermo IEC.4394 g primary standard grade anhydrous potassium dihydrogen phosphate (KH2PO4) that has been dried for 2 h at 110°C in about 800 mL RODI water. electronic digital.2908 potassium antimony tartarate [K(SbO)C4H4O6·1/2H2O] in 100 mL RODI water.10 5. Procedure 7.2 0.6 mg P L-1 = 1. Reagents 6. 6. Store in polyethylene containers. Store in dark bottle and refrigerate (reagent A). with Cary WinUV software. Make fresh weekly. Place the sample in shaker and shake for 30 min at 200 oscillations min-1 at room temperature (20°C± 2°C). 100-mL.8 5. 1-cm light path. Dilute to volume with RODI water and invert to thoroughly mix. In addition. trace pure grade 6. If sample is moist. mix thoroughly.0 mL WSSPS 6. and 0. Needham Heights.3 Molybdate solution.0 mg P L-1. with tips 2500 µL and 10 mL Cups.2 Sulfuric acid (H2SO4).7 5. Make fresh daily. 2-L Pipettes.0 mL WSSPS 6.112 g of ascorbic acid in 400 mL of reagent A and mix (reagent B). plastic Cuvettes. concentrated. 10. Cary 50 Conc.2 Add 25. MA Volumetric flasks.1 Weigh 2.0 mg P L-1.0 mg P L-1 = 0. Make fresh daily. Computer. H2SO4 diluted to 1-L). plastic.0 mL of RODI water to sample.7. Dissolve 12. dark. 0.6 Working stock standard P solution (WSSPS). 4. 100.7. Store in a refrigerator.. 6. 6.2 mg P L-1 = 0. 36 N. Varian Australia Pty Ltd. Dissolve 0.5 Stock standard P solution (SSPS). 0. pipet 100 mL SSPS and in 700 mL RODI water. dissolve 0. Add these two dissolved reagents to 1-L 5 N H2SO4 (141 mL conc. Varian Australia Pty Ltd.7 Standard P calibration solutions (SPCS) or working standards.2.5 0. and invert to thoroughly mix.6 5.1 Reverse osmosis deionized (RODI) water. 0.4 Ascorbic acid: Dissolve 2.6. 6.11 5.1 0. air-dry soil to nearest mg on an electronic balance and place into a 50-mL centrifuge flask.5 g of air-dry soil. weigh enough soil to achieve ≈ 2. and 25-mL Bottles.0 g ammonium molybdate tetrahydrate [(NH4)6Mo7O24·4H2O] in approximately 250 mL RODI water. 0. Dilute to volume with RODI water and invert to thoroughly mix.5 mL WSSPS 6.0 mg P L-1. Daigger Scientific Dispenser.0 mL WSSPS (blank) Add 4 mL reagent B. and selected SPCS. Centra GP-8.7. dilute each SPCS to mark with RODI water (extracting solution).5 mL WSSPS 6. 7.5. To five 25-mL volumetric flasks add as follows: 6.14 Centrifuge. and dilute with RODI water to 2-L. UV-Visible.1 mg L-1 solution made from SSPS.4 0. ASTM Type I grade of reagent water 6.7.4 mg P L-1 = 1.5 g of <2-mm or fine-grind. In a 1-L volumetric flask. In a 1-L volumetric flask. 224 .3 0. and printer 6. Varian. plastic.8. 2500 µL and 10 mL. 6.4.8 Quality Control Samples: 0.12 5.5-mL. SSL soil standard is routinely included in a batch for quality control.8 mg P L-1 = 2. Prepare fresh daily. 30 mL or 10 mL Spectrophotometer. 2-L. 7.9 5.7. blanks.13 5.

Soil solution. add 4-mL reagent B and 19 mL RODI water. p. Maximum intensity develops in 10 min. If extracts are not to be determined immediately after collection. p. if R2 <0.7.5 Transfer SPCS and sample extracts into 4. Sample concentration is calculated from the regression equation. required (125) C2 = Dilution. Carson (ed. 1993. Charlottesville. 7. 7. Rejection criteria for SPCS. 1974. N. Olsen. if SPCS as samples > ± 20%. and if SSL standard > ± 20% mean. Report Report data to the nearest 0. 1982. Record results to the nearest 0. S. Madison. decant. Jackson. filter. Inc.01. Sommers. Natl. 8. F. Analyze samples within 24 h. and D. Press of Virginia.3 Remove the sample from the shaker. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 7. Calculations Convert extract P (mg L-1) to soil P (mg kg-1) as follows: Soil P (mg kg-1) = [(A x B x C1 x C2 x R x 1000)/E] where: A = Sample extract reading (mg kg-1) B = Extract volume (L) C1 = Dilution.L. Keeney (eds. Page. ASA and SSSA. 11. An agenda for agriculture. WI.4 Pipet 2-mL of sample extract into plastic cup. 10.L. In A. if blanks as samples > 0.R. Acad. M... 1958. Agron.01 unit for the sample extract and each SPCS. References Adams. Autozero with calibration blank. VA.H. 225 . and collect extract in receiving cup.7 Calibrate the instrument using the SPCS. 7. Univ. 7.5-mL cuvettes.W. Monogr. R. Miller. 2nd ed. The data system will then associate the concentrations with the instrument responses for each SPCS. Prentice-Hall.J. Phosphorus.E. Centrifuge at 3000 rpm for 20 min. and L. Englewood Cliffs. 441-481. Rejection criteria for batch.9 If samples are outside the calibration range. National Research Council. In E. DC.8 Run samples using calibration curve. 7.6 Set spectrophotometer to 882 nm. Part 2. Color is stable for 24 h. if performed R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = Conversion factor to kg-basis E = Sample weight (g) 9.99. Chemical and microbiological properties. Soil and water quality. Committee on long-range soil and water conservation. Press. Washington. Soil chemical analysis.) Methods of soil analysis.) The plant root and its environment. then store samples at 4°C. dilute samples with extracting solution and rerun.R.1 mg P kg-1 soil. 9. 403-430.

and P loadings. 1983. 1974). Adv. 1958). Revised March.1. Method I2601-78. 3. Water soluble P has been defined as P measured in water. The water or dilute salt extracts represent an attempt to approximate the soil solution P concentration. Soil Tests (4D) Aqueous Extraction (4D2) Single-Point Extraction (4D2a) 1:10.005 mg P L-1 positive error in orthophosphate (LACHAT.G. Menzel.in the sample. displaced soil solutions. and sediments (National Research Council.W. 1968. 30 min (4D2a1) Flow Injection. U.S.g. and then filtered until clear extracts are obtained. Glassware should be washed with 1:1 HCl and rinsed with deionized water. 1982) and (2) to determine the composition of the soil solution so that the chemical environment of the plant roots may be defined in quantitative terms (Adams. U.Rigler.N. Interferences Silica forms a pale blue complex which also absorbs at 880 nm. soils. 1982). Even though the water soluble fraction principally consists of inorganic orthophosphate ions. Methods for determination of inorganic substances in water and fluvial sediments. air-dry soil is mechanically shaken for 30 min in 25-mL of reverse osmosis deionized water (RODI). U. Method 365. Methods for chemical analysis of water and wastes. These forms are well documented but questions still remain concerning the exact nature of the constituents and ionic forms found in water. As an index of P availability.5-g sample of <2-mm. 1993). if they are used. These forms influence P availability in relation to root absorption and plant growth. This ion reacts with ammonium molybdate and antimony potassium tartrate under acidic conditions to form a complex. Chapter Al. 226 . the objectives of this method are (1) to determine the P concentration level in the soil extract that limits plant growth (Olsen and Sommers. or saturation paste extracts (Olsen and Sommers. 1993. Sharpley.01 M CaCl2). Glassware contamination is a problem in low-level P determinations. Book 5. and R. A. The impact of soil and fertilizer phosphorus on the environment. 1987. Data are reported as mg P kg-1 soil (4D2a1b1). Absorbance is proportional to the concentration of PO43. dilute salt extracts (e. 2. Agron. 1968). 0. 41:297-324. Further observations inconsistent with the hypothesis that the molybdenum blue method measures orthophosphate in lake water. Geological Survey. there is evidence that some organic P is also included (Rigler. Automated Ion Analyzer (4D2a1b) Phosphorus (4D2a1b1) Air-Dry or Field-Moist. runoff and water quality problems. A flow injection automated ion analyzer is used to measure the orthophosphate ion (PO43-). 1983. Department of Interior. 1993). The sample is then centrifuged until solution is free of soil mineral particles. The sum of water soluble P and pH 3 extractable P has also been defined as the available P in runoff (Jackson. EPA-600/4-79-020. Summary of Method A 2. 1993)..S.S. Environmental Protection Agency. Limnology and Oceanography 13:7-13. This complex is reduced with ascorbic acid to form a blue complex which absorbs light at 880 nm. < 2 mm (4D2a1b1a-b1) 1. Commercial detergents should rarely be needed but.. Application Phosphorus occurs in soil in both the solution and solid phase. F. use P-free preparation for lab glassware (LACHAT. This interference is generally insignificant as a Si concentration of approximately 30 mg SiO2 L-1 would be required to produce a 0.

6. orthophosphate in waters. long stem. Milwaukee. Eberbach 6000. 50-mm diameter 5. compressed gas 6.2 Helium. Treatment with bisulfite will also remove the interference due to arsenates (LACHAT.5 Stock antimony potassium tartrate solution. Store in dark bottle and refrigerate. WI 5. add about 500 mL RODI water. MA 5. concentrated. sleeve guards. plastic.8 Bottles. 42. LACHAT Instruments. Ann Arbor. WI 5.3 Mechanical reciprocating shaker. Thermo IEC.16 Pipettes. Thoroughly wash hands after handling these metal salts.9 Cups. 25-mL (standards) 5. 60° angle. plastic 5. Equipment 5. QuikChem Method (10-115-01-1-A.17 Vials.4 Centrifuge. then add 35. QuikChem AE. 30 mL or 10 mL 6. 4.0-mg sensitivity 5. MI 5. trace pure grade 6.13 Automated Dilution Station. 227 . and gloves) and eye protection (face shields. with computer and printer 5. 1-L 5. Dilute to volume with RODI water and invert three times. Stir for 4 h. Whatman No.19 Dispenser. Milwaukee. Safety Wear protective clothing (coats. LACHAT Instruments. Use safety showers and eyewash stations to dilute spilled acids and bases.01 to 2.7 Volumetric flasks. Use sodium bicarbonate and water to neutralize and dilute spilled acids.14 Sample Processing Module (SPM) or channel. 6. Degas with helium ≈ 5 min. WI.18 Culture tubes.6 Molybdate color reagent. Milwaukee. 200 oscillations min-1. electronic digital.Concentrations of ferric ion >50 mg L-1 will cause a negative error due to competition with the complex for the reducing agent ascorbic acid. Eberbach Corp. Milwaukee.0 mL concentrated sulfuric acid (CAUTION: The solution will get very hot!).6 Funnel. glass.0 g ammonium molybdate tetrahydrate [(NH4)6Mo7O24·4H2O] in approximately 800 mL RODI water. Reagents 6. 5. 150 mm 5.15 Computer. ±1. add 72 mL stock antimony potassium tartrate solution and 213 mL stock ammonium molybdate solution. Swirl to mix. Samples high in Fe can be pretreated with sodium bisulfite to eliminate this interference. Dilute to the mark with RODI water and invert to thoroughly mix. Milwaukee.0 g antimony potassium tartrate (potassium antimony tartrate hemihydrate [K(SbO)C4H4O6·1/2H2O] in approximately 800 mL RODI water.3 Sulfuric acid (H2SO4).1 Reverse osmosis deionized (RODI) water.5 Filter paper. In 1 L volumetric flask. 1 1⁄2 in strokes. In 1-L volumetric flask dissolve 40. aprons. LACHAT Instruments. or safety glasses). 50-mL. goggles. polyethylene 5. Needham Heights.10 Flow Injection Automated Ion Analyzer.. In 1-L flask. 0. and printer 5. 36 N. Dilute to the mark and invert to thoroughly mix. When it can be comfortably handled. Restrict the use of concentrated H2SO4 and HCl to a fume hood. 2500 µL and 10 mL.11 XYZ Sampler. ASTM Type I grade of reagent water 6.12 Reagent Pump. Centra GP-8. LACHAT Instruments. LACHAT Instruments. 1-L and 250-mL 5. 2500 µL and 10 mL 5. 1993). WI. plastic.4 Stock ammonium molybdate solution. dark. Store in plastic and refrigerate. with tips.2 Centrifuge tubes. dissolve 3. WI 5. Many metal salts are extremely toxic and may be fatal if ingested. WI 5. LACHAT Instruments. with QuikChem software. 10-mL (samples) 5.1 Electronic balance. When preparing reagents.0 mg P L-1). exercise special care. Milwaukee.

Shake for 30 min at 200 oscillations min-1 at room temperature (20°C± 2°C).4394 g primary standard grade anhydrous potassium dihydrogen phosphate (KH2PO4) that has been dried for 2 h at 110°C in about 800 mL RODI water. Do not degas.4 0.00 mg P L-1= 0 mL WSSPS (blank) Dilute each SPCS to the mark with RODI water and invert to thoroughly mix. 7.0 mL WSSPS 6. Working stock standard P solution (WSSPS).0 mg P L-1 (ppm). Invert to thoroughly mix.2 1.6.0 mg P L-1. dissolve 60.1 2. If extracts are not to be determined immediately after collection.6 Refer to the operating and software reference manuals for LACHAT set-up and operation.2 Add 25. Centrifuge at 2000 rpm for 10 min decant. 7.20. 0.01 mg P L-1 = 0. 0.10 6.0 g dodecyl sulfate (CH3(CH2)11OSO3Na). To seven 250-mL volumetric flasks add as follows: 6. In a 1-L volumetric flask. 1.0.0.00 mg P L-1. dissolve 0. Do not degas.11 Ascorbic acid reducing solution. Pump RODI water through system for 20 min. Dissolve 65 g sodium hydroxide (NaOH) and 6 g tetrasodium ethylenediamine tetraacetic acid (Na4EDTA) in 1. 7. and 0.7 Turn main power switch "ON" and allow 15 min for heater module to warm up to 37°C. 10.25 mL WSSPS 6.7 6. Procedure 7.0 mL WSSPS 6. and collect extract in receiving cup.6 0.5 g of <2-mm or fine-grind. 7.11.5 g of air-dry soil. If sample is moist. Make fresh weekly. Degas with helium ≈ 5 min.11.11. Dilute to volume and invert to thoroughly mix. 7. In l-L volumetric flask.25 mL WSSPS 6. 7.05. Standard P calibration solutions (SPCS) or working standards. air-dry soil to nearest mg on an electronic balance and place into a 50-mL centrifuge tube. Stock standard P solution (SSPS).0 mL WSSPS 6.20 mg P L-1 = 5. Store in a refrigerator.7 0.11. dilute 100. 0.5.1 Weigh 2.8 6.5 Transfer SPCS standards into plastic vials and place in descending order in XYZ sample trays marked "Standards".11. Transfer the sample to the shaker. In a 1-L volumetric flask.0 L RODI water.11. Analyze samples within 24 h. 7. Optional: After dilution to volume and degassing.0 mg P L-1 = 50. weigh enough soil to achieve ≈ 2. 7.5 ml WSSPS 6.11.05 mg P L-1 = 1. set speed to 35.0 g ascorbic acid in about 700 mL RODI water. 2. filter.0 mg P L-1 = 25. Sodium hydroxide .5 0. Prepare fresh weekly.01.9 6. dissolve 1. 100.8 On reagent pump. Store in polyethylene containers. Make fresh daily.3 0.0 mL of RODI water to sample.0 mL SSPS to mark with RODI water. Make fresh daily. 0.3 Remove the sample from the shaker. then store samples at 4°C. 228 .EDTA rinse.5 mg P L-1 = 12.4 Transfer sample extracts into culture tubes and place in XYZ sample trays marked "Samples". Dilute to volume with RODI water and invert three times.

7.00.5 Calibration strategy for segments A .G (0.2 Inject to start of peak period: 18 s. 7.20. 7. The data system then associates the concentrations with the instrument response for each SPCS.S.13 Some of the method parameters as they relate to calibration standards are as follows: 7. and chord 1 .4 with the most signal-to-noise ratio in chords 1 and 5.11 On computer main menu. Scatter is indicative of air bubbles and irregular reagent flow.3 The protocol (replications) for the calibration standards is as follows: AA BB CCC DDDD EEEE FFFF GG 7. Geological Survey 1993). and then "Edit" to create new sample tray followed by "Submit" to run new sample tray. i.14.50.00 mg P L-1) with a data format of ####.14. The most peak area should be between chords 2 .13. no manual timing. U. Department of Interior.7.20 to 0..3 Inject to end of peak period: 52 s 7. To see if peaks are being timed correctly. 0. 1. 7.4 The check standard is 2. Some of these parameters have been modified from the QuikChem Method 10-115-011-A. where standard assumptions are in effect. A calibration passes only when both criteria are met.14 Method parameters in relation to timing are as follows: 7.10 Pump reagents into manifold. calibration strategies are based on the full chord.0 to 0.99. Maximum number of consecutive trays between check standard is one.05. 0.5 are sections of peak from start of peak to end of peak. A good baseline needs to be smooth and at zero absorbance.e.1 Cycle period: 40 s 7. Continue this step and observe baseline.9 On computer main menu.D (2.13.13.S. The normal strategy requires a minimum correlation coefficient of 0.13. 0.14.13. Environmental Protection Agency.00.15 Method parameters in relation to data presentation are as follows: 229 . and maximum elapse time between check standards is 2 h.5. 0. select water soluble P method.4 Automatic timing. data rounded to 3 places. Chord 0 is full chord. scan across correlation coefficients for all chords 1 . "Tray Definition and Submit".13. Modifications are primarily related to the criteria and strategies for calibration standards and to injection timing. and 0. 7. 7. In addition. System unit receives the downloaded method and initializes it.1 There are 7 calibration standards (2. select "Methods" and then "Analysis Select and Download". Both segments require a maximum standard deviation in slope of 50%. Also observe for any back-pressure in manifold tubing.0 mg P L-1.###.6 The instrument is calibrated with the injection of SPCS. 7.14.01. select "Samples". 7. orthophosphate in waters (U. On method list. 7. Strategies are user designated. 1983.2 The segments/boundaries for the calibration standards are A .D and D . 7. maximum number of consecutive samples between check standard is 60.20 mg P L-1) and D . LACHAT Instruments.G are normal.12 Method parameters specific to water soluble P are defined within the "Method Definition" menu. 1993. 7.00 mg P L-1).

16 Method parameters in relation to data results are as follows: 7. Soil chemical analysis. LACHAT Instruments. Inc. 11. place the transmission lines into the NaOH . 1993. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 7. M.17 Refer to the "Method Definition" for water soluble P for other method parameters not discussed here.20 Upon completion of run.. 1958. dilute samples with extracting solution and reanalyze. 1974. References Adams.1 Top Scale Response: 0.18 Run samples using calibration curve. LACHAT Instruments.1 Set Default Chord to 3.16. Press of Virginia.15. In E.02 to 2. 10. WI.2 Bottom Scale Response: 0. 8. Univ.19 If samples are outside calibration range. Jackson. Soil solution. p. Prentice-Hall. 441-481..EDTA solution. 7.0 mg P L-1. Then place these lines in RODI water and pump for an additional 5 min and proceed with the normal "Shut-down" procedure.15.00 abs 7. Sample concentration is calculated from the regression equations.W. 0. Carson (ed. Report results to the nearest 0.1 mg P kg-1 soil.7. Milwaukee. orthophosphate in waters. Calculations Convert extract P (mg L-1) to soil P (mg kg-1) as follows: Soil P (mg kg-1) = [(A x B x C x R x 1000/E] where: A = Sample extract reading (mg L-1) B = Extract volume (L) D = Dilution. NJ. Englewood Cliffs. Charlottesville. 7. Report Report data to the nearest 0.01 unit for the sample extract and each SPCS. 7. 230 . 6645 West Mill Rd.50 abs 7. QuikChem method 10-115-01-1-A.) The plant root and its environment.L. F. This change must be made to both the sample and the calibration RDF's. Pump the solution for approximately 5 min to remove any precipitated reaction products. if performed R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = Conversion factor to kg-basis E = Sample weight (g) 9.

Interferences Many procedures may be used to determine P.National Research Council. 1987.1. The NH4F complexes the aluminum in solution and limits readsorption of P on iron oxides (Kuo. 9. EPA-600/4-79-020. 221. Adsorbed phosphorus is the in the anion form adsorbed by different charged surface functional groups that have varying degrees of adsorption affinity. 3. and time. Geological Survey. Press. Chapter Al. Method 365. The impact of soil and fertilizer phosphorus on the environment. Soil and water quality. The Bray P-1 has limited ability to extract P in calcareous soils due to the neutralization of the dilute acid by carbonates. Studies have shown that incomplete or excessive extraction of P to be the most significant contributor to interlaboratory variation.. U. F. Page. 1988). Methods for determination of inorganic substances in water and fluvial sediments. 1993.W. Absorbance of the solution is read using a spectrophotometer at 882 nm. Olsen.S. and partially extracts iron phosphates compounds. Acad.H. the Olsen method is preferred. Phosphorus. Agron.L. Summary of Method A 2. shaking rate.N. <2 mm (4D3a1a-b1) 1. Committee on long-range soil and water conservation.S. 1983. 403-430. Limnology and Oceanography 13:7-13. and then filtered until clear extracts are obtained. and L. Monogr. U. Revised March. Further observations inconsistent with the hypothesis that the molybdenum blue method measures orthophosphate in lake water. Chemical and microbiological properties.. Dual-Beam (4D3a) Phosphorus (4D3a1) Air-Dry or Field-Moist. 1993. 1983. This procedure has been shown to be satisfactory for some calcareous soils (Smith et al. DC. In general. Keeney (eds. 2. The sample is centrifuged until solution is free of soil mineral particles.G. Soil Tests (4D) Bray P-1 Extraction (4D3) UV-Visible Spectrophotometer. and R. Part 2. 231 . In A. U. The acid solubilizes calcium and aluminum phosphates. Sharpley. A. Application The Bray P-1 procedure is widely used as an index of available P in the soil. Book 5. 1982. 41:297-324. 221. An agenda for agriculture.) Methods of soil analysis.5-g soil sample is shaken with 25 mL of Bray P-1 extracting solution for 15 min. Miller. Menzel. This extraction uses the ascorbic acid-potassium antimony-tartarate-molybdate method. WI. The FiskeSubbarrow method is less sensitive but has a wider range before dilution is required (North Central Regional Publication No. Environmental Protection Agency. Department of Interior. North Central Regional Publication No. An alternative procedure for calcareous soils is to use the Bray P-1 extracting solution at a 1:50 soil:solution ratio. and D. Madison. Method I2601-78. this method has been most successful on acid soils (Olsen and Sommers. acidified ammonium fluoride solution. 2nd ed.R. 1968.E. ASA and SSSA. Sommers. 1957. Adv. Bray and Krutz (1945) originally designed the Bray P-1 extractant to selectively remove a portion of the adsorbed form of P with the weak. Methods for chemical analysis of water and wastes. S. For calcareous soils. 1982). The Bray P-1 procedure is sensitive to the soil/extractant ratio. Rigler.. Agron. 1996).R. A 2-mL aliquot is diluted with 8-mL of ascorbic acid molybdate solution. p. Washington.S. Data are reported as mg P kg-1 soil (4D3a1). R. Natl. 1988).

Thoroughly wash hands after handling these metal salts.2 Mechanical reciprocating shaker. Mix 25 mL of STMS solution with 800 mL of RODI water. ±0. 0. 9-cm diameter 5. 2500 µL and 10 mL. Cary 50 Conc. plastic 5. Make fresh daily.1 Electronic balance.455 g of antimony potassium tartarate (potassium antimony tartarate hemihydrate [K(SbO)C4H4O6·1/2H2O] in the ammonium molybdate solution. Ann Arbor. In a 1-L volumetric flask.5-mL. Add 10 mL of ascorbic acid solution and dilute to 1 L with RODI water.12 Computer.4 Funnel.0 mg P L-1 = 12. To six 250-mL volumetric flasks add as follows: 6.03 N NH4F. Make fresh weekly.7 Pipettes.5 mL WSSPS 232 . Make fresh weekly.0 mg P L-1. 6.4. Add 200 mL of 1. Dilute to 1-L volume with extracting solution water and invert to thoroughly mix. 4. 0.6 Centrifuge. Dissolve 60 g of ammonium molybdate tetrahydrate [(NH4)6Mo7O24·4H2O] in 200 mL of boiling RODI water. Needham Heights. Allow to cool to room temperature.3 Centrifuge tubes. Thermo IEC. Dual-View.6 ± 0.7 Ascorbic acid solution. Use sodium bicarbonate and water to neutralize and dilute spilled acids.. Slowly and carefully add 700 mL of concentrated H2SO4. Whatman 42. Prepare fresh daily. Store in a polyethylene bottle. Allow to stand at least 1 h before using. 60° angle.11 Spectrophotometer.4394 g primary standard grade anhydrous potassium dihydrogen phosphate (KH2PO4) that has been dried for 2 h at 110°C in about 800 mL extracting solution.0 N HCl and dilute to 8 L with RODI water. goggles.1 5. Cool and dilute to 1 L with RODI water. with Cary WinUV software. 6. Varian. 200 oscillations min-1. 1 N.10 Dispenser.33 mL of concentrated HCl to RODI water and dilute to 1-L volume. aprons. 4. MI 5.88 g of NH4F in 4 L RODI water. Equipment 5. Use safety showers and eyewash stations to dilute spilled acids and bases. Reagents 6.2 Hydrochloric acid (HCl). Centra GP-8. trace pure grade 6.8.. Store in polyethylene containers.8 Working ascorbic acid molybdate solution (WAMS). 5.10-mg sensitivity 5. Restrict the use of concentrated H2SO4 and HCl to a fume hood. 1 1⁄2 in strokes. 50-mm diameter 5. polyethylene 5. Eberbach 6000.3 HCl.10 Standard P calibration solutions (SPCS) or working standards. The solution pH should be 2. 0. 6. plastic. 6. 6. Safety Wear protective clothing (coats.9 Working stock standard P solution (WSSPS). 2. Eberbach Corp.5 Bray No. 6. Dissolve 1. 100. Many metal salts are extremely toxic and may be fatal if ingested.6 g of ascorbic acid in RODI water and dilute to 50 mL with RODI water.9 Cuvettes. Carefully add 83. 0. Store in a refrigerator.025 N HCl and 0. concentrated.0.4 Sulfuric acid (H2SO4). or safety glasses). Dissolve 8. ASTM Type I grade of reagent water 6.10. Allow to equilibrate to room temperature before use. 5. concentrated.0. Varian Australia Pty Ltd. 36 N 6. electronic digital. Dissolve 6. 30 mL or 10 mL 5. long stem. ashless. MA 5.1 Reverse osmosis deionized (RODI) water.5 Filter paper. sleeve guards. Store in a refrigerator. with tips 2500 µL and 10 mL 5. exercise special care.0. 12 N. Daigger Scientific 5. and printer 6.6 Sulfuric-tartarate-molybdate solution (STMS).8 Cups.4. and gloves) and eye protection (face shields. Varian Australia Pty Ltd. 5. UV-Visible. dissolve 0.5. 1-cm light path. When preparing reagents. 50-mL. 1 Extracting solution. Store in the dark in the refrigerator.0 mg P L-1.

7. Also transfer a 2mL aliquot of each SPCS to a plastic cup.0 mg P L-1 = 10.10. Shake for 15 min at 200 oscillations min-1 at room temperature (20°C).0 mL WSSPS 6.0 mg P L-1 = 0 mL WSSPS (blank) Dilute each SPCS to the mark with extracting solution and invert to thoroughly mix.2 Dispense 25.4 mg P L-1 = 1. 7. The data system will then associate the concentrations with the instrument responses for each SPCS.8 Set the spectrophotometer to read at 882 nm. If extracts are not to be determined immediately after collection. Rejection criteria for batch.10.0 mL WSSPS 6. Centrifuge at 2000 rpm for 10 min.0 mL WSSPS 6. Sample concentration is calculated from the regression equation. 7.0 mg P L-1 = 5. 8.8 mg P L-1 = 2.9 Calibrate the instrument using the SPCS.11 If samples are outside the calibration range. if SSL standard > ± 20% mean. International Soil Exchange) from The Netherlands are routinely included in a batch for quality control. decant.4 0. air-dry soil to nearest mg on an electronic balance and place into a 50-mL centrifuge tube. If SPCS as samples > ± 20%. where MAD = median of absolute deviations.10.2 4.01 unit for the sample extract and each SPCS. filter. Procedure 7. and selected SPCS. Analyze samples within 72 h. blanks.10 Run samples using calibration curve.0 mL WSSPS 6.6 Dispense 8 mL of the WAMS to sample aliquot and to each SPCS.99.0 mL of extracting solution to tube. Rejection criteria for SPCS. 7. Use a clean pipette tip for each sample and SPCS. 6. if R2 <0. and collect extract in receiving cup.1 mg L-1 solution made from SSPS.5 g of <2-mm or fine-grind.3 2.5 g of air-dry soil. then store samples at 4°C. 7. 7.6 0. Record results to the nearest 0. dilute sample extracts with extracting solution and re-analyze.01. 7. SSL soil standard and WEPAL ISE’s (Wageningen Evaluating Programmes for Analytical Laboratories. Autozero with calibration blank.5 0. If sample is moist. In addition.10.3 Transfer the sample in the shaker. and if ISE > (3 x MAD). The color reaction requires a minimum of 20 min before analyst records readings. Swirl to mix.6.7 Transfer sample extract and SPCS to cuvettes.11 Quality Control Samples: 0. 7. Calculations Convert the extract P (mg L-1) to soil P (mg kg-1) as follows: 233 .1 Weigh 2. 7.5 Use the pipette to transfer a 2-mL aliquot of the sample to a plastic cup.4 Remove the sample from the shaker. weigh enough soil to achieve ≈ 2. 7.10. if blanks as samples > 0. 7.

Bray P-1 and Mehlich No. Chemical and microbiological properties. OH. of IL. Report Report data to the nearest 0. Soil Sci. 59:39-45. MS. this method has been most successful on acid soils (Olsen and Sommers. if performed R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = Conversion factor to kg-basis E = Sample weight (g) 9.E.W. Application The Bray P-1 procedure is widely used as an index of available P in the soil. The NH4F complexes the aluminum in solution and limits readsorption of P on iron oxides (Kuo.) Methods of soil analysis. Miller. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Ellis. No.H. B. WI. Madison. 5. 1957. acidified ammonium fluoride solution. p. and Olsen sodium-bicarbonate are closely associated with pH buffering of extractant (acid versus alkaline) (Burt et al. ND. F. and partially extracts iron phosphates compounds. 403-430.to three-fold. Exp. ASA and SSSA. Phosphorus. IN. KS. North Central Regional Publication No. 9. Determination of total. Monogr.R. Stn.L... MN. References Bray. In D. R. organic. 1996). Olsen. Soc. In general. and J. MI. 10. SD. ASA and SSSA. Am. Kurtz. 3 are nearly comparable in their abilities to extract native P but exceed Olsen sodium-bicarbonate method by two. WI.1 mg P kg-1 soil. Phosphorus. 1982). Recommended chemical soil test procedures for the North Central region. Kuo. Keeney (eds. Sparks (ed. Soil Sci. 1988. Agron. Soil Tests (4D) Bray P-1 Extraction (4D3) Flow-Injection.. Proc. In A. 234 . 2002). WI. Grava. and L. and L. and USDA cooperating. NE.Soil P (mg kg-1) = =[(A x B x C x R x 1000)/E] where: A = Sample extract reading (mg L-1) B = Extract volume (L) C = Dilution. 221. Page.R. 3. Chemical methods. 1982. <2 mm (4D3b1a-b1) 1.G. For most soils. and available forms of phosphorus in soils. 1945. indicating that predictive models for Bray P-1. Madison. Part 3. Mehlich No. Bray and Krutz (1945) originally designed the Bray P-1 extractant to selectively remove a portion of the adsorbed form of P with the weak.L. 869-919. Automated Ion-Analyzer (4D3b) Phosphorus (4D3b1) Air-Dry or Field-Moist. and D.) Methods of soil analysis. Part 2. Sommers. Agric. IA. 1996.H. Smith. Use of acid-fluoride solutions for the extraction of available phosphorus in calcareous soils and in soils to which rock phosphate has been added. 21:400-404. S. The acid solubilizes calcium and aluminum phosphates. Adsorbed phosphorus is the in the anion form adsorbed by different charged surface functional groups that have varying degrees of adsorption affinity.T. S.. R. The Bray P1 has limited ability to extract P in calcareous soils due to the neutralization of the dilute acid by carbonates. 2nd ed. p. 11.

Interferences Silica forms a pale blue complex which also absorbs at 660 nm. 25-mL (standards) 5.9 Cups. 3. Samples high in iron can be pretreated with sodium bisulfite to eliminate this interference.19 Culture tubes. WI 5. Data are reported as mg P kg-1 soil (4D3b1). WI 5.in the sample. Milwaukee.16 Computer. Milwaukee. sleeve guards. and H2SO4 to a fume hood. 50-mm diameter 5. This interference is generally insignificant as a silica concentration of approximately 4000 mg L-1 would be required to produce a 1 mg L-1 positive error in orthophosphate (LACHAT Instruments. Milwaukee.3 Mechanical reciprocating shaker. electronic digital. Milwaukee.. Thoroughly wash hands after handling these metal salts.4 to 20 mg P L-1). glass. Use sodium bicarbonate and water to neutralize and dilute spilled acids. 150 mm 5. Milwaukee. Eberbach Corp. dark.4 Centrifuge.6 Funnel. Milwaukee. or safety glasses). Eberbach 6000. MA 5.15 Sample Processing Module (SPM) or channel. plastic. The sample is then centrifuged until solution is free of soil mineral particles. Centra GP-8. the sensitivity of the method is reduced. 1989). 5. With increasing acidity. MI 5. The determination of phosphorus is sensitive to variations in acid concentrations in the sample since there is no buffer. standards. aprons. Concentrations of ferric iron greater than 50 mg L-1 will cause a negative error due to competition with the complex for the reducing agent ascorbic acid. Equipment 5. Absorbance is proportional to the concentration of PO43. Whatman No. 1 1⁄2 in strokes. LACHAT Instruments. QuikChem Method (12-115-01-1-A. 0. 50-mL. LACHAT Instruments. Use safety showers and eyewash stations to dilute spilled acids and bases. 1989).0-mg sensitivity 5. A flow injection automated ion analyzer is used to measure the orthophosphate ion (PO43-). LACHAT Instruments. 30 mL or 10 mL 5. 200 oscillations min-1. WI.7 Volumetric flasks.11 Flow Injection Automated Ion Analyzer. LACHAT Instruments. exercise special care.10 Dispenser. and blanks should be prepared in a similar matrix. and printer 5.13 Reagent Pump. Samples. with QuikChem software. 2500 µL and 10 mL.14 Automated Dilution Station. LACHAT Instruments.5-g soil sample is mechanically shaken for 15 min in 25-mL of Bray P-1 extracting solution. WI 5. 4. Treatment with bisulfite will also remove the interference due to arsenates (LACHAT Instruments. goggles. When preparing reagents. and then filtered until clear extracts are obtained. orthophosphate in waters. This complex is reduced with ascorbic acid to form a blue complex which absorbs light at 660 nm. and gloves) and eye protection (face shields. 1-L 5. 10-mL (samples) 235 . Needham Heights. plastic. with computer and printer 5.2. Safety Wear protective clothing (coats. WI 5.12 XYZ Sampler. with tips 2500 µL and 10 mL 5. Thermo IEC.5 Filter paper.18 Vials. long stem. plastic 5.8 Bottles. WI.1 Electronic balance. Ann Arbor. 42. NH4F. ±1.2 Centrifuge tubes. QuikChem AE. LACHAT Instruments. Many metal salts are extremely toxic and may be fatal if ingested. Summary of Method A 2.17 Pipettes. 60° angle. polyethylene 5. This ion reacts with ammonium molybdate and antimony potassium tartrate under acidic conditions to form a complex. Restrict the use of concentrated HCl. 1-L and 250-mL 5.

12 Sodium hydroxide .00 mg P L-1= 0 mL WSSPS (blank) Dilute each SPCS to the mark with extracting solution and invert to thoroughly mix. 6. To 1-L container.4 mL concentrated H2SO4 and bring volume with RODI water. compressed gas 6. Degas with helium ≈ 5 min.9 Molybdate color reagent. dissolve 0.11 0.14.14. Degas with helium ≈ 15 min.7 Stock ammonium molybdate solution.0 N HCl and dilute to 8 L with RODI water. Store in dark bottle and refrigerate. Store in a polyethylene bottle.6 ± 0. and 0.4 Sulfuric acid (H2SO4). Dissolve 65 g sodium hydroxide (NaOH) and 6 g tetrasodium ethylenediamine tetraacetic acid (Na4EDTA) in 1.0 g dodecyl sulfate (CH3(CH2)11OSO3Na). Dilute to the mark with RODI water and invert to thoroughly mix. Procedure 7. Reagents 6.88 g of NH4F in 4 L RODI water. trace pure grade 6.10 Ascorbic acid reducing solution. 6. 36 N. Store in a refrigerator.03 M NH4F.5 g of <2-mm or fine-grind.05.33 mL of concentrated HCl to RODI water and dilute to 1-L volume. Dilute to volume with RODI water and invert to thoroughly mix. Dilute to the mark and invert to thoroughly mix. Carefully add 83. Make fresh weekly. and 0. trace pure grade 6.1 Weigh 2. Prepare fresh daily.0 mg P L-1. Store in polyethylene containers. Store in refrigerator.80 mg P L-1 = 2 mL WSSPS 6.00 mg P L-1 = 10 ml WSSPS 6. 236 . (CAUTION: The solution will get very hot!) Invert to thoroughly mix. If sample is moist. 12.4 0. dissolve 1. 4. Do not degas.4394 g primary standard grade anhydrous potassium dihydrogen phosphate (KH2PO4) that has been dried for 2 h at 110°C in about 800 mL extracting solution. 0. dissolve 3. The solution pH should be 2. concentrated. In a 1-L volumetric flask.6. 6.2 Helium. 6.00. In 1 L volumetric flask. 0.0 g ammonium molybdate tetrahydrate [(NH4)6Mo7O24·4H2O] in approximately 800 mL RODI water. Store in plastic and refrigerate.8 M H2SO4 Carrier.EDTA rinse.6 Bray No. After dilution to volume and degassing.14 Standard P calibration solutions (SPCS) or working standards. add 44.13 Working stock standard P solution (WSSPS). dissolve 60. add 72 mL stock antimony potassium tartrate solution and 213 mL stock ammonium molybdate solution.2 12. In l-L volumetric flask. 20. Dilute to volume with RODI water and invert to thoroughly mix. Dilute to 1-L volume with extracting solution and invert to thoroughly mix.000 mg P L-1 as PO43-.00 mg P L-1 = 50 mL WSSPS 6.3 Hydrochloric acid (HCl).5 HCl.00. Degas with helium ≈ 5 min. 1 Extracting Solution. Stir for 4 h. concentrated. air-dry soil to nearest mg on an electronic balance and place into a 50-mL centrifuge tube. In 1-L flask.1 Reverse osmosis deionized (RODI) water.8 Stock antimony potassium tartrate solution.5 g of air-dry soil. 100.00 mg P L-1 = 30 mL WSSPS 6. ASTM Type I grade of reagent water 6. Make fresh weekly.025 M HCl. 6. 6.800. In 1-L volumetric flask dissolve 40. 6.5 0. To five 250-mL volumetric flasks add as follows: 6.0 g ascorbic acid in about 700 mL RODI.0 L RODI water.3 4. 12 N. Add 200 mL of 1.14.14. 6.14.0 g antimony potassium tartrate (potassium antimony tartrate hemihydrate [K(SbO)C4H4O6·1/2H2O] in approximately 800 mL RODI water. weigh enough soil to achieve ≈ 2. 1 N.00.1 20. Dissolve 8. 7. 6. Allow to equilibrate to room temperature before use.

7. 7. 7. filter.13 Method parameters specific to Bray P-1 are defined within the "Method Definition" menu.7 Refer to the operating and software reference manuals for LACHAT set-up and operation. System unit receives the downloaded method and initializes it. 1993). and collect extract in receiving cup. 7. 0. 7. Centrifuge at 2000 rpm for 10 min.5 Transfer sample extracts into culture tubes and place in XYZ sample trays marked "Samples". Shake for 15 min at 200 oscillations min-1 at room temperature (20°C± 2°C). Some of these parameters have been modified from the QuikChem Method 12-115-01-1-A. 7. then store samples at 4°C. Maximum number of consecutive trays between check standard is one..00. Scatter is indicative of air bubbles and irregular reagent flow. Department of Interior. Geological Survey. 1983. select "Methods" and then "Analysis Select and Download". 4. U. and maximum elapse time between check standards is 2 h. "Tray Definition and Submit".14.11 Pump reagents into appropriate chambers of the manifold. Continue this step and observe baseline.3 The protocol (replications) for the calibration standards is as follows: AA BB CC DDD EEE. 7. decant.3 Transfer the sample to the shaker.C (20. 7.00. data rounded to 3 places.6 Transfer SPCS standards into plastic vials and place in descending order in XYZ sample trays marked "Standards". 7. 7. select Bray P-1 Method. Also observe for any back-pressure in manifold tubing.7. 7. Modifications are primarily related to the criteria and strategies for calibration standards and to injection timing.9 On reagent pump.14.1 There are 5 calibration standards (20.S.###.00 mg P L-1) with a data format of ####. 7.8 Turn main power switch "ON" and allow 15 min for heater module to warm up to 60°C. i. 1989. 237 . On method list.4 Remove the sample from the shaker. Environmental Protection Agency.12 On computer main menu. If extracts are not to be determined immediately after collection. C . and then "Edit" to create new sample tray followed by "Submit" to run new sample tray.0 mL of extracting solution to tube.10 On computer main menu.14. 12. and 0.2 The segments/boundaries for the calibration standards are A .80. 7.0 to 0.14. LACHAT Instruments. 7. A good baseline needs to be smooth and at zero absorbance.E (4.0 mg P L-1).00. 7.2 Dispense 25.4 The check standard is 20.0 to 4.S.0 mg P L-1.14 Some of the method parameters as they relate to calibration standards are as follows: 7. maximum number of consecutive samples between check standard is 60. select "Samples". orthophosphate in soils (U. set speed to 35. Analyze samples within 72 h.e.0 mg P L-1).

99.14. The data system then associates the concentrations with the instrument response for each SPCS.14.3 Inject to end of peak period: 46 s 7. To see if peaks are being timed correctly.5 are sections of peak from start of peak to end of peak.17 Refer to the "Method Definition" for Bray P-1 for other method parameters not discussed here. 7.15 Method parameters in relation to timing are as follows: 7. Strategies are user designated.15. dilute samples with extracting solution and reanalyze. 8. Chord 0 is full chord. and chord 1 . if performed R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 238 .EDTA solution.5. Calculations Convert extract P (mg L-1) to soil P (mg kg-1) as follows: Soil P (mg kg-1) = [(A x B x C x R x 1000)/E] where: A = Sample extract reading (mg L-1) B = Extract volume (L) C = Dilution. Sample concentration is calculated from the regression equations.18 Run samples using calibration curve.6 The instrument is calibrated with the injection of SPCS.7. 7. In addition.16.E are normal. place the transmission lines into the NaOH . calibration strategies are based on the full chord. Pump the solution for approximately 5 min to remove any precipitated reaction products.20 Upon completion of run.16.19 If samples are outside calibration range. 7.50 abs 7. Report results to the nearest 0.4 Automatic timing. where standard assumptions are in effect.15.1 Top Scale Response: 0.00 abs 7. scan across correlation coefficients for all chords 1 .15. Manual timing may be helpful in this method. The most peak area should be between chords 2 . 7.1 Cycle period: 40 s 7.4 with the most signal-to-noise ratio in chords 1 and 5. Both segments require a maximum standard deviation in slope of 50%.16 Method parameters in relation to data presentation are as follows: 7. 7. A calibration passes only when both criteria are met. Then place these lines in RODI water and pump for an additional 5 min and proceed with the normal "Shut-down" procedure.2 Inject to start of peak period: 18 s.01 unit for the sample extract and each SPCS.5 Calibration strategy for segments A – C and C . 7. The normal strategy requires a minimum correlation coefficient of 0.15. 7.2 Bottom Scale Response: 0.

E.1 mg P kg–1 soil. and L. R. References Bray. Geological Survey. 2002. Miller. QuikChem method 12-115-01-1-A. and partially extracts iron phosphate compounds. It was originally designated by Bray and Kurtz (1945) to extract the easily acid soluble P a well as a fraction of adsorbed phosphates. Report Report data to the nearest 0. Sommers. Determination of total. ASA and SSSA. p.D. Phosphorus. Monogr. Madison. The NH4F complexes the aluminum in solution and limits readsorption of P on iron oxides (Kuo. 11. 1993. Chemical and microbiological properties. 9..C. The sample is centrifuged until solution is free of soil mineral particles. and L. In A. p.S.2. Soil Sci. 1982. ASA and SSSA. 5.H. Page. Benham. Application The Bray P-2 procedure functions to extract a portion of the plant available P in the soil.S. Method 353. Kurtz. Soil Sci.. <2 mm (4D4a1a-b1) 1.E.4 to 20 mg P L-1. Sparks (ed. but it is not as widely used by soil testing laboratories as Bray P-1. EPA-600/4-79-020. phosphorus as orthophosphate.) Methods of soil analysis. Commun. WI.S. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. U. The HCl solublizes calcium and aluminum phosphates. Olsen. 1996. Bray P-2 Extraction (4D4) UV-Visible Spectrophotometer.H. 6645 West Mill Rd. 1989. M. Milwaukee. 1983. Wilson. Summary of Method A 2. Dual-Beam (4D4a) Phosphorus (4D4a1) Air-Dry or Field-Moist. WI. Environmental Protection Agency.R. Method I2601-78.L. U. Department of the Interior. 0. 1945. Part 2. 10. Madison. U. Methods for determination of inorganic substances in water and fluvial sediments. 239 . S. Book 5. Mays. Part 3. 2. Burt. organic. LACHAT Instruments. The higher acid concentration of the Bray P-2 should allow greater extraction of P in calcareous soils compared to Bray P-1.R.A. and available forms of phosphorus in soils. Methods for chemical analysis of water and wastes. Phosphorus. 1983. Phosphorus characterization and correlation with properties of selected benchmark soils of the United States. 1996). and then filtered until clear extracts are obtained.) Methods of soil analysis.5-g soil sample is shaken with 25 mL of Bray P-2 extracting solution for 15 min. A 2-mL aliquot is diluted with 8-mL of ascorbic acid molybdate solution. R.1000 = Conversion factor to kg-basis E = Sample weight (g) 9. Agron.L. The difference is a slightly higher concentration of HCl (0. S. Kuo. Data are reported as mg P kg-1 soil (4D4a1). In D.025 N to 0. Absorbance of the solution is read using a spectrophotometer at 882 nm.. Chemical methods. 869-919. 403-430. and D.1 N) in the Bray P-2.T. WI.. Keeney (eds. Chapter Al. No. 33:117-141.. Plant Anal. 59:39-45. It has a similar composition to Bray P-1 extraction solution. Revised March. 2nd ed. R. LACHAT Instruments. and M.

50-mm diameter 5. Dissolve 60 g of ammonium molybdate tetrahydrate [(NH4)6Mo7O24·4H2O] in 200 mL of boiling RODI water.88 g of NH4F in 4 L RODI water. Whatman 42.03 N NH4F.6 g of ascorbic acid in RODI water and dilute to 50 mL with RODI water. 200 oscillations min-1. Dissolve 8. The Fiske-Subbarrow method is less sensitive but has a wider range before dilution is required (North Central Regional Publication No. trace pure grade 6. Ann Arbor. 4.4 Sulfuric acid (H2SO4)..10 Dispenser. Dissolve 1. 1 1⁄2 in strokes. concentrated. and printer 6. Studies have shown that incomplete or excessive extraction of P to be the most significant contributor to interlaboratory variation. 0. 5. ASTM Type I grade of reagent water 6. Thoroughly wash hands after handling these metal salts.12 Computer. 6. 4. 1957.5 Bray No.7 Pipettes.33 mL of concentrated HCl to RODI water and dilute to 1-L volume. 50-mL. Dual-View. polyethylene 5.5 Filter paper. The higher acid concentration of the Bray P-2 should allow greater extraction of P in calcareous soils compared to Bray P-1.6 Sulfuric-tartarate-molybdate solution (STMS). Many metal salts are extremely toxic and may be fatal if ingested. 9-cm diameter 5. but it is not as widely used by soil testing laboratories as Bray P-1. Interferences Many procedures may be used to determine P.8 Cups.3 HCl. 6. with Cary WinUV software.7 Ascorbic acid solution. 1 N.9 Cuvettes.0 N HCl and dilute to 8 L with RODI water. goggles. 1988). Varian..3. Eberbach Corp. long stem. When preparing reagents. Allow to cool to room temperature. 2 Extracting solution. Use sodium bicarbonate and water to neutralize and dilute spilled acids. concentrated. For calcareous soils. 240 . Restrict the use of concentrated H2SO4 and HCl to a fume hood. Varian Australia Pty Ltd. 12 N. Reagents 6.4 Funnel. Eberbach 6000..1 Reverse osmosis deionized (RODI) water. ±0. 36 N 6. MA 5. Cary 50 Conc. plastic. the Olsen method is preferred. Safety Wear protective clothing (coats. electronic digital. UV-Visible. Varian Australia Pty Ltd. 6.1 Electronic balance. sleeve guards. aprons.455 g of antimony potassium tartarate (potassium antimony tartarate hemihydrate [K(SbO)C4H4O6·1/2H2O] in the ammonium molybdate solution. and time. Slowly and carefully add 700 mL of concentrated H2SO4. 2500 µL and 10 mL. or safety glasses). The Bray procedure is sensitive to the soil/extractant ratio. 221. and gloves) and eye protection (face shields.11 Spectrophotometer. 221. shaking rate. Carefully add 83. MI 5. Add 800 mL of 1.1 N HCl and 0. Equipment 5. Daigger Scientific 5. 60° angle. This extraction uses the ascorbic acid-potassium antimony-tartarate-molybdate method.5-mL. Use safety showers and eyewash stations to dilute spilled acids and bases. North Central Regional Publication No. Dissolve 6. Store in a polyethylene bottle. with tips 2500 µL and 10 mL 5. Store in the dark in the refrigerator.10-mg sensitivity 5. An alternative procedure for calcareous soils is to use the Bray P-1 extracting solution at a 1:50 soil:solution ratio. Centra GP-8. 30 mL or 10 mL 5. Needham Heights. Thermo IEC. plastic 5.3 Centrifuge tubes. ashless. exercise special care.6 Centrifuge. Make fresh daily. 1988).2 Hydrochloric acid (HCl). 5. This procedure has been shown to be satisfactory for some calcareous soils (Smith et al. Cool and dilute to 1 L with RODI water. 1-cm light path.2 Mechanical reciprocating shaker.

Mix 25 mL of STMS solution with 800 mL of RODI water.0 mL of extracting solution to tube.0 mL WSSPS 6.0. then store samples at 4°C. blanks. 7. 7. 7.1 5.5 g of air-dry soil. 7.1 mg L-1 solution made from SSPS.3 2. and selected SPCS.9 Working stock standard P solution (WSSPS).3 Transfer the sample in the shaker. 100. Centrifuge at 2000 rpm for 10 min. Use a clean pipette tip for each sample and SPCS.99. Store in a refrigerator. In a 1-L volumetric flask. Also transfer a 2mL aliquot of each SPCS to a plastic cup.9 Calibrate the instrument using the SPCS. 5. To six 250-mL volumetric flasks add as follows: 6. 2.8. If sample is moist. filter.10. If extracts are not to be determined immediately after collection. Allow to stand at least 1 h before using.4 Remove the sample from the shaker. 241 .4394 g primary standard grade anhydrous potassium dihydrogen phosphate (KH2PO4) that has been dried for 2 h at 110°C in about 800 mL extracting solution.0 mL WSSPS 6. Procedure 7. and collect extract in receiving cup.10.0. Add 10 mL of ascorbic acid solution and dilute to 1 L with RODI water. Autozero with calibration blank.0 mg P L-1 = 10.0 mg P L-1 = 12.8 mg P L-1 = 2.4 mg P L-1 = 1. dissolve 0. Prepare fresh daily.10 Standard P calibration solutions (SPCS) or working standards.8 Set the spectrophotometer to read at 882 nm. SSL soil standard and WEPAL ISE’s (Wageningen Evaluating Programmes for Analytical Laboratories.4 0.2 4. The color reaction requires a minimum of 20 min before analyst records readings. air-dry soil to nearest mg on an electronic balance and place into a 50-mL centrifuge tube. Make fresh weekly.0 mg P L-1.Working ascorbic acid molybdate solution (WAMS). In addition. 6.8 6.11 Quality Control Samples: 0.0 mg P L-1 = 0 mL WSSPS (blank) Dilute each SPCS to the mark with extracting solution and invert to thoroughly mix. Store in polyethylene containers.5 0.10. Allow to equilibrate to room temperature before use.0 mg P L-1. Shake for 15 min at 200 oscillations min-1 at room temperature (20°C).0 mg P L-1 = 5.7 Transfer sample extract and SPCS to cuvettes.5 Use the pipette to transfer a 2-mL aliquot of the sample to a plastic cup.0 mL WSSPS 6.5 mL WSSPS 6. The data system will then associate the concentrations with the instrument responses for each SPCS.0 mL WSSPS 6. 0.10. if R2 <0. Analyze samples within 72 h. Store in a refrigerator.10. weigh enough soil to achieve ≈ 2.2 Dispense 25. 7. Swirl to mix.0. International Soil Exchange) from The Netherlands are routinely included in a batch for quality control. 0. decant. 4.6 Dispense 8 mL of the WAMS to sample aliquot and to each SPCS.5 g of <2-mm or fine-grind. 7. 0. Make fresh weekly.4. Rejection criteria for SPCS. 7.10.1 Weigh 2. 6. 6. Dilute to 1-L volume with extracting solution water and invert to thoroughly mix.6 0. 7. 7.

where MAD = median of absolute deviations. Keeney (eds. MI.. WI. Olsen. In A.) Methods of soil analysis. <2 mm (4D5a1a-b1) 1. 1996). References Bray. If SPCS as samples > ± 20%. Sparks (ed. and D..H. MS.E. NE. ND. Part 2. Soc. Solubility of Ca-phosphate in 242 .5. ASA and SSSA. if performed R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = Conversion factor to kg-basis E = Sample weight (g) 9.10 Run samples using calibration curve. 7. Calculations Convert the extract P (mg L-1) to soil P (mg kg-1) as follows: Soil P (mg kg-1) = [(A x B x C x R x 1000)/E] where: A = Sample extract reading (mg L-1) B = Extract volume (L) C = Dilution.L. This extractant is most applicable to neutral to calcareous soils (Buurman et al. 10. S. IN.) Methods of soil analysis. 1982.01 unit for the sample extract and each SPCS. and if ISE > (3 x MAD). Proc. Smith. and available forms of phosphorus in soils. 21:400-404. OH. p.7. R. Ellis. and L. Exp. ASA and SSSA. In D.. and L. Agron. 59:39-45. S. Grava. Kurtz. Sommers. No. of IL.. Madison.5 M sodium bicarbonate solution at pH 8.W. Sample concentration is calculated from the regression equation. Soil Tests (4D) Olsen Sodium-Bicarbonate Extraction (4D5) UV-Visible Spectrophotometer. 869-919. Kuo. 1945. Dual-Beam (4D5a) Phosphorus (4D5a1) Air-Dry or Field-Moist. 11. Chemical methods. MN.G. Monogr.11 If samples are outside the calibration range. Application Olsen extractant is 0. Phosphorus. Report Report data to the nearest 0. 1988. Chemical and microbiological properties. 403-430.R. 9. Page. North Central Regional Publication No. Phosphorus. Stn. Record results to the nearest 0. organic. 9.01. Recommended chemical soil test procedures for the North Central region. WI.L. R. 5. SD. Miller. B. Determination of total. 221.1 mg P kg-1 soil. Use of acid-fluoride solutions for the extraction of available phosphorus in calcareous soils and in soils to which rock phosphate has been added. Soil Sci. 2nd ed. WI. Rejection criteria for batch. Am.R. Part 3. and USDA cooperating. IA.H. KS. Agric. and J.T. p. dilute sample extracts with extracting solution and re-analyze. Soil Sci. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. if SSL standard > ± 20% mean. 1996. F. if blanks as samples > 0. 1957. Madison.

ASTM Type I grade of reagent water 6.3 Sulfuric acid (H2SO4). 1-cm light path.5-mL. a phosphomolybdate complex forms that can be reduced by ascorbic acid. 1000µL and 10 mL. 4. While Mehlich No. 1999). Bray P-1. Eberbach Corp. 3 on calcareous soils (R2= 0. long stem.10 Cuvettes. relationships developed between some P tests (e.918). 1 M. and substances that influence the oxidation-reduction conditions of the system (Olsen and Sommers. with Cary WinUV software. 3. even though the quantity of Mehlich No. Ann Arbor. 30 mL or 10 mL 5. Use safety showers and eyewash stations to dilute spilled acids and bases. 5.4 Funnel. UV-Visible. Allow to cool. Safety Wear protective clothing (coats. Mehlich No.5 Filter paper. 1982).. polyethylene 5. 3) may have limited predictive capability with increasing soil P content (Burt et al.. and Olsen sodium-bicarbonate are linearly related. Interferences The Mo blue methods. 1000µL and 10 mL 5. 2. 4. Data are reported as mg P kg-1 soil (4D5a1). carefully add 56 mL concentrated H2SO4 to 150 mL RODI water. 4 M.11 Spectrophotometer.8 Cups.g. are based on the principle that in an acid molybdate solution containing orthophosphate ions. 3 extractable P is considerably higher (Soil and Plant Analysis Council. plastic 5. Varian Australia Pty Ltd. 6. Varian Australia Pty Ltd.2 Mechanical reciprocating shaker. 1999).1 Electronic balance. Needham Heights. and gloves) and eye protection (face shields. 36 N. Olsen P. alkaline. aprons. 5. or neutral soils in increased because of the precipitation of Ca++ as CaCO3 (Soil and Plant Analysis Council. Dilute 5-mL of sample extract with 5-mL of color reagent. Restrict the use of concentrated H2SO4 and HCl to a fume hood. trace pure grade 6. Daigger Scientific 5. 60° angle. exercise special care.. Reagents 6. Varian. MA. and other reducing agents to a Mo color.1 Reverse osmosis deionized (RODI) water. goggles. Eberbach 6000. electronic digital. and printer 6. Summary of Method A 1. silicates. 1 1⁄2 in strokes. arsenates.calcareous. ±1. Centra.0-g soil sample is shaken with 20 mL of Olsen sodium-bicarbonate extracting solution for 30 min. The sample is centrifuged until solution is free of soil mineral particles. Thermo IEC. Whatman 42. Use sodium bicarbonate and water to neutralize and dilute spilled acids. concentrated. To 250-mL volumetric. 50-mm diameter 5. 150 mm 5. Thoroughly wash hands after handling these metal salts. The intensity of blue color varies with the P concentration but is also affected by other factors such as acidity.2 Sulfuric acid (H2SO4). Make to final volume with RODI water. which are very sensitive for P. Thermo IEC.9 Dispenser.0-mg sensitivity 5.3 Centrifuge tube. SnCl2.4 NaOH. GP-8. Cary 50 Conc. Olsen extractant correlates with Mehlich No. Many metal salts are extremely toxic and may be fatal if ingested.7 Pipettes.12 Computer. plastic. Equipment 5. When preparing reagents. 3. 50 mL. and then filtered until clear extracts are obtained. with tips. or safety glasses). 200 oscillations min-1. MI 5. Dual-View. sleeve guards. Dissolve 4 g NaOH in 100 mL RODI water. 2000). Invert to thoroughly mix. 5. 243 .6 Centrifuge. The absorbance of the solution is read using a spectrophotometer at 882 nm.

1mg P L-1 solution made from SSPS.13 Quality Control Samples: 0.0 g of air-dry soil. Store in the dark in the refrigerator.5 6.Olsen Sodium Bicarbonate Extracting solution ( 0.12. To 6-L container.0 mg P L-1. To six 50-mL volumetric flasks. Make fresh weekly.2 1. then store samples at 4°C. 7.1 2.3 Transfer the sample to the shaker.8. Make to final volume.12. 6. 1. 0. 6.3 1. 6. 0.4 0.4394 g primary standard grade anhydrous potassium dihydrogen phosphate (KH2PO4) that has been dried for 2 h at 110°C in about 800 mL extracting solution. 6. Check pH every day.5 0.5 with 1M NaOH.75% ascorbic acid.0. add 50 mL 4 M H2SO4.1 Weigh 1. 4%.0 mL of extracting solution to tube. air-dry soil to the nearest mg into a 50-mL centrifuge tube.5 M NaHCO3).12.2 mg P L-1 = 15 mL WSSPS 6. filter. 1. Prepare fresh daily. Pipet 10 mL of 100 mg P L-1 SSPS to 250-mL volumetric flask. add as follows: 6. dissolve 0. or working standards. 6.275% potassium antimony – (III) oxide tartarate. Store in a refrigerator. Shake for 30 min at 200 oscillations min-1 at room temperature (20°C± 2°C). SSL soil standard and WEPAL ISE’s (Wageningen Evaluating Programmes for Analytical Laboratories. International Soil Exchange) from The Netherlands are routinely included in a batch for quality control.12 Standard P calibration solution (SPCS). Dilute to 250-mL volume with extracting solution and invert to thoroughly mix. Store in polyethylene containers.7 Potassium antimony – (III) oxide tartarate.2 Dispense 20. Store in the refrigerator. 6. Dissolve 1.0 g of <2mm or fine-grind. and 200 mL RODI water. Make fresh weekly. Mix thoroughly. and 0. Allow to equilibrate to room temperature before use. If sample is moist.8 mg P L-1 = 10 mL WSSPS 6. dissolve 252 g NaHCO3 in RODI water.0 mg P L-1 = 0 mL WSSPS (blank) Dilute each SPCS to mark with extracting solution and invert to thoroughly mix. 100.6 Ammonium molybdate. Centrifuge at 2000 rpm for 10 min. 6. 2. To a 500-mL bottle. If extracts are not to be determined immediately after collection. 7. Prepare fresh daily. 7. Dilute to 1-L volume with extracting solution and invert to thoroughly mix. In addition.11 Working stock standard P solution (WSSPS). 4.9 Color developing reagent.4 Remove the sample from the shaker.10 Stock standard P solution (SSPS).12.0 mg P L-1= 25 mL WSSPS 6. Make fresh weekly. Adjust the pH to 8. decant.75%. 1. Dissolve 4 g of [(NH4)6Mo7O24·4H2O] in 100-mL volumetric with RODI water.4.2. 30 mL 1.75 g ascorbic acid in 100 mL RODI water.0 mg P L-1. blanks. 244 . Dilute to volume with RODI water. 15 mL 4% ammonium molybdate.6 0. 0. In a 1-L volumetric flask. Store in the refrigerator.12. Analyze samples within 72 h.0 mg P L-1.6 mg P L-1 = 20 mL WSSPS 6.275%. 5 mL 0. Procedure 7. and collect extract in receiving cup. Mix well after each addition. and selected SPCS.12.6. Dissolve 0. weigh enough soil to achieve ≈ 1. 6.275 g [K(SbO)C4H4O6·1/2H2O] in 100 mL RODI water.8 Ascorbic acid.4 mg P L-1 = 5 mL WSSPS 6. 7.

Color will remain stable for 24 h. 11. Calculations 8. Backhuys Publ. 7.. if R2 <0. Velthorst. and M.A.7 Transfer sample extract and SPCS to cuvettes. and if ISE > (3 x MAD). van Lagen. Autozero with calibration blank. Record results to the nearest 0. 7. B. R. if performed R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = Conversion factor to kg-basis E = Sample weight (g) 9. Soil Sci. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. if SSL standard > ± 20% mean. M. Also transfer a 5mL aliquot of each SPCS to a plastic cup. 1996. 7. if SPCS as samples > ± 20%.6 Dispense 5 mL of color developing reagent to sample aliquot and to each SPCS. Report Report data to the nearest 0. Plant Anal.. 7. P.11 If samples are outside calibration range. E. Phosphorus characterization and correlation with properties of selected benchmark soils of the United States. where MAD = median of absolute deviations.C.99.1 Convert the extract P (mg L-1) to soil P (mg kg –1) as follows: Soil P (mg kg-1) = [(A x B x C x R x 1000)/E] where: A = Sample extract reading (mg L-1) B = Extract volume (L) C = Dilution.8 Set the spectrophotometer to read at 882 nm.7.1 mg P kg-1 soil. if blanks as samples > 0. Mays.10 Run samples using calibration curve. Allowing 1 h for color development usually improves results. 10. Burt. and E. Sample concentration is calculated from the regression equation. Commun. Use a clean pipette tip for each sample and SPCS. Swirl to mix. 2002.9 Calibrate the instrument using the SPCS. Manual for soil and water analysis.01. 245 .D. 7. The data system will then associate the concentrations with the instrument responses for each SPCS. The Netherlands. Rejection criteria for batch. dilute sample extracts with extracting solution and re-analyze. Benham. References Buurman. Leiden. Rejection criteria for SPCS.5 Use the pipette to transfer a 5-mL aliquot of the sample to a plastic cup. Do not place sample cups close together as carbon dioxide is released and solution will bubble. 33:117-141. 8.J. Wilson.01 unit for the sample extract and each SPCS. The color reaction requires a minimum of 20 min before analyst records readings.. 7.

even though the quantity of Mehlich No. Safety Wear protective clothing (coats. The Mehlich No. aprons. and NH4OAc (Soil and Plant Analysis Council. Many metal salts are extremely toxic and may be fatal if ingested. When preparing reagents.Olsen. 3 Extraction (4D6) UV-Visible Spectrophotometer. Mehlich No.E.966) but does not correlate with Bray P-1 on calcareous soils (Soil and Plant Analysis Council. WI. Data are reported as mg P kg-1 soil (4D6a1). and then filtered until clear extracts are obtained.918). and substances that influence the oxidation-reduction conditions of the system (Olsen and Sommers. Miller. In A. Mehlich No. The intensity of blue color varies with the P concentration but is also affected by other factors such as acidity. 403-430. R. 3 extractant is neutralized less by carbonate compounds in soil than the double acid (Mehlich No. 3. 1993).R. 3 was developed by Mehlich (1984) as a multielement soil extraction (Ca. P is extracted by reaction with acetic acid and Fl compounds. 9. 1984). 3 procedure. exercise special care. P). 1999). Na. goggles. Agron. Absorbance of the solution is read using a spectrophotometer at 882 nm. and gloves) and eye protection (face shields. Chemical and microbiological properties. Council on Soil Testing and Plant Analysis. which are very sensitive for P. Thoroughly wash hands after handling these metal salts. Equipment 5.) Methods of soil analysis. Keeney (eds. Dual-Beam (4D6a) Phosphorus (4D6a1) Air-Dry or Field-Moist. Interferences The Mo blue methods. In the Mehlich No. Part 2. and other reducing agents to a Mo color. or safety glasses). ±1. Page. 1. Extraction of P by Mehlich No. 1982). 1999). CRC Press. 5. are based on the principle that in an acid molybdate solution containing orthophosphate ions. 3 is a used an index of available P in the soil. silicates.L. 2.5-mL of sample extract with 13. Madison. FL. 2. Use safety showers and eyewash stations to dilute spilled acids and bases. with ascorbic acid most commonly used by agricultural laboratories (Murphy and Riley. S. 3 is designed to be applicable across a wide range of soil properties ranging in reaction from acid to basic (Mehlich. ASA and SSSA. The sample is centrifuged until solution is free of soil mineral particles. Sommers. 4.R.. arsenates.0-mg sensitivity 246 . < 2 mm (4D6a1a-b1) 1. and D. Mg. 3 extractable P is considerably higher (Soil and Plant Analysis Council. 1982. 1999. 1962). 3 extracting solution for 5 min. 3 correlates with Olsen extractant on calcareous soils (R2= 0. Summary of Method A 2. Phosphorus. and L. p.5-g soil sample is shaken with 25 mL of Mehlich No. sleeve guards. Soil Tests (4D) Mehlich No. K. Mehlich No. Mehlich No. Mg. K. Mehlich No.H. Use sodium bicarbonate and water to neutralize and dilute spilled acids. 2nd ed. 3 can also be used to extract Ca. a phosphomolybdate complex forms that can be reduced by ascorbic acid. 1) and the Bray P-1. Handbook on reference methods for soil analysis. SnCl2. Boca Raton. 3 correlates well with Bray P-1 on acid to neutral (R2 = 0. Soil and Plant Analysis Council.5-mL of working solution. Restrict the use of concentrated H2SO4 and HCl to a fume hood. and Na in a wide range of soils and correlates well with Mehlich No. 1999). and is less aggressive towards apatite or other Ca-phosphate than the double acid and Bray P-2 extractants (Tran and Simard. Dilute 0. Monogr. Application Mehlich No.1 Electronic balance.

5. Dissolve 8.3 Centrifuge tubes. 1.8. 50-mL. 247 . Rural Route 1.8 g of ascorbic acid in RODI water and dilute to 100mL with RODI water. 1000 µL and 10 mL 5.8 0.0. dissolve 0. 4. Needham Heights. 0. 0. 200 oscillations min-1.0 mg P L-1 = 2.5 2. Store in a refrigerator. 3 Extractant.7 Pipettes. 1000 µL and 10 mL. Make fresh weekly.3 8.8. 0.5-mL.8. Allow to equilibrate to room temperature before use. Varian Australia Pty Ltd. with tips. long stem.0. Glen Rock. 6.2 N CH3COOH. Box 686. 10.6 Centrifuge. Centra. 2. PA. 4. 6.6 Working ascorbic acid molybdate solution (WAMS).0 mg P L-1. Thermo IEC. 12. Cool and dilute to 2 L with RODI water.5 mL WSSPS 6. Eberbach Corp.8. Prepare fresh daily. Eberbach 6000.11 Spectrophotometer. 50-mm diameter 5.1 Reverse osmosis deionized (RODI) water.4 4. ASTM Type I grade of reagent water 6. Store in the dark in the refrigerator.1 12. 8.5 Filter paper.001 M EDTA). concentrated. 0.0. UV-Visible.0 mg P L-1 = 10 mL WSSPS 6. 6.8.6 1.0. MI 5.015 N NH4F.9 0.10 Cuvettes. MA 5. 6.0. polyethylene 5.8. Dilute 20 mL of STMS solution and 10 mL of the ascorbic acid solution with RODI water to make 1-L.8 mg P L-1 = 2 mL WSSPS 6. Reagents 6. Dual-View.0 mg P L-1 = 30 mL WSSPS 6. Whatman 42. Ann Arbor.8.8.9 Cups.425 g of antimony potassium tartarate (potassium antimony tartarate hemihydrate [K(SbO)C4H4O6·1/2H2O] in the ammonium molybdate solution. Dissolve 2.4394 g primary standard grade anhydrous potassium dihydrogen phosphate (KH2PO4) (dried for 2 h at 110°C) in about 800 mL extracting solution. Store in polyethylene containers. 36 N.5 Ascorbic acid solution.8 Standard P calibration solutions (SPCS) or working standards. Store in a refrigerator.7 Working stock standard P solution (WSSPS). Premixed Mehlich No.0 mg P L-1 = 25 mL WSSPS 6.2 Sulfuric acid (H2SO4). Simpson Road. Varian. Daigger Scientific 5. Make fresh daily. Cary 50 Conc.8.0 mg P L-1 = 20 mL WSSPS 6.3 Mehlich No. and printer 5. 6.8 Dispenser. 100. 1 1⁄2 in strokes. 0. Hawk Creek Laboratory. Varian Australia Pty Ltd.25 N NH4NO3. 0.4 and 0.2 10. Slowly and carefully add 1400 mL of concentrated H2SO4 and mix well.7 0. Dilute to 1-L volume with extracting solution and invert to thoroughly mix. Dissolve 100 g of ammonium molybdate tetrahydrate [(NH4)6Mo7O24·4H2O] in 500 mL of RODI water.4 Sulfuric-tartarate-molybdate solution (STMS). Allow solution to come to room temperature before using. Prepare fresh weekly. GP-8.8. In nine 250-mL volumetric flasks add as follows: 6.2 6. 1-cm light path.. 17327. 30 mL or 10 mL 5.4 Funnel. electronic digital. 150 mm 5. 3 Extracting solution (0. plastic 5.13 N HNO3.0. Special-20.0 mg P L-1. plastic.0 mg P L-1 = 5 mL WSSPS 6. 60° angle.. trace pure grade 6.12 Computer with Cary WinUV software.0 mg P L-1 = 0 mL WSSPS (blank) Dilute each SPCS to the mark with extracting solution and invert to thoroughly mix. In a 1-L volumetric flask.Mechanical reciprocating shaker.4 mg P L-1 = 1 mL WSSPS 6.

if SSL standard > ± 20% mean.10 Run samples using calibration curve. if R2 <0. weigh enough soil to achieve ≈ 2. Rejection criteria for SPCS. The color reaction requires a minimum of 20 min before analyst records readings. and selected SPCS.1 mg P L -1 solution made from SSPS. Rejection criteria for batch. 7. In addition.9 Quality Control Samples: 0. if performed 248 .11 If samples are outside calibration range.7 Transfer sample extract and SPCS to cuvettes.5 Use the pipette to transfer a 1 mL (or 0. 7. The data system will then associate the concentrations with the instrument responses for each SPCS. 7.5-mL) aliquot of each SPCS to a plastic cup. 7. filter. if blanks as samples > 0. blanks.6. then store samples at 4°C. Color will remain stable for 6 h. Calculation 8. and collect extract in receiving cups. 7. SSL soil standard and WEPAL ISE’s (Wageningen Evaluating Programmes for Analytical Laboratories.4 Remove the sample from the shaker. Procedure 7.3 Transfer the sample to the shaker. air-dry soil to the nearest mg into a 50-mL centrifuge tube. Shake for 5 min at 200 oscillations min-1 at room temperature (20°C± 2°C). Sample concentration is calculated from the regression equation. 7.01 unit for the sample extract and each SPCS. Also transfer a 1 mL (or 0. dilute sample extracts with extracting solution and re-analyze. Allowing 1 h for color development usually improves results.2 Dispense 25.5-mL) aliquot of the sample to a plastic cup. 7. 7. If sample is moist.1 Weigh 2. 7. Analyze samples within 72 h. where MAD = median of absolute deviations. Centrifuge at 2000 rpm for 10 min. 7. If extracts are not to be determined immediately after collection. International Soil Exchange) from The Netherlands are routinely included in a batch for quality control.0 mL of extracting solution to the tube.6 Dispense 27 mL (or 13.99.9 Calibrate the instrument by using the SPCS. Swirl to mix. Record results to the nearest 0.8 Set the spectrophotometer to read at 882 nm. if SPCS as samples > ± 20%. 7. and if ISE > (3 x MAD). Autozero with calibration blank. decant.5 g of air-dry soil.5 g of <2-mm or fine-grind.01.5 mL) of the WAMS to sample aliquot and to each SPCS. Use a clean pipette tip for each sample and SPCS. 8.1 Convert extract P (mg L-1) to soil P (mg kg-1) as follows: Soil P (mg kg -1) = [(A x B x C x R x 1000)/E] where: A = Sample extract reading (mg L-1) B = Extract volume (L) C = Dilution.

Handbook on reference methods for soil analysis. Part 2. Commun.R. Mg. Monogr. 1993). and Zn (Elrashidi et al. Mn. 3 procedure. Cd. p. and L. 10. Fe..R. Mg. Summary of Method A 2. and R. Tran. Mehlich No. Mehlich No. 27:31-36. Mehlich No.. Additionally.5-g soil sample is shaken with 25 mL of Mehlich No. Cobalt.E. 3 extractant is neutralized less by carbonate compounds in soil than the double acid (Mehlich No.R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = Conversion factor to kg-basis E = Sample weight (g) 9. Sommers. 3 extracting solution for 5 min. Selenium.. WI. Cu. The Mehlich No. T. Soil and Plant Analysis Council. 3 correlates with Olsen extractant on calcareous soils (R2= 0. Acta. Can. 1) and the Bray P-1. Calibration standards are prepared for elemental analysis. 3 Extraction (4D6) Inductively Coupled Plasma Atomic Emission Spectrophotometer (4D6b) Axial Mode (4D6b1) Ultrasonic Nebulizer (4D6b1a) Aluminum. 15:1409-1416.R. Arsenic. S. R. Extraction of P by Mehlich No. 1992). 1984). P). In M. and Na in a wide range of soils and correlates well with Mehlich No. Iron. 1999. 3 was developed by Mehlich (1984) as a multielement soil extraction (Ca. 1982. Miller. Mehlich 3 soil text extractant: A modification of Mehlich 2 extractant. 1984. Calcium. Soil Sci. The sample is centrifuged until solution is free of soil mineral particles. Page. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Simard. In the Mehlich No.R. J.. Soil Sci. Soc. ASA and SSSA.) Methods of soil analysis. 3 can be used to extract Al. 11. Inc. Sodium. 403-430. 3 is designed to be applicable across a wide range of soil properties ranging in reaction from acid to basic (Mehlich. Olsen. Lewis Publ. FL. Plant Anal. Phosphorus. Mehlich No. K. and D. and J. and then filtered until clear extracts are obtained. Boca Raton.966) but does not correlate with Bray P-1 on calcareous soils (Soil and Plant Analysis Council. 1993.L. References Mehlich. 1962. 3 correlates well with Bray P-1 on acid to neutral (R2 = 0.) Soil sampling and methods of analysis. Copper. 2nd ed. Chemical and microbiological properties. Potassium Magnesium. 3 extractable P is considerably higher (Soil and Plant Analysis Council.918). Phosphorus. Chromium. Chem.R. 2003).. K. 3 is a used an index of available P in the soil. Pb.S. Riley. Boca Raton. even though the quantity of Mehlich No. Madison. Murphy. 1. In A. Application Mehlich No. Cadmium. Mehlich No. and is less aggressive towards apatite or other Ca-phosphate than the double acid and Bray P-2 extractants (Tran and Simard. 1999). Mehlich No. Manganese. and Zinc (4D6b1a1-18) Air-Dry or Field-Moist (4D6b1a1-18a-b1) 1. Keeney (eds. A modified single solution method for the determination of phosphate in natural waters. Mehlich III-extractable elements. Nickel. Agron. 1999). A. Ni.1mg P kg –1 soil. P is extracted by reaction with acetic acid and Fl compounds. and NH4OAc (Soil and Plant Analysis Council. 2. Mehlich No. Anal. CRC Press. FL. A 249 . Barium. Report Report data to the nearest 0. p. Na. Carter (ed. Council on Soil Testing and Plant Analysis. Lead. 2. 3 can also be used to extract Ca. 9. 43-50.H.

3.6 Centrifuge. 10. Samples and standards are matrix-matched to help reduce interferences. 6. Rural Route 1.7 Pipettes. SC. GP-8.2 Mechanical reciprocating shaker.blank of Mehlich No. Mn. Cr. PA. 10. 1000 µL and 10 mL. Make fresh weekly. Cu. An inductively coupled plasma atomic emission spectrophotometer (ICP-AES) is used for analysis. polyethylene 5.0 mm id). aprons. and Zn are determined by an inductively coupled plasma atomic emission spectrophotometer (ICP-AES) in radial mode. 200 oscillations min-1. Fe.. Ca. Ni. Reagents 6. Whatman 42. Na. Background corrections are made by ICP-AES software. K. Se.2) extracting solution. 100. Na. Al. P. 20. Restrict the use of concentrated acids to a fume hood. 4. As. Thoroughly wash hands after handling these metal salts. 0. Ba. CT. Glen Rock. 45 MHz free running.001 M EDTA). Store in a polyethylene container. ASTM Type I grade of reagent water 6. or safety glasses). Cr. 1000 mg L-1: of Al. electronic digital. K. Thermo IEC.11 RF generator. 1 1⁄2 in strokes. N069-5362 6. Cr.4 Mixed Standard High A. N069-1662. Ni. MI 5. CFT Series 5. Al. CT. Co. 3 Extractant. Perkin-Elmer Corp. Ann Arbor. Norwalk. Safety Wear protective clothing (coats. respectively: To a 500-mL volumetric. Special-20..13 Recirculating chiller. Norwalk. Invert to thoroughly mix. The concentration of Al. 5.015 N NH4F. 0. Perkin-Elmer Corp..3) and dilute to volume with Mehlich No. Ca. Neslab. 3 is prepared.996%) and Nitrogen (minimum purity=99. Mg.10 Inductively coupled plasma atomic emission spectrophotometer (ICP-AES).3 Primary standards. with tips. 100.3 Centrifuge tubes.1 Reverse osmosis deionized (RODI) water. Use sodium bicarbonate and water to neutralize and dilute spilled acids. Fe.. 20. 50-mm diameter 5. Norwalk. and Zn. Perkin-Elmer Corp. Interferences are corrected or minimized by using both an internal standard and inter-elemental correction factors.2 N CH3COOH. Norwalk.9 Cups. floor mounted power unit. 40. Centra. 250 . AS-90. plastic 5. P. Mg. 3 (Section 6. Part No. Needham Heights. Part No. As. 5. exercise special care. 17327. 100. Ba. goggles. Hawk Creek Laboratory. and 5 mL of the 1000 mg L-1 Ca. 6.14 Compressed gasses. Perkin-Elmer Corp. 0. K. Fe. Mg. 3 Extracting solution (0. Cd. 50-mL.999%) 5. Na. sleeve guards.5 Filter paper. Eberbach Corp. with WinLab software ver.13 N HNO3. 30 mL or 10 mL 5. CT. Co.8 Dispenser.25 N NH4NO3. Se. Data by this procedure (4D6b1a1-18) are reported as mg kg-1 soil.4 Funnel. add 50. 5. Many metal salts are extremely toxic and may be fatal if ingested. careful selection of specific wavelengths for data reporting is important. and 10 mg L-1 of Ca. Also. CT. and printer 5. Use safety showers and eyewash stations to dilute spilled acids and bases. Na (Section 6. 60° angle.16 Quartz torch. Argon (minimum purity=99. High Purity Standards. When preparing reagents.12 Computer. alumina injector (2. 0. K. 5. 4. MA 5.2 Mehlich No. 150 mm 5. 50. Simpson Road. Charleston.. Pb.15 Autosampler.0-mg sensitivity 5. Store in a refrigerator. Cd.1 Electronic balance. 20. Premixed Mehlich No. Box 686. long stem. Mg.1. Fe. Mn. 50. Equipment 5. Eberbach 6000. and gloves) and eye protection (face shields. Perkin-Elmer Optima 3300 Dual View (DV). Pb. 1000 µL and 10 mL 5. Cu. Interferences Spectral and matrix interferences exist. ±1.

7 6. K. K. Ba. Na. Store in a refrigerator. 0. Pb. 10. and Zn. 10.3 Transfer the sample to the shaker. respectively: To a 100-mL volumetric. Store in a refrigerator. 50. Mg.1. As. 10. 1 mg L-1 of P. Mixed Standard High B. Zn. 0. and Cr. 0. 25. Invert to thoroughly mix. Na. 0. Make fresh weekly.1 mg L-1 of P. K. 0. 0. Mn. Ni. 0.8 6. Se. then store samples at 4°C.2 Dispense 25. Store in polyethylene container. 3 extracting solution.5. 0.1. Invert to thoroughly mix. Na. add 10 mL of Mixed Standard Low B and dilute to volume with Mehlich No. Store in polyethylene container.6 6. 1. Mg.01. Ni. and Pb (Section 6. Pb. 0. Procedure Extraction of Al.5.5 mg L-1 of Ca. and 0. decant. 0. As. Fe. Store in a refrigerator.1.01. 10. 1. Cu. Make fresh weekly. If extracts are not to be determined immediately after collection. 0. and Zn 7. 1. As. Centrifuge at 2000 rpm for 10 min. 1.13 Mixed Standard Medium A. Ba. 1.5 6. Pb.1.1 and 0. respectively: To a 100-mL volumetric. Ni. Mixed Standard Very Low A. Make fresh weekly. As. 10. Mn. Store in a refrigerator. and Pb.1. Make fresh weekly. 10. 0. Se. Invert to thoroughly mix. Al. 50. Store in a refrigerator. Ni. 1. 0. Ca. add 25. 1.1. Se. Make fresh weekly. Ba. 10. respectively: To a 100-mL volumetric. 1. and 1 mL of the 1000 mg L-1 of P. Store in a refrigerator. If sample is moist. 10 mg L-1 of P.01. Invert to thoroughly mix. Fe. 0. 10. Cd. No initial dilutions of samples are necessary prior to analysis. Mg. Al. As. Use ultrasonic nebulization of sample.12 6. 0. Se. Mn. Store in a refrigerator. 0. 1. 3 extracting solution. Cd. 0. add 10 mL of Mixed Standard Medium B and dilute to volume with Mehlich No. and Cr. ICP-AES Set-up and Operation 7. Make fresh weekly. 1. 1. respectively: To a 100-mL volumetric. respectively: To a 100-mL volumetric. Co. Ni. 0. respectively: To a 100-mL volumetric. Cu. Co. 5. add 10 mL of Mixed Standard High B and dilute to volume with Mehlich No. Mn.10 6. add 10 mL of Mixed Standard Medium A and dilute to volume with Mehlich No. 1. weigh enough soil to achieve ≈ 2.1 Weigh 2. Store in polyethylene container. and Zn. 0. 10. Blanks: To a 100-mL volumetric. add 10 mL of Mixed Standard Low A and dilute to volume with Mehlich No. Ba.1. Co. Store in a polyethylene container. Mn. Se. 0. 250.11 6. and Cr. Al.5. 1.05 mg L-1 of Ca. P. 7. 0.01. Co. 0. 0. Fe. add 50 mL of Mixed Standard High A and dilute to volume with Mehlich No. Ni. Mixed Standard Medium B.5 g of <2-mm or fine-grind. and collect extract in receiving cups.0 mL of extracting solution to the tube. Zn. Perform instrument 251 . Cd. 0. and 5 mg L-1 of Ca. Cu. Store in a polyethylene container.01 mg L-1 of P. 20. 1. Mn. Cr.01. Mixed Standard Low A.1. Shake for 5 min at 200 oscillations min-1 at room temperature (20°C± 2°C). Fe. 3 extracting solution. 2. filter. 1.01.5 g of air-dry soil.1. 1.6. As. K. Ba. Cu. 1. Store in polyethylene container.25. Invert to thoroughly mix. Mixed Standard Low B.5 Use the ICP-AES in axial mode to analyze elements. air-dry soil to the nearest mg into a 50-mL centrifuge tube. Invert to thoroughly mix. Make fresh weekly.1. Make fresh weekly. Store in a refrigerator.2. Invert to thoroughly mix. Mg. 5. 50. Cd.3) and dilute to volume with Mehlich No. Ba.4 Remove the sample from the shaker. 2. Co. 7. Mehlich No. 3 extracting solution.5. 1. Se. Cd.01. Co. 10. Analyze samples within 72 h. 3 extracting solution. Cu. Na. Pb.01. Store in polyethylene container. 0. and Zn. 3 (Section 6.01. 10. 7. Mixed Standard Very Low B. 1. Cu. 3 extracting solution.2) extracting solution. respectively: To a 100-mL volumetric. Cd. 3 extracting solution. 0. 0. Store in polyethylene container. Invert to thoroughly mix. 7. 5. 1.

215. 588.608 178. The fraction digested needs to be identified with each sample. 252 .753. 317.558 324.857.221. Calculations The calculation of mg kg-1 of an element in the soil from mg L-1 in solution is as follows: Analyte concentration in soil (mg kg-1) = [A x B x C x R x 1000]/E A = Sample extract reading (mg L-1) B = Extract volume (L) C = Dilution.604.525 455.6 Use the Mehlich No.checks (Hg alignment.69 233.710 205. The instrumental detection limits are calculated by using 3 times the standard deviation of 10 readings of the blank. Rerun all elements and use only the data needed from the diluted analysis. Report Data are reported to the nearest 0.197 7.7 Establish detection limits using the blank standard solution.003.998 196.932 280.1mg kg-1. 231. The selected wavelengths are as follows (reported wavelength listed first and in boldface): Element Al Fe Ca Mg Na K Mn P As Ba Cd Co Cr Cu Ni Pb Se Zn Wavelength ----------. Check instrument alignment and gas pressures to obtain optimum readings with maximum signal to noise ratio. BEC and %RSD of 1 mg L-1 Mn solution) prior to analysis as discussed in operation manual of instrument. 214.271. 327.570 257. 3 extracting solution to dilute those samples with concentrations greater than the high standard.075 589. 279.490 260.887.396 232. 396.nm --------308.153 259. 238.939.026 213.501. if performed R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (3D2) 1000 = Conversion factor to kg-basis E = Sample weight (g) 9.507 226.592. 8. 206.435 228. 220.353.995 766. These values establish the lower detection limits for each element. 216. Analyses are generally performed at two or more wavelengths for each element.614 267. Analyzed values lower than the detection limits are reported as "ND" or non-detected. 214. 7.915 193.204 315.

. Commun. Phosphorus (citrate-soluble. Riley. 1999). Data are reported as mg P2O5 kg-1 soil (4D7a1). Boca Raton. Plant Anal. Page. Miller. 1993. (England and Wales) and is based on the method developed by Dyer (1894).) Methods of soil analysis. 2003.R. Carter (ed. The sample is shaken for 16 h and filtered. <2 mm (4D7a1a-b1) 1. A. Method 960. 1982.E. Soil Sci.. 11. A modified single solution method for the determination of phosphate in natural waters. A 1:10 soil:solution is maintained for all samples.A. and Plant Anal. 1962. FL.. Soil Tests (4D) Citric Acid Soluble (4D7) UV-Visible Spectrophotometer.A. J. FL. 1984. 9. Keeney (eds. WI..D. The AOAC citrate-soluble P method considers the recovery of phosphite source materials as available phosphorus. Sommers. Monogr. Mehlich III-extractable elements. a high citrate level in sample may interfere with the molybdate blue test. even though the Association of American Plant Food Control Officials does not recognize phosphite as a source of available phosphorus. Negative interferences in the P2O5 determination are arsenate. fluoride. Madison. Interferences Unreacted carbonates interfere with the extraction of P2O5. citric acid soluble P2O5 is a criterion for distinguishing between mollic (<250 ppm P2O5) and anthropic epipedons (>250 ppm P2O5) (Soil Survey Staff. Method 963. Part 2.S. Can. In A. M. Chemical and microbiological properties.03) are recognized methods in the Official Methods of Analysis by the Association of Analytical Communities (AOAC) International (AOAC.10. Soil and Plant Analysis Council. Summary of Method A sample is checked for CaCO3 equivalent.R. and D. Chem. Mays. Lewis Publ. 403-430.) Soil sampling and methods of analysis. T. and L. 27:31-36. 253 . Lee.. if the sample is heated. ASA and SSSA. Inc. M. S.L. 1999). 2. Olsen. Positive interferences in the analytical determination of P2O5 are silica and arsenic. In M. Assessment of Mehlich3 and ammonium bicarbonate−DTPA extraction for simultaneous measurement of fifteen elements in soils.R. Soc. Mehlich 3 soil text extractant: A modification of Mehlich 2 extractant. Murphy. Anal. Sufficient citric acid is added to sample to neutralize the CaCO3 plus bring the solution concentration of citric acid to 1%. the method can be modified by evaporating the extract and ashing in a muffle furnace to destroy the citric acid. 1999. Sufficient citric acid is added to sample to neutralize the CaCO3. Acta.H. However. If this occurs. Boca Raton. and C.R.01) and phosphorus (citrate insoluble. and J.S. 34:2817-2838. Precision and Accuracy Precision and accuracy and precision data are available from the SSL upon request. and R. R. Simard. Council on Soil Testing and Plant Analysis. 43-50. Commun. 2000).R. Agron. Ammonium molybdate and stannous chloride are added. The procedure described herein is used by N. CRC Press. Dual-Beam (4D7a) Phosphorus (4D7a1) Air-Dry or Field-Moist. Additional data on anthropic epipedons from several parts of the world may permit improvements in this definition (Soil Survey Staff.W. Mehlich. Absorbance is read using a spectrophotometer at 660 nm.A. Application In soil taxonomy. Soil Sci. 3. Tran. Handbook on reference methods for soil analysis. Soil Sci. 2nd ed. p. 15:1409-1416. References Elrashidi. p.

0.thorium. Dispense concentrated acids and bases in fume hood. ±0. UV-Visible. Daigger Scientific 5. 12 N.3 Citric acid solution. Cary 50 Conc. Store in a refrigerator. MI 5. 4. Whatman 42.0 mL of 10% citric acid solution to 1-L with RODI water 6.2 Mechanical reciprocating shaker. 6. 6.0.5-mL.4 Citric acid solution. Dissolve 1.0.0 g of ammonium molybdate [(NH4)6MO7O24·4H2O] in 300 mL of distilled water.7 Working stannous chloride solution (WSCS). Make fresh weekly. graduated. Use immediately as solution is only stable for ≈ 4 h. 2. Store in brown bottle in the dark in a refrigerator. add 1 ml of 1% citric acid solution.. 6. Varian Australia Pty Ltd. polyethylene 5. long-stem. 150 mm 5.5 Ammonium molybdate solution. 6.10 Spectrophotometer.5%. and gloves) and eye protection (face shields. with gas release caps 5.0. Equipment 5. thiosulfate. 4. dissolve 100 g of anhydrous citric acid (C6H8O7) in RODI water and bring to volume with RODI water. thiocyanate. 60° angle. Eberbach Corp. Invert to mix thoroughly. Use the safety showers and eyewash stations to dilute spilled acids and bases. Add 2 mL of the working 254 . Add 5 ml of 2 N HCl. Varian Australia Pty Ltd.2 Hydrochloric acid (HCl). Dual-View. concentrated. 50-mL.6 Funnel.1 Reverse osmosis deonized (RODI) water 6.11 Computer. Make fresh weekly. Store in polyethylene bottles.3 Centrifuge tubes. 3. 250 mg L-1 P. 200 oscillations min-1. 1 1⁄2 strokes. bismuth. 5. 1.0. Pipet 10. Solution is stable for ≈ 3 months. 1. electronic digital. sulfide. and printer 6.1 Electronic balance. Store in a refrigerator. 1-cm light path. Allow to cool.0 mL of SSPS and dilute to 1-L in a volumetric flask with RODI water. 6.9 Working stock standard P2O5 solution (WSSPS). 4. and dilute to 25-mL with RODI water. Follow standard laboratory procedures. 1000 µL and 10 mL 5.8 Stock standard P2O5 solution (SSPS). Safety Wear protective clothing (coats.10 Standard P2O5 calibration solutions (SPCS). sleeve guards. Pipet 0. Eberbach 6000. Dilute 2 mL of SSCS with 100 mL of RODI water. with tips. and 5. Ann Arbor. Make to 1-L volume with RODI water. Transfer to a 1-L volumetric flask and carefully add 310 mL of concentrated HCl. 30-mL or 10-mL 5.6 Stock stannous chloride solution (SSCS). 6. especially concentrated acids and bases. Dissolve 15. 5. Use sodium bicarbonate and water to neutralize and dilute spilled acids. trace pure grade 6. 1%.099 g of potassium dihydrogen orthophosphate (KH2PO4) that has been dried for 2 h at 110°C with RODI water in 1-L volumetric flask.0 mL of WSSPS into 50-mL tubes. plastic. goggles.5 Filter paper. Varian. 2.9 Cuvettes.10-mg sensitivity 5. 50-mm diameter 5. 1000 µL and 10 mL. Dilute 100. or excess molybdate. Dissolve 10 g of stannous chloride (SnCl2·2H2O) in 100 mL of concentrated HCl. Make to 1-L volume with RODI water. 10%. 4 mL of ammonium molybdate solution. or safety glasses) when preparing reagents.. Invert to mix thoroughly.7 Pipettes. aprons. Reagents 6. Invert to mix thoroughly. In a 1-L volumetric. A concentration of Fe >1000 ppm interferes with P2O5 determination.5 mg L-1 P. with Cary WinUV software.8 Dispenser.4 Bottles. Refer to Snell and Snell (1949) and Metson (1956) for additional information on interferences in the citric acid extraction of P2O5. Make fresh daily.

1 19.1 9. place in a mechanical shaker and shake for 16 h at 200 oscillations min.2 22.8 27.0 8.2 4.0 23.0 18. ____________________________________________________________________________________________________________ %CC1 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 mL CA2 3. and SSL soil standard are routinely included in a batch for quality control. 0.2 ____________________________________________________________________________________________________________ 1 2 %CC = percent calcium carbonate in a sample CA = ml of 10% citric acid needed to be diluted to 30-ml volume with RODI water and added to sample 7.1 24. Collect extract.1 16.5 4.4 3. 7. then store samples at 4° C. Add required volume of 10% citric acid into a graduated cylinder and bring to a volume of 30-mL with RODI water.8 17.7 11.8 22.3 25.1 Weigh 3 g of <2-mm or fine-grind.8 4.5 Remove the sample from shaker and filter. air-dry soil to the nearest mg into a bottle with gas release tops.11 Quality Control Samples: 0.9 10.5 24. Store in a refrigerator.9 % CC 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 mL CA 15. Place the bottle in a mechanical shaker and shake the bottle for 6 h at 200 oscillations min-1 at room temperature (20°C ± 2°C) to dissolve and neutralize the CaCO3. blanks.5 19.3 10.6 18.8 12.50 mg L-1. Final concentrations are 0.4 11.2 17.4 16.9 5. proceed to step 7. Analyze samples within 72 h. Add this solution to the soil.7 21.1 14.0 26.1 11. Allow to equilibrate to room temperature before use.4 Cap the bottles.6 26.3 15.3. If the soil does not contain free carbonates.3 23. weigh enough soil to achieve ≈ 3 g of air-dry soil. 7. Procedure 7.4.20.4 8.0 13. 6.at room temperature (20°C ± 2°C).7 14. 0.stannous chloride solution (WSCS).6 8.4 21. Invert to mix thoroughly.2 7. 7.1 mg P L -1 solution from SSPS.9 25. Table 1. 0.7 19.0 %CC 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 mL CA 21.40. Volume of 10% citric acid (mL) required to decompose CaCO3 (%) and to bring to solution concentration to 1% in a final volume of 30 mL for 3-g sample.9 20.0.2 If the soil contains free CaCO3.0 3.6 23. 255 . Proceed to step 7.3 20.3 If the soil contains no free CaCO3. If sample is moist.6 13.4 26.4 18.8 7. add 30 mL of 1% citric acid solution to the sample.30.7 16. Prepare fresh weekly.7 6.2 12.7 24. 7.4 13.3 5. 0.5 6. refer to Table 1 to determine the amount of 10% citric acid solution required to neutralize the CaCO3. If extracts are not to be determined immediately after collection.5 14.10. and 0. selected SPCS.5 9.8 % CC 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 mL CA 9. respectively.1 6.

Phosphorus.7 Transfer sample extract and SPCS to cuvettes. Methods of chemical analysis for soil survey samples. Inc. Methods 960.T. 2000. 1949.01 and 963. 3rd ed. Snell. Phosphorus (Citrate-Soluble) in Fertilizers and Phosphorus (Citrate-Insoluble) in Fertilizers.. Calculations Convert the extract P2O5 (mg L-1) to soil P2O5 (mg kg-1) as follows: Soil P2O5 (mg kg-1) = [A x B x C1 x C2 x R x 1000 x 2. Chem. Samples are treated the same as SPCS (Section 6.01.01 unit for the sample extract and each SPCS.630-681. N. 7.9 Calibrate the instrument by using the SPCS. Van Nostrand Co. Rejection criteria for SPCS. D. Record results to the nearest 0. No.99. 11. The data system will then associate the concentrations with the instrument responses for each SPCS.7. Bull. Report Report the 1% citrate acid extractable P2O5 in mg kg-1 to nearest whole number. Soc. if R2 <0.10 Run samples using calibration curve.D. 1956. Trans.6 Pipet 1 mL of sample extract into a plastic cup. A. Run samples using calibration curve.11 If samples are outside calibration range.03) C1 = Automatic dilution (1:25) C2 = Dilution. and diluted to 25-mL with RODI water. 1894. if SPCS as samples > ± 20%. dilute sample extracts with extracting solution and re-analyze. Metson. 7. F.29 = Conversion factor P to P2O5 E = Sample weight (g) 9. Official Methods of Analysis. Rejection criteria for batch. Add 2 mL working stannous chloride solution (WSCS). Sample concentration is calculated from the regression equation. 7. International. Dept.03. 65:115-167.29]/E where: A = P2O5 in sample extract (mg L-1) B = Extract volume (L) (0. if necessary R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = Conversion factor to kg-basis 2. Autozero with calibration blank. Dyer. Add 4 mL of ammonium molybdate solution to all samples and SPCS. Swirl to mix and allow to stand 20 min for color development. if blanks as samples > 0. Sci. 7. Snell. and if SSL standard > ± 20% mean. p. References American Association of Analytical Communities (AOAC). A blank has all reagents contained in the sample extract except the soil. 256 . 8. 7. respectively.. and C. and Industrial Res. 12.8 Set the spectrophotometer to read at 660 nm. 10. Colorimetric methods of analysis.Z. Vol 2.J. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.10). Soil Bur.

. NV 5. The New Zealand P retention (Blakemore et al. <2 mm (4D8a1a-b1) 1. 2. ±1. goggles. Equipment 5. 30 mL or 10 mL 5. 150 mm 5. Use safety showers and eyewash stations to dilute spilled acids and bases. plastic 5. sleeve guards. MI 5. Safety Wear protective clothing (coats.8 Dispenser.5 Centrifuge tubes. Govt. 4. Soil Tests (4D) New Zealand P Retention (4D8) UV-Visible Spectrophotometer. Soil taxonomy. Restrict the use of concentrated HNO3 to a fume hood. Varian.9 Filter paper. 1987) is the initial P concentration minus the P remaining in the sample solution and is reported as percent P retained (4D8a1). The factors that affect soil P retention are not well understood.11 Cuvettes. Office. 1985).0-mg sensitivity 5. Reno. with printer 257 . 3. Interferences No significant problems are known to affect the P retention measurement.. 1999). 1984). An aliquot of the supernatant is transferred to a colorimetric tube to which nitric vanadomolybdate acid reagent (NVAR) is added. Summary of Method A 5-g soil sample is shaken in a 25-mL aliquot of a 1000 mg L-1 P solution for 24 h. aprons.2 Mechanical reciprocating shaker. 1-cm path.4 Centrifuge. 100 oscillations min-1.12 Spectrophotometer. 1 1⁄2 in strokes.7 Pipettes.1 Electronic balance. Use sodium bicarbonate and water to neutralize and dilute spilled acids. Ann Arbor. The mixture is centrifuged at 2000 rpm for 15 min. or safety glasses). Phosphate retention is also called P adsorption. allophane and imogolite have been considered as major materials that contribute to P retention in Andisols (Wada. Andisols and other soils that contain large amounts of allophane and other amorphous minerals have capacities for binding P (Gebhardt and Coleman. 5. However. USDA-NRCS. Print. When preparing reagents. A basic system of soil classification for making and interpreting soil surveys. Application In soil taxonomy. sorption.13 Computer. Eberbach Corp. Daigger Scientific 5.5-mL. UV-Visible. electronic digital. Many metal salts are extremely toxic and may be fatal if ingested. 5. 1000 µL and 10 mL. with tips. Cary 50 Conc. 4. 50 mL. Absorbance of the solution is read using a spectrophotometer at 466 nm. Varian Australia Pty Ltd. or fixation.Soil Survey Staff.3 Digital diluter/dispenser with syringes.. with Cary WinUV software. exercise special care. This absorbance correlates to the concentration of the non–adsorbed P that remains in the sample solution. gas tight. 10000 and 1000 µL. 1000 µL and 10 mL 5. plastic. Whatman 42. Centra GP-8 5. 1999. Thoroughly wash hands after handling these metal salts. Microlab 500. Washington DC.6 Cups. 2nd ed. and gloves) and eye protection (face shields. polyethylene 5. Dual-Beam (4D8a) Phosphorus (4D8a1) Air-Dry or Field-Moist. Varian Australia Pty Ltd. the P retention of soil material is a criterion for andic soil properties (Soil Survey Staff. Eberbach 6000.

8 Diluent for Standard P calibration solutions (DSPCS). Mix the nitric acid solution with the vanadate solution and then add the molybdate solution. No fine-grind material is used for this procedure.10 Quality Control: SSL soil standard is routinely included in every batch of 24 samples for quality control.9.6 g of NH4VO3 in 500 mL of boiling RODI water.55 and 4. Carefully and slowly dilute 200 mL of concentrated HNO3 to 2 L of RODI water. Dilute to 2 L with RODI water.7 Nitric vanadomolybdate acid reagent (NVAR). Make fresh weekly. 6. 60. Reagents 6. To six 100-mL volumetric flasks add the appropriate amount of PRS (1000 mg L-1) and bring to volume with DSPCS solution as follows: 6. 20. 7. 2 g L-1 RODI water 6.1 Reverse osmosis deionized (RODI) water.9.9 Standard P calibration solutions (SPCS). and 0% P retained. Dissolve 35. Add 54. Mix well. air-dry soil to the nearest mg into a 50-mL centrifuge tube. Allow the solution to cool to room temperature and dilute to 2 L with RODI water. ASTM Type I grade of reagent water 6.0 mL of P-retention solution to centrifuge tube.65. Add the acid to the water. weigh enough soil to achieve ≈ 5 g of air-dry soil. 258 . 100. vanadate solution.9.9.2 Use the dispenser to add 25.2 80% SPCS = 1: 20 (200 mg L-1) = Add 20 mL PRS and bring to 100-mL volume with DSPCS solution. 6. concentrated. Procedure 7.6 Molybdate solution.5 20% SPCS = 1:5 (800 mg L-1) = Add 80 mL PRS and bring to 100-mL volume with DSPCS solution. 1000 mg L-1 P.1 Weigh 5g of <2-mm or fine-grind. Dissolve 32 g of ammonium molybdate [(NH4)6Mo7O24·4H2O] in 50°C RODI water.9. Allow to equilibrate to room temperature before use. 6. Store in a refrigerator.2 g of KH2PO4 that has been dried for 2 h at 110°C and 217.4 P retention solution (PRS).3 Nitric acid (HNO3). 6.6 g of sodium acetate trihydrate (CH3COONa·3H2O) in RODI water. 16 N 6. 6.5 Nitric acid solution. Dissolve 1.4 40% SPCS = 3:20 (600 mg L-1) = Add 60 mL PRS and bring to 100-mL volume with DSPCS solution.6. 80. Dilute to 8 L with RODI water.9. 0. 6. 6.6 0% SPCS = 1:4 (1000 mg L-1) = Add 100 mL PRS to a 100-mL volumetric. Carefully and slowly add 12 mL of concentrated HNO3. 40. Allow the solution to cool to room temperature. Add 92 mL of glacial acetic acid. The solution pH should range between 4. 6. If sample is moist.4 g of sodium acetate trihydrate (CH3COONa·3H2O) and 23 mL of glacial acetic acid and dilute to 2 L with RODI water.2%.3 60% SPCS = 1:10 (400 mg L-1) = Add 40 mL PRS and bring to 100-mL volume with DSPCS solution. 6. 6. Note: This solution needs to be made in this order.2 Superfloc 16. 7. 6.1 100% SPCS = (0 mg L-1) = Bring to 100-mL volume with DSPCS solution.

. Analyze samples within 72 h.. Phosphate adsorption. K. Govt.for this proce 9. Washington DC. A basic system of soil classification for making and interpreting soil surveys. The data system will then associate the % P retained with the instrument responses.K. 43 p. 7.6 The color reaction requires a minimum of 30 min before the analyst records readings. Auto zero with the calibration blank. if SPCS as samples > ± 20%. NZ Bureau Scientific Report 80.H.) Anodosols. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. dilute sample extracts with extracting solution and re-analyze. Shake for 24 h at 100 oscillations min-1 at room temperature (20°C± 2°C). and N.5-mL cuvette.A. NZ Soil Bur. 11.. decant. 0. filter. 8. i. Tan (ed. Print. 1999. Lower Hutt. New York. If extracts are not to be determined immediately after collection. Stewart (ed. if blanks as samples > 0. and B.) Advances in Soil Science. Add 2 to 3 drops of Superfloc. the absorbance is equated to the SPCS. Gebhardt..02% w/v to each tube. 2nd ed.C. 1985. 173-229. Benchmark papers in soil science series. Soil taxonomy. L. Springer-Verlag. 7. then store samples at 4°C. Sample P retention is calculated from the regression equation. Coleman. 7. Australia. USDA-NRCS. and if SSL standard > ± 20% mean. References Blakemore. NY. NZ.01.01 unit for the sample extract and each SPCS. and collect extract in receiving cup. Soil Survey Staff. Calculations None. Report Report the percent New Zealand P retention to the nearest whole number. Searle. The distinctive properties of Andosols. H. In K. Record results to the nearest 0. Centrifuge at 2000 rpm for 15 min.5 Use the digital diluter to add the nitric vanadomolybdate acid reagent (NVAR) to each sample supernatant and to each SPCS. Office.4 Remove sample from the shaker.e. Daly. if R2 <0. Methods for chemical analysis of soils.3 Transfer the sample to the shaker. 237-248. use a dilution of 1:20 sample dilution. p.7 Set the spectrophotometer to read at 466 nm. Rejection criteria for batch. Van Nostrand Reinhold. 7. 1987. 7. Rejection criteria for SPCS. Wada. To fill a 4.99. 1984. 259 .10 If samples are outside calibration range. Anion adsorption of allophanic tropical soils: III.8 Calibrate the instrument using the SPCS.T. 7. P.L. 7.7. Co. 10. Melbourne. p.9 Run samples using calibration curve. In B.

or safety glasses).(4D9a1a1-2.4 Centrifuge.0-mg sensitivity 5.1 Electronic balance. goggles. The nitrate is quantitatively reduced to nitrite by passage of the sample through a copperized cadmium column. 1 1⁄2 in strokes. 50-mm diameter 260 . Application The inorganic combined N in soils is predominantly NH4+ and NO3.and/or NO2. MI 5. Cadmium is toxic and carcinogenic. 2500 µL and 10 mL.5-g soil sample is mechanically shaken for 30 min in 25 mL of 1 M KCl solution. The nitrite (reduced nitrate plus original nitrite) is then determined by diazotizing with sulfanilamide followed by coupling with N-1-naphthylethylenediamine dihydrochloride. In this method. Equipment 5. Automated Ion Analyzer (4D9a1a) Nitrate-Nitrite (4D9a1a1-2) Air-Dry or Field-Moist. do all transfers over a special tray or beaker dedicated to this purpose. 2. send the cadmium-copper column to LACHAT for repacking. The resulting water soluble dye has a magenta color which is read at 520 nm. with tips. Safety Wear protective clothing (coats.5 Pipettes. 1982). electronic digital.(Keeney and Nelson. Whatman No. Thoroughly wash hands after handling these metal salts. 5. sleeve guards. All forms of nitrogen. Restrict the use of NH4OH and concentrated HCl to a fume hood.2 Centrifuge tubes. Use safety showers and eyewash stations to dilute spilled acids and bases. polyethylene.Soil Tests (4D) 1 M KCl Extraction (4D9) Cadmium-Copper Reduction (4D9a) Sulfanilamide N-1-Naphthylethylenediamine Dihydrochloride (4D9a1) Flow-Injection. 1993). 25 mL. 3. and gloves) and eye protection (face shields. EDTA is added to the buffer to reduce this interference (LACHAT. 42 filter paper. 4. Nitrogen in the form of ammonium ions and nitrate are of particular concern because they are very mobile forms of nitrogen and are most likely to be lost to the environment (National Research Council.7 Funnel. If repacking the cadmium-copper reduction column. 42. 50-mL. Use sodium bicarbonate and water to neutralize and dilute spilled acids. Wear gloves and follow the precautions described on the Material Safety Data Sheet. 60° angle.in the sample. Eberbach Corp. Ann Arbor.. ±1. exercise special care.6 Filter paper. long stem. Interferences Low results can be obtained for samples that contain high concentration of Fe. 2500 µL and 10 mL 5. Oak Ridge 5. <2 mm (4D9a1a1-2a-b1) 1. 200 oscillations min-1. Summary of Method A 2. A flow injection automated ion analyzer is used to measure the soluble inorganic nitrate (NO3-). 1993). Preferably. Data are reported as mg N kg-1 soil as NO3. polyethylene 5. respectively).3 Mechanical reciprocating shaker. 1993). 150 mm 5. however. Many metal salts are extremely toxic and may be fatal if ingested. aprons. or other metals. Absorbance is proportional to the concentration of NO3. The sample is then filtered through Whatman No. Cu. When preparing reagents. are subject to transformation to ammonium ions and nitrate as part of the nitrogen cycle in agroecosystems and all can contribute to residual nitrogen and nitrogen losses to the environment (National Research Council. Eberbach 6000.

1 Stock standard nitrate solution (SSNO3S). LACHAT Instruments.7.7. glass. LACHAT Instruments.0 mg N L-1 as NO3.18 5.7.13 5.2 Working stock standard nitrate solution (WSSNO3S). Milwaukee. It is recommended that when running a 1 channel method for NO2. 1-L and 250-mL Bottles.5. add 500 mL RODI to a 1-L volumetric flask.0 g sulfanilamide.+ NO3or NO2. Slowly add 300 g NaOH. 6.0 mg N L-1 as NO3. LACHAT Instruments. 6.5 g potassium chloride (KCl) in 800 mL RODI water. Milwaukee.7 The following are standards preparation for a 1 channel system determining NO2. 6.and a 2 channel system where one channel is used for NO2. Make fresh daily. Milwaukee.and the other channel is used for determining NO2-. To five 250-mL volumetric flasks add as follows: 6.00 mg N L-1 as NO3. Used to adjust ammonium chloride buffer to pH 8.9 5.14 5. plastic. 2. WI Sample Processing Module (SPM) or channel. 10-mL (samples) 6.standards are used. LACHAT Instruments.00.0 mg N L-1). Add 105 mL concentrated HCl.15 5. ASTM Type I grade of reagent water 6.0 g N-1naphthylethylenediamine dihydrochloride (NED). Make fresh weekly. 6. and printer Vials.4).0 g disodium EDTA. In a hood. 6. WI Computer. Store in dark bottle and discard when pink. Store in a refrigerator. 0.6 1 M KCl extracting solution.7. Dilute to mark and invert to thoroughly mix. and 0.00. dark. add 250 ml RODI water.in 1 M KCl.02 to 20.+ NO3.2 Helium. 6. Dilute to mark.7. 40. either NO2. 95 mL ammonium hydroxide (NH4OH) and 1.00 mg N L-1 = 25. To a 1-L volumetric flask. QuikChem AE.3 15 M NaOH. QuikChem Method (12-107-04-1-B.+ NO3. compressed gas 6.8 5. Dilute to mark with RODI water and invert to thoroughly mix.0 mL WSSNO3S 261 . and 1.in 1 M KCl. WI Reagent Pump. WI.or NO3standards may be used. Degas with helium ≈ 5 min.standard sets are recommended. Make fresh daily.00 mg N L-1 = 125. Degas with helium ≈ 5 min.5 (reagent 6. 0.17 5. Store in polyethylene containers.in 1 M KCl. 1-L Cups. nitrate/nitrite in 1 M KCl 0.19 Volumetric flasks. WI Automated Dilution Station. The extracting solution is used also as the carrier and a component of the N standards. Milwaukee.11 5. add 100 ml SSNO3S.80.16 5.3. 30 mL or 10 mL Flow Injection Automated Ion Analyzer. pH 8.08. For the 2 channel system. plastic.12 5.3 Standard nitrate calibration standards (SNO3CS) or working standards. invert to thoroughly mix. Dissolve 74. plastic Dispenser.1 10. Invert to mix. 25-mL (standards) Culture tubes. To a 1-L volumetric flask. with computer and printer XYZ Sampler. LACHAT Instruments.4 Ammonium chloride buffer. For the 1 channel system. Dilute to mark with 1 M KCl and invert to thoroughly mix. WI.5.5 g KCl in 600 mL RODI water.2 2.10 5. LACHAT Instruments. Reagents 6. 6. add 600 mL RODI H2O followed by 100 mL 85 percent phosphoric acid (H3PO4). Milwaukee.1 Reverse osmosis deionized (RODI) water.444 g potassium nitrate (KNO3) dried in an oven for 2 h at 110° C and 74. 200.that NO3. Dissolve and dilute to mark. Degas with helium ≈ 5 min. (CAUTION: The solution will get very hot!) Swirl until dissolved. Shake to wet and stir to dissolve 20 min. Cool and store in a plastic bottle. with QuikChem software. 10. dissolve 1.3. In a 500-mL container. the use of both NO2+ NO3. Milwaukee.0 mL WSSNO3S 6.5 Sulfanilamide color reagent. carrier and standards diluent. In a 1-L volumetric flask. 20.

5 Transfer WNCS standards into plastic vials and place in descending order in XYZ sample trays marked "Standards".08. Store in polyethylene containers.00 mg N L-1 = 25.00 mg N L-1 = 125. Make fresh daily. 7.4 0.7. pump all reagents into manifold. Turn pump off.7.7.08 mg N L-1 = 1.6.0 mL WSSNO2S 6. Dilute to mark with RODI water and invert to thoroughly mix. Make fresh weekly. In a 1-L volumetric flask.3. 0. and 0.2 2. filter.7.0 mL WSSNO3S 6. Procedure Extraction 7. 7. 2. Do not degas. 7.0 mL WSSNO3S (blank) Dilute each SNO3CS to the mark with 1 M KCl and invert to thoroughly mix.00 mg N L-1 = 0. add 100 ml SSNO2S. Store in a refrigerator.4 Transfer sample extracts into culture tubes and place in XYZ sample trays marked "Samples". and 74.6. then store samples at 4°C.5 Working stock standard nitrite solution (WSSNO2S). On the column. 10. Connect the open tubing on 262 . If sample is moist. Transfer the sample to a shaker. If extracts are not to be determined immediately after collection.214 g potassium nitrite (KNO2). To five 250-mL volumetric flasks add as follows: 6.2 Add ≈ 25 mL of 1 M KCl to sample.3.3 0.1 10.7 Turn main power switch "ON". 6.6.in 1 M KCl.7.0 mL WSSNO2S 6.0 mL WSSNO2S 6. 6.3.6 Refer to the operating and software reference manuals for LACHAT for set-up and operation.6 Standard nitrite calibration standards (SNO2CS) or working standards. To a 1-L volumetric flask. 6. 20. 200. 7.0 mg N L-1 as NO2. and collect extract in receiving cups.6. disconnect the center tubing from one of the union connectors and immediately connect to the outlet tubing of the buffer mixing coil.8 Before inserting cadmium-copper reduction column.7. Analyze samples within 24 h.986 g sodium nitrite (NaNO2) or 1.5 g KCl in 800 mL RODI water. 7.5 0.00.0 mg N L-1 as NO2. Shake for 30 min at 200 oscillations min-1 at room temperature (20°C ± 2°C).00 mL WSSNO2S 6. Decant.80 mg N L-1 = 10. Do not degas.4 0.6.1 Weigh 2.7. 7.00 mL WSSNO3S 6.00.80 mg N L-1 = 10.00 mg N L-1 as NO3.08 mg N L-1 = 1.0 mL WSSNO2S (blank) Dilute each SNO2CS to the mark with 1 M KCl and invert to thoroughly mix.7. Flow Injection Set-up and Operation 7.00 mg N L-1 = 0.in 1 M KCl.4 Stock standard nitrite solution (SSNO2S).80.3 0.6. Make fresh daily.7.in 1 M KCl. 0.7. dissolve 0.7. 7. weigh enough soil to achieve ≈ 2. air-dry soil to the nearest mg and place into a 50-mL centrifuge tube. Dilute to mark with 1 M KCl and invert to thoroughly mix.5 g of air-dry soil.3 Remove the sample from the shaker.5 0.5 g of <2-mm or fine-grind.

80. LACHAT Instruments.11 Method parameters specific to 1 M KCl N are defined within the "Method Definition" menu.C (10. 0. In addition.5 are sections of peak from start of peak to end of peak. If air is introduced accidentally. System unit receives the downloaded method and initializes it.nitrite) are as follows: 7. 263 .12. The normal strategy requires a minimum correlation coefficient of 0. A calibration passes only when both criteria are met. Average life of column is approximately 600 samples. 1983. calibration strategies are based on the full chord. 7. turn the pump on maximum.5. and maximum elapse time between check standards is 2 h. and then "Edit" to create new sample tray followed by "Submit" to run new sample tray. On computer main menu.4 Check standard is 10.0 to 0. scan across correlation coefficients for all chords 1 .12. and 0. The most peak area is supposed to be in chords 2 4 with the most signal-to-noise ratio in chords 1 and 5. select "Methods" and then "Analysis Select and Download". Scatter is indicative of air bubbles and irregular reagent flow. nitrate-nitrite in 2 M (1 M) KCl soil extracts (U.99.13. connect the column into the manifold. with a data format of ####. Also observe for any back-pressure in manifold tubing. 7.3 The protocol (replications) for the calibration standards is as follows: AA BB CCC DDD EE. Strategies are user designated. 1993).00 mg N L-1). Continue this step and observe baseline. To see if peaks are being timed correctly. Do not let air enter the column.E are normal.00. 7. data rounded to 3 places. 7.12. The data system is calibrated with the injection of SNO3CS and/or SNO2CS. U.8 mg N L-1) and C .1 There are 5 calibration standards (10. Department of Interior. and tap column.. The data system then associates the concentrations with the instrument response for each SNO3CS and/or SNO2CS. "Tray Definition and Submit".13 Method parameters in relation to timing are as follows: 7. 0. Chord 0 is full chord.E (0.5 Calibration strategy for segments A .C and C .12 Some of the method parameters as they relate to calibration standards (nitrate .8 to 0.1 Cycle period: 40 s 7.2 The segments/boundaries for the calibration standards are A . 7. 7. 7.e. 7.12. Return the pump to normal speed. A good baseline needs to be smooth and at zero absorbance. Maximum number of consecutive trays between check standard is one. select 1 M KCl N method. continue to pump reagents into manifold. On method list. working up the column until all air is removed.9 On computer main menu. select "Samples".0 mg N L-1).2 Inject to start of peak period: 27 s. 2. 7.the column to the tee fitting where the color reagent is added.12. Some of these parameters have been modified from the QuikChem Method 12-107-041-B. Both segments require a maximum standard deviation in slope of 50%.6 The instrument is calibrated with the injection of SNO3CS and/or SNO2CS. maximum number of consecutive samples between check standard is 60.12.0 mg N L-1.S. Environmental Protection Agency.S.10 Upon connection of cadmium column and downloading of 1 M KCl Method.00. 1993.13. 7.08. the column needs to be replaced. Upon degradation. Geological Survey. i. and chord 1 .###.

15 Refer to the "Method Definition" for 1 M KCl nitrate for other method parameters not discussed here. Nitrogen . 10.50 abs 7. Chemical and microbiological properties.16 Run samples using calibration curve. place the transmission lines into RODI water and pump for approximately 20 min and proceed with the normal "Shut-down" procedure. References Keeney. Upon completion of analysis.17 If samples are outside calibration range. Some fittings may need to be soaked overnight or placed in a sonic bath for 10 to 15 min to remove any KCl accumulations.7.13. Miller. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.00 abs 7.19 The accumulation of 1 M KCl in the manifold tubing and the fittings may cause clogs over time. the valves and fittings need to be washed with RODI water. 643-698. WI. Sample concentration is calculated from the regression equations.and/or NO2-.H.14 Method parameters in relation to data presentation are as follows: 7.3 Inject to end of peak period: 63 s 7.4 Automatic timing.) Methods of soil analysis. 7.1mg N kg-1 soil as NO3. Nelson. Report results to the nearest 0.14. Calculations Convert extract N (mg L-1) to soil N (mg kg-1) as follows: Soil N = [ (A x B x C x R x 1000)/E] where: A = Sample extract reading (mg N L-1) B = Extract volume (L) C = Dilution. dilute samples with extracting solution and reanalyze. ASA and SSSA.R. 8. 2nd ed.2 Bottom Scale Response: 0.13. 11. R. if performed R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = Conversion factor to kg-basis E = Sample weight (g) 9.R.. Monogr. 7. no manual timing.W. 7.18 Upon completion of run. 7. and D. Keeney (eds. 264 . 9. Part 2. where standard assumptions are in effect. In A. D. Madison. Agron.L.01 unit for the sample extract and each SPCS.inorganic forms. and D. p.14. Report Report data to the nearest 0. 1982.1 Top Scale Response: 0. Page. 7.

1983. Book 5. Absorbance of the solution is read at 660 nm. LACHAT Instruments. 1992). Data are reported as mg N kg-1 soil as NH3 by procedure 4D10a1a1. and gloves) and eye protection (face shields. 1993. Press. This method involves estimation of the ammonium produced by a 1-week period of incubation of soil at 40°C (Keeney and Bremner. 5. 3. stoppered. <2 mm (4D10a1a1a-b1) 1. EDTA is added to eliminate this problem (Keeney and Nelson. Washington. The method described herein for estimating mineralizable N is one of anaerobic incubation and is suitable for routine analysis of soils. 0. Geological Survey. aprons.S.S. Method 353. especially concentrated acids and bases. ±1. Safety Wear protective clothing (coats.S. 1992.1 Electronic balance. and incubated at 40°C for 1 week. 1983. An agenda for agriculture. Environmental Protection Agency. U. 1993. Interferences The temperature and incubation period must remain constant for all samples.2 Test tubes.02 to 20. Soil Tests (4D) Aerobic Incubation (4D10) 2 M KCl Extraction (4D10a) Ammonia –Salicylate (4D10a1) Flow Injection. Equipment 5. goggles.2. Use sodium bicarbonate and water to neutralize and dilute spilled acids.0 mg N L-1. nitrate in 2 M (1 M) KCl soil extracts. Committee on long-range soil and water conservation.LACHAT Instruments. Method I2601-78. 4. The test can be performed on field-moist or air-dry soil samples. 6645 West Mill Rd. 1966) under anaerobic conditions to provide an index of N availability. Natl. Method Summary An aliquot of air-dry homogenized soil is placed in a test tube with water. 16-mm x 150-mm 5.0-mg sensitivity 5. U. Soil and water quality. Thoroughly wash hands after handling reagents. WI. Dispense concentrated acids and bases in a fume hood. or safety glasses) when preparing reagents. A flow injection automated ion analyzer is used to measure the ammonium produced in the soil after incubation. Automated Ion Analyzer (4D10a1a) N as NH3 (Mineralizable N) (4D10a1a1) Air-Dry or Field-Moist. Methods for chemical analysis of water and wastes. Application The most satisfactory methods currently available for obtaining an index for the availability of soil N are those involving the estimation of the N formed when soil is incubated under conditions which promote mineralization of organic N by soil microorganisms (Environmental Protection Agency. Acad. 2..3 PVC stoppers 265 . Soil extracts can contain sufficient concentrations of calcium and magnesium to cause precipitation during analysis. Use the safety showers and eyewash stations to dilute spilled acids and bases. The contents are rinsed with 2 M KCl. DC. Department of Interior. EPA-600/4-79-020. QuikChem method 12-107-04-1-B. Revised March. Milwaukee. sleeve guards. Methods for determination of inorganic substances in water and fluvial sediments. Chapter Al. National Research Council. 1982). U.

WI 5. Milwaukee.2 8.9 Standard N calibration solutions (SNCS) or working standards. Mix thoroughly. In a 500-mL volumetric. 0.00 mg P L-1 = 5.10 mg P L-1 = 0.00. 50-mL.00 mg P L-1 = 50.2 Helium.15 Culture tubes. Whatman No. Chicago.00 mg N L-1. 0. 6. Make fresh daily. Dissolve 150 g KCl in RODI water and dilute to 1-L volume.0 ml SSNS 6. Invert to mix thoroughly.25 mL SSNS 6. plastic. glass.3 Potassium chloride (KCl). Do not degas with helium.9. and printer 5. Milwaukee. 6.0 g sodium phosphate dibasic heptahydrate (Na2HPO4·7H20) in 900 mL RODI water.9. LACHAT Instruments.50 mg P L-1 = 1. 20. Dilute to 1-L and invert to mix thoroughly.. Store in dark bottle in a refrigerator. QuikChem Method (12-107-06-2-A.0 mL SSNS 6. Degas with helium. 6.9. Dissolve 66 g EDTA in 900 mL RODI water.5 5. WI 5. 6.4 EDTA (ethylene tetraacetic acid disodium salt dihydrate). Quality Lab Inc.12 Sample Processing Module (SPM) or channel.00 mg P L-1= 0. 8. Invert to mix thoroughly. Dissolve 150 g sodium salicylate [salicylic acid sodium salt (C6H4(OH)(COO)Na)]. To six 250-mL volumetric flasks add as follows: 6.8 Stock standard N solution (SSNS).0 g sodium nitroprusside [sodium nitroferricyanide dihydrate (Na2Fe(CN)5NO·2H2O)] in 800 mL RODI water.4 5.10. Degas with helium. IL Centrifuge. 6.7 5.9 XYZ Sampler. 6.0 g NaOH and 50. WI. 25-mL (standards) 5.0 mg P L-1).0 mL SSNS 6. Dissolve 28. ASTM Type I grade of reagent water 6.5. 60° angle. QuikChem AE. Dilute to volume with RODI water and invert to thoroughly mix.9. In a 1-L volumetric flask.14 Vials.9. Milwaukee.00 mg P L-1 = 20.00. dissolve 150 g potassium chloride (KCl) and 0. LACHAT Instruments. 0. Milwaukee. LACHAT Instruments. WI 5.10 Reagent Pump. ammonia (salicylate) in 2 M KCl soil extracts. 266 . 150 mm Funnel.6 Salicylate-Nitroprusside Color Reagent. 2 M.5 NaOH.3 2. 0. Milwaukee.05 to 10.3819 g of ammonium chloride (NH4Cl) that has dried for 2 h at 110°C in about 800 mL RODI water.25 mL SSNS 6.1 20. LACHAT Instruments. compressed gas 6. Degas with helium. WI 5. 100. Milwaukee. carrier and standards diluent.5 0. dilute 250 mL of 5.11 Automated Dilution Station. LACHAT Instruments. 10-mL (samples) 6. Model 10-140. and 1.25% sodium hypochlorite (NaOCl) to mark with RODI water. long stem.1 Reverse osmosis deionized (RODI) water.6 0. Store in polyethylene containers.0 mL SSNS (blank) Dilute to mark with 2 M KCl.4 0.9.7 Hypochlorite Reagent.6 5. Degas with helium.0. with QuikChem software. Degas with helium. 2. buffer.8 Incubator. Dilute to 1L and invert to mix thoroughly. 42.50. polyethylene Filter paper. LACHAT Instruments. WI 5.0 mg N L-1. Make fresh weekly. 50-mm diameter Flow Injection Automated Ion Analyzer.13 Computer. Dilute to 1-L and invert to mix thoroughly. 6% solution. Reagents 6. Store in a refrigerator.

set speed to 35. Also observe for any backpressure in manifold tubing.25 g. "Tray Definition and Submit". Scatter is indicative of air bubbles and irregular reagent flow.4.6 Transfer WNCS standards into plastic vials and place in descending order in XYZ sample trays marked "Standards". Some of these parameters have been modified from the QuikChem Method 12-107-062-A. If extracts are not to be determined immediately after collection. 7. Flow Injection Set-up and Operation 7.9 On reagent pump. Complete the transfer by rinsing the tube with 3 times with 4 ml of 2 M KCl.25 g. Environmental Protection Agency.7) into appropriate chambers of the manifold. 7. even though contained in polyethylene bottles.8 Turn main power switch "ON" and allow 15 min for heater module to warm up to 60°C.5 ±1 mL of RODI water. weigh enough soil to achieve ≈ 5 or 1. select "Samples". then store samples at 4°C.5. A good baseline needs to be smooth and at zero absorbance. select "Methods" and then "Analysis Select and Download". weigh 1. 7. 7. System unit receives the downloaded method and initializes it. respectively. Ammonia is volatile and will leave the sample slowly.11 Pump reagents (6. Refer to the manufacturer's instructions for set-up and operation of the incubator. Analyze samples within 24 h. 6. 7. If sample is moist.1 Weigh 5 g of <2 mm. LACHAT Instruments.7. 7. air-dry soil to the nearest mg into a 16-mm x 150-mm test tube.12 On computer main menu.3 At the end of 7 days.7 Refer to the operating and software reference manuals for LACHAT for set-up and operation. Modifications are primarily related to the criteria and strategies for calibration standards and to injection timing. of air-dry soil. and then "Edit" to create new sample tray followed by "Submit" to run new sample tray.5 Transfer sample extracts into culture tubes and place in XYZ sample trays marked “Samples”. 7.2 Add 12. shake. Procedure Anaerobic Incubation of Soil Sample 7.10 On computer main menu. and place in a 40°C constant-temperature incubator for 7 days.S. 7.6.13 Method parameters specific to mineralizable N are defined within the "Method Definition" menu. using a total of 12.14 Some of the method parameters as they relate to calibration standards are as follows: 267 . Filter contents into a centrifuge tube. 7.5 ±1 mL of the KCl. remove the tube and shake for 15 s. 2001). 7. select Mineralizable N Method. On method list. If soil is fine-grind. ammonia (salicylate) in 2 M KCl soil extracts (U. 7. 6. 1979. Do not add ethanol to overcome any wetting difficulties as ethanol may act as an interference with microbial activity. Stopper the tube. 6.4 Transfer the contents of the test tube to another test tube. 7. Continue this step and observe baseline.

5.00 abs 7.3 Inject to end of peak period: 46 s 7. In addition. 7.50 abs 7.00 mg P L-1). Chord 0 is full chord.00 mg P L-1) with a data format of ####. To see if peaks are being timed correctly.00.15 Method parameters in relation to timing are as follows: 7.14. Strategies are user designated. Maximum number of consecutive trays between check standard is one. and maximum elapse time between check standards is 2 h.14.5 are sections of peak from start of peak to end of peak. scan across correlation coefficients for all chords 1 .0 to 2.01 unit for the sample extract and each SNCS.1 Cycle period: 40 s 7.5.7. The normal strategy requires a minimum correlation coefficient of 0.4 The check standard is 20 mg P L-1.15. 7.F (2. i.15.15. data rounded to 3 places.1 Top Scale Response: 0. where standard assumptions are in effect. 7. 7.14. The data system the associates the concentrations with the instrument response for each SNCS.5 Calibration strategy for segments A – C and C .00. 7.1.14.16.3 The protocol (replications) for the calibration standards is as follows: AA BB CC DD EE FF. Both segments require a maximum standard deviation in slope of 50%.###. The most peak area should be between chords 2 . 7. and chord 1 . calibration strategies are based on the full chord.4 Automatic timing. 7. 0. maximum number of consecutive samples between check standard is 60.C (20.16. 8. 7. and 0..99.16 Method parameters in relation to data presentation are as follows: 7. Then place these lines in 268 .2 Inject to start of peak period: 25 s.50. place the transmission lines into the 1 M HCl. 2. Manual timing may be helpful in this method.2 The segments/boundaries for the calibration standards are A .17 Refer to the "Method Definition" for Mineralizable N for other method parameters not discussed here. 0.4 with the most signal-to-noise ratio in chords 1 and 5.14.00.00 to 0. A calibration passes only when both criteria are met.20 Upon completion of run. dilute samples with extracting solution and reanalyze. Report results to the nearest 0.00 mg P L-1). 7.19 If samples are outside calibration range. 7. Pump the solution for approximately 5 min to remove any precipitated reaction products.14.F are normal.18 Run samples using calibration curve. 7. Sample concentration is calculated from the regression equations.6 The instrument is calibrated with the injection of SNCS.10.1 There are 6 calibration standards (20.e.2 Bottom Scale Response: 0. C .

Handbook of laboratory methods for forest health monitoring.D. 10. Chemical and microbiological properties. 1996. Carbonate content of a soil is used to define carbonatic. Amer et al. In A. Agron.M. particle-size..L. 1982. Mineralizable N. and D.. Las Vegas. Part III.. D. Keeney. The formation of calcic and petrocalcic horizons has been related to a 269 . 1999). Environmental Protection Agency.R. 8. <2 mm (4E1a1a1a1) Air-Dry. Byers.W. NV.R. Nelson. Page. R.) Methods of soil analysis. Report Report data to the nearest mg N kg-1 soil as NH3. References Environmental Protection Agency. Comparison and evaluation of laboratory methods of obtaining an index of soil nitrogen availability. ASA and SSSA.g.S. 58:498-503.E. Part 2. 643-698. phosphate. WI. Calculations Convert extract N (mg L-1) to soil N (mg kg-1) as follows: Soil N = [(A x B x C x R x 1000)/E] where: A = Analyte reading (mg L-1) B = Extract volume (L) C = Dilution. and D. Office of Research and Development.. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Monogr. R. Talibudeen an Arambarri.E. Carbonate and Gypsum (4E) 3 N HCl Treatment (4E1) CO2 Analysis (4E1a) Manometer. 2nd ed. Environmental Monitoring Systems Laboratory. 11. 1985. J. Keeney. Calcium carbonate provides a reactive surface for adsorption and precipitation reactions. erosion. Miller. Nitrogen – inorganic forms. e. Boischot et al. The determination of calcium carbonate (CaCO3) equivalent is a criterion in soil taxonomy (Soil Survey Staff.RODI water and pump for an additional 5 min and proceed with the normal "Shut-down" procedure. Bremner. Agron. and calcareous soil classes and to define calcic and petrocalcic horizons (Soil Survey Staff. Lewis. 1966. and J.R. and genesis of the soil. if performed R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = Conversion factor to kg-basis E = Sample weight (g) 9. Application The distribution and amount of CaCO3 are important for fertility. <20 mm (4E1a1a1a2) 1. Madison. 9. U.H.). Keeney (eds. Soil analytical laboratory. trace elements. 1999). Electronic (4E1a1) Calcium Carbonates (4E1a1a1) Air-Dry. D. Section 10. available water-holding capacity. 1950). G. p. Baldwin (eds. T.. and organic acids (Loeppert and Suarez. Van Remortel. 1992. 1964. and M.

5. goggles. 5. Interferences Chemical interference is the reaction by the acid with other carbonates. 3.2 Electronic balance. oz.g. the analyst should not hold the vessel any longer than necessary to tighten the cap. oz. ≈ 5 to 10 s are required to equalize the internal pressure of the bottle. Ann Arbor. ±0. The evolved CO2 is measured manometrically. The septa should be replaced at regular intervals. and K.10-mg sensitivity 5. standard..7 Manometer. Omega Engineering. Some bottles may break without shattering. in some soils with hard carbonate concretions. e. and gloves) and eye protection (face shields. 3. 2. 4. clear glass. Equipment 5. Summary of Method The amount of carbonate in the soil is measured by treating the samples with HCl. 25. sleeve guards. 03-255-5. 54-mm diameter with 12. Use the safety showers and eyewash stations to dilute spilled acids.9 Mechanical rotating shaker. Discard any bottle with hairline cracks or obvious defects.2 x 50.). 1991). CT.4 mm (1 in). Thoroughly wash hands after handling acids. hand-held gauge and differential pressure. Connect needle to pressure tubing on transducer.8 Hypodermic needle. For best results. some of which include translocation and net accumulation of pedogenic carbonates from a variety of sources as well as the alteration of lithogenic (inherited) carbonate to pedogenic carbonate (soil-formed carbonate through in situ dissolution and reprecipitation of carbonates) (Rabenhorst et al.variety of processes. After the septum has been pierced with a needle. 23 gauge.to 20-mm basis (4E1a1a1a2). PCL-200 Series. With extensive use. carbonates are determined on both the <2-mm (4E1a1a1a1) and the 2. 5.6 Flanged stopper No. Place in machined cap. carbonates of Mg. the septa leak gas under pressure. Safety Wear protective clothing (coats.. Eberbach Corp.8 x 57. 5. or safety glasses) when handling acids. aprons.3 Threaded weighing bottles.2 mm (1/8 x 2 x 2 1/4 in) 5. that may be present in soil sample.1 Electronic balance. The amount of carbonate is then calculated as percent CaCO3. 120 mL (4 fl. O-ring seal. The CaCO3 equivalent is most commonly reported on the <2-mm base. Fisher Scientific.5 O-rings. 5.. However. The calculated CaCO3 is only a semiquantitative measurement (Nelson. The analyst should not touch the glass of the vessel when reading the pressure.4 Machined PVC caps for threaded 120-mL (4 fl. MI. Use sodium bicarbonate and water to neutralize and dilute spilled acids. When sealing the vessel. Keep other personnel away from the area when filling capsules. 140 rpm. If high pressure develops in the bottle. 48-mm neck size. High pressure may develop inside the bottle if there is a large amount of calcareous sample. Na. 270 . grind rim of bottle with 400-600 grit sandpaper on a flat glass plate. Analytical interference may be caused by temperature changes within the reaction vessel.7-mm diameter hole drilled in center. 1982). ±1mg-sensitivity 5. The internal pressure must be equalized with the atmosphere.) weighing bottles. 5. Eberbach 6140. Stanford. Do not use more than 2 g of any sample in the bottles. The gelatin capsule may leak acid while being filled. wide-mouth. release the pressure by venting the gas with a syringe needle. Use the fume hood when diluting concentrated HCl.

USP. 0.2 Methyl red indicator 6.3. NJ.025.75 g).5 to 2 g of fine-grind. Ultrex.g. The quality control check sample serves as a single point check. 12 N 6.7 Release any pressure in the bottle by piercing the stopper with a hypodermic needle. <2-mm Basis 7. 7. 271 . measure the pressure in the bottle by piercing the stopper of the cap with a hypodermic needle connected to the manometer.9. 0.3. If this happens.1mg.3 Use a 0..2 Use a 1-g sample weight. 0. 7. 7. 0.7 CaCO3. Add a few crystals of methyl red indicator. size 11.3. After this 1 h.1 Use a 2-g sample weight if effervescence is None. 7.1 Reverse osmosis deionized (RODI) water.3 Weigh 0.3 Hydrochloric acid (HCl). Remove samples from oven. if effervescence is Violent. Very Slight.5 Gelatin capsule. 7. 0.3. concentrated.4 Lubricate the O-ring of bottle cap with gylcerine from a squeeze bottle.6.5-g sample weight. Vary the sample weight according to the CaCO3 content based on effervescence of sample (procedure 1B1b2b5) as follows: 7.4 through 7. 3 N. wide-mouth bottle.05.1 Calibrate the manometer quarterly or whenever equipment changes (e.4 HCl.8 After 5 to 10 min. ASTM Type I grade of reagent water 6.rings.01%. Methyl red indicator will turn yellow if HCl is consumed by sample. place in desiccator and cool to ambient temperature. 6. Torpac Inc. The HCl may squirt or leak out of capsule. discard the capsule. assay dried basis 100.6 Gylcerine. 7. The presence of carbonates (effervescence with HCl) is also checked during lab preparation (procedure 1B1b2b5). If this reaction occurs.1. 6. Fairfield.6 Place the capsule in bottle and cap bottle immediately. Proceed as outlined in Sections 7. old rubber septum replaced).2. Shake the bottle at a rate of 140 rpm on the shaker for the first 10 min and last 10 min of a 1-h interval at room temperature (20°C ± 2°C). 7. Run 3 blanks and a quality control check sample with every batch of 24 samples. Dry the standard samples in the oven for 2 h at 110°C. air-dry soil sample to the nearest mg and place in a 120-mL. or Slight.2 A CaCl2 pH >6. 6. Procedure Manometer Calibration 7. the HCl dissolves through the capsule. 7. adjust the sample size (smaller). 0. Reagents 6. if effervescence is Strong. Dilute 500 mL of concentrated HCl with 1500 mL RODI water. 0. 10 mL. 7.4. 0. Put the gylcerine in a small squeeze bottle and use as a lubricant for the O.5.5 Dispense 10 mL of 3 N HCl into a gelatin capsule and carefully place the top on the capsule.. Remove the needle after ≈ 5 to 10 s. Weigh to the nearest 0.95 is generally used as an indicator of the presence of carbonates. Calibrate by weighing three replicates of CaCO3 standards (0.

5 Carbonate = (A x B) + [C x (1-B)] where: Carbonate = Carbonate as CaCO3 on a <20-mm basis (%) A = CaCO3 in <2-mm fraction (%) B = Weight of the <20-mm fraction minus the weight of the 2. Record the manometer readings (mm Hg).2 Calculate the regression equation for the corrected manometer readings. Calculations 8. 272 . Precision and Accuracy Precision and accuracy data are available from the SSL upon request.1 Correct the manometer readings as follows: CR = (MR – BR) where: CR = Corrected reading MR = Manometer reading BR = Blank reading Three blanks are run with each batch of 24 samples. 8. <20-mm Basis 7.to 20-mm fraction on a fine-grind (<180 µm) airdry sample by the above method.4 CCE = [(CR x Slope + Intercept) /Sample Weight (g)] x AD/OD where: CCE = Calcium Carbonate Equivalent (%) in <2-mm fraction or 2. The average of three blanks is used as BR. 10. intercept) equation to estimate % CaCO3 in the sample as follows: 8.to 20-mm fraction and in the <2-mm fraction are combined and converted to a <20-mm soil basis.to 20-mm fraction divided by the weight of <20-mm fraction (procedures 1B2b2f and 3A2).9 Auto-zero the manometer before taking readings. 8.10 Determine carbonate content of the 2. 7.7.to 20-mm fraction (%) 9. 8.to 20-mm fraction CR = Corrected manometer reading AD/OD = Air-dry/oven-dry ratio (procedure 3D1) 8.11 The carbonate in the 2. Use the CaCO3 weights as the dependent variable (regressed or predicted values) and the corresponding manometer readings as the independent variable. Report Report CaCO3 equivalent as a percentage of oven-dry soil to the nearest whole number. C = CaCO3 in 2.3 Use the corrected (CR) linear regression (slope.

Am. Agron. After centrifuging. Washington. Soc. Monogr. Gypsum content of a soil is a criterion for gypsic and petrogypsic horizons and for mineralogical class at the family level (Soil Survey Staff. 49:1137-1142. Loeppert. leaching may disrupt this sequence. Office. 436. Carbonate and Gypsum (4E) Aqueous Extraction (4E2) Precipitation in Acetone (4E2a) Conductivity Bridge (4E2a1) Electrical Conductivity (4E2a1a) Gypsum. p. The percent gypsum (uncorrected) is used to calculate percent gypsum (corrected).5% gypsum (Nelson. Gypsum from deposits high in gypsum are usually highest in the lower part of the soil profile.H. gypsum. Talibudeen. break irrigation canals. Mahmoud. Nettleton (ed. WI. Gypsum is reported on both the <2. Govt. Qualitative and Quantitative (4E2a1a1) Air-Dry. Carbonate and gypsum. 2nd ed. Fixation de l’acide phosphorique sur le calcaire des sols.D. 1996. Soil Sci. p. Soil subsidence through solution and removal of gypsum can crack building foundations. Nelson. H. and V.. The percent gypsum (corrected) is used to correct the AD/OD (air-dry/oven-dry ratio). References Amer. In D. 9.T.. Madison. 1982.C. L. characteristics. In procedure 4E2a1a1. and L. Soil Sci. 61-74. 1950. Publ. WI. 2nd ed. Plant Soil 2:311-322. and make roads uneven. Part 2. Chemical and microbiological properties. DC. J.P. Book Series No. R. WI. ASA and SSSA. Wilding. and genesis of carbonate. Genesis of calcic and petrocalcic horizons in soils over carbonate rocks. Madison. 62:93-97. 2.E. In W. The gypsum content in the soil may be used to determine if reclamation of sodic soils requires chemical amendments. M. Print. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. < 2 mm (4E2a1a1a1) Air-Dry. Page. Soil Survey Staff. 1999). ASA and SSSA.A.. Madison. Acetone is added to a portion of the clear extract to precipitate the dissolved gypsum. Handb. However. ASA and SSSA. The AD/OD and corrected AD/OD are determined in procedures 3D1 and 3D3. Keeney (eds. A. 1985. 273 .L.11. The influence of the amount and the origin of calcium carbonates on the isotopically-exchangeable phosphate in calcareous soils.R. Sabel. M. USDA-NRCS Agric. P. 1964. Soil Sci. 1999. Miller. The electrical conductivity (EC) of the solution is read. Arambarri. Part 3 – Chemical methods. Agric. U. Failure can be a problem in soils with as little as 1. and J. 5. The EC reading is used to estimate the gypsum content in meq 100 g-1. < 20 mm (4E2a1a1a2) 1. Gypsum formation by precipitation of calcium sulfate (CaSO4) is usually highest at the surface layers. Application If the electrical conductivity of a soil sample >0. gypsum content is determined. In A. Rabenhorst. Carbonate and gypsum. L. R.and the <20-mm base. gypsum content (meq 100 g-1) is converted to percent gypsum (uncorrected). 437-474. Am. and D. the gypsum is redissolved in water. Suarez. and silica accumulations in soils. Summary of Method A soil sample is mixed with water to dissolve gypsum. No. Boischot. Am.) Methods of soil analysis.S.) Methods of Soil Analysis.. Spec. 1991. Soc. and D. 1982). O. J. 181-197.50 dS cm-1 by procedure 4F1a1a1. Corrosion of concrete is also associated with soil gypsum. p. West. 26. and P. Sparks (ed.L. Hebert. Zeta potential and surface area of calcium carbonate as related to phosphate sorption. F.) Occurrence. Coppenet. Sci. R.

6 Pipette. General Laboratory Centrifuge 5. MV1. 185-mm diameter. Ann Arbor. Procedure 7. use fine-ground samples to reduce sampling errors. 90 cm 5.010 N.5. Reagents 6.2 Potassium chloride (KCl). 4.5 Pipette.4 Dispenser. The corrected AD/OD uses the correction for the crystal water of gypsum.. 0. 200 oscillations min-1.8 Centrifuge tubes. Safety Acetone is highly flammable. 5.7456 g of dry reagent grade KCl in RO water and bring to 1-L volume. Dissolve 0. Gypsum content on a <2-mm basis is reported in procedure 4E2a1a1a1. 0. solvent. 5. mini. OR 5. Use a nonsparking centrifuge.0 g of fine-grind. Equipment 5. conical 5. VWR Scientific Products 6. Eberbach Corp. ±1. purity 99% 7.0-mg sensitivity 5. 274 .to 20-mm fraction prepared by procedure 1B1b2f1a1. 10 mL. Follow standard laboratory safety precautions.11 Filter paper. 6. 0° to 100°C 5.12 Funnel. Whatman No. Proper use and appropriate load balance of the centrifuge is required. Gypsum content may also be determined on the 2.5. 10 mL. MI 5. 100 mL and 10 mL 5.85 mmhos cm-1.respectively. Erhlenmeyer. Conductivity at 25°C is 1. polypropylene. 5. GLC-1.3 Acetone. Pistolpet.13 Flask. Incomplete dissolution of gypsum is also possible. Avoid open flames and sparks.2 Use a dispenser to add 100 mL of RO water to sample and 1 blank. Manostat 5.41 mmhos cm-1. In soils with large gypsum crystals.1 g).1 Electronic balance.10 Conductivity bridge and conductivity cell.1 Weigh 5. If a trace of gypsum is present. Interferences Loss of the precipitated gypsum is the most significant potential error. the sulfates of Na and K are also precipitated by acetone. The gypsum determined on the 2. The concentration limits for sulfates of Na and K are 50 and 10 meq L-1. plain. or 0.to 20-mm fraction and the gypsum determined on the fine earth (prepared by procedure 1B1b2d2) are combined and converted to a <20-mm soil basis. repeat the procedure using a smaller sample size (2. Sorvall. respectively. a 20-g sample size may be used. 7. 20 mL.1 Reverse osmosis (RO) water. Dry KCl overnight or at least 4 h in oven (105°C).14 Vortexer. electronic digital. Amber Science. with caps. Eugene. Gypsum on a <20-mm basis is reported in procedure 4E2a1a1a2. folded.25. If the EC reading is >0. Care in handling the precipitated gypsum is required. Standard laboratory equipment includes fire blankets and extinguishers for use when necessary. Eberbach 6000. 15 mL. 2V 5. Wheaton. 3. When present in sufficiently high concentrations. 250 mL 5. 0.9 Thermometer. with tips.7 Centrifuge.3 Mechanical reciprocating shaker.2 Bottles. Markson Model 1056. 1. ASTM Type III grade of reagent water 6. 250 mL. air-dry soil into a 500-mL Wheaton bottle to the nearest mg.

Digital reading should be 0.3 Cap the bottle and shake at an oscillating rate of 200 oscillations min-1 for 30 min at room temperature (20°C ± 2°C). 7.14 Carefully remove stopper and rinse it and the inside rim of tube with acetone (1 or 2 mL).21 Read the EC of dissolved precipitate by drawing up solution into cell and flush at least once.10 Use acetone (1 or 2 mL) to rinse stopper and inside rim of tube to prevent gypsum loss.6 Use a solvent dispenser to add 5 mL acetone.00.8 Carefully release pressure within tube by loosening the stopper.13 Add 5 mL of acetone to the tube.7 Cap tube with a polyethylene stopper and mix. The first few mL of filtrate is usually cloudy and should be discarded. 7. 7.7. Drain tube upside down for 5 min. 7.010 N KCl solution into the cell. 7. 7.15 Centrifuge the sample tube at 2200 rpm for 5 min. repeat the procedure using a smaller sample weight.08609 x AD/OD]/[Sample Weight (g) x 5] where: % Gypsumuc= % Gypsum in <2 mm fraction or 2 to 20-mm fraction 275 . 7.18 Stopper and shake with Vortexer until the precipitate dissolves. 7. 7. 7. 7. % Gypsumuc = [Gypsum x Water x 0. 7.16 Discard supernatant.85 mmhos cm-1.17 Use a dispenser to add 10 mL of RO water to tube. Invert and drain the tube on filter paper or on towel for 5 min. 7. Collect the clear filtrate in a 250-mL flask.11 Remove stopper and centrifuge at 2200 rpm for 5 min.4 Filter the suspension. 8.20 Flush the cell and fill with RO water. 7. 7. 7. Use Vortexer to shake sample. 7. 7.5 Pipet 5 mL of filtrate into 15-mL conical centrifuge tube. Calculations 8.1 Calculate % Gypsumuc (Gypsum uncorrected) by using Table 1 to convert EC reading (mmhos/cm) to gypsum content (meq/100 g) and proceeding with the following the equation.22 If the EC reading is >0.12 Decant and discard supernatant.9 Let stand for at least 10 min to allow the precipitate to flocculate.19 Calibrate the EC meter and cell by drawing the 0. Replace stopper. 7.

4 The following equation for calculation of % Gypsumc (gypsum corrected) assumes the crystal-water content of gypsum is 19.3 Alternatively to using Table 1.to 2-mm fraction divided by the weight of the <20-mm fraction C = Gypsum (%) in the 20. Madison.to 2-mm fraction 9. Nelson.E. 1999. R. Determining soil gypsum content and expressing properties of gypsiferous soils. 1978. Agron. ASA and SSSA. = Volume RO water (100 mL) to dissolve gypsum = Conversion factor (gypsum % = meq 100 g-1 x 0. The corrected AD/OD (procedure 6F3) uses the correction for the crystal water of gypsum.5 Use the % Gypsumuc to recalculate the AD/OD (procedure 3D1). Govt.Gypsum Water 0. 436. Chemical and microbiological properties. Report Report gypsum as a percent to the nearest whole unit. 1982. DC.) Methods of soil analysis. References Nelson. Nettleton. Soc.08609) = Air-dry/oven-dry ratio.. Refer to Table 1.1579713 x Log (EC – blank)) x Water x 0.B)] where: A = Gypsum (%) in <2-mm fraction B = Weight of the <20-mm fraction minus the 20. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. 9. and W.. Handb.C. 42:659-661. 10. Soil Sci.420384 + 1. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. calculate % Gypsumuc from the following equation: Result = (Exp (2. 2nd ed. L. 11.08609 AD/OD 5 = Gypsum (meq L-1). In A.001942 x % Gypsumuc] 8.S. Part 2.08609 x ADOD)/(Sample Weight x 5) 8. Enter Table 1 using both the x and y axis for the EC reading to determine gypsum content (meq L-1).21%).42% (Nelson et al. Klamath. R.E. Soil Survey Staff. 276 .H. Office. R. (procedure 3D1) = Filtrate (5 mL) 8. p.L. Washington. 8. and D. 181-197. Am.6 Calculate gypsum on <20-mm basis (procedure 4E2a1a1) as follows: (%) Gypsum = A x B + [C x (1 . J.2 Table 1 converts EC (mmhos cm-1) to gypsum (meq L-1) for the above calculations.R. USDA-NRCS Agric. Keeney (eds. 1978) as opposed to the theoretical water content (20. 2nd ed. Monogr. % Gypsumc = [% Gypsumuc]/[1 + 0. Page. U. Print.D. WI. Carbonate and gypsum. Miller. 8.

Amber Science.9 |10.09 0.50 3. 5. with lids.00 6.Table 1.00 10. If salt prediction or conductivity is <0. 30 mL (1 fl.4 Dispenser.88 6. Safety No significant hazards are associated with this procedure.00 5.85 3.00 2.70 8. a correction may be required.90 2.45 6.70 0.70 0.00 3.55 9. 0 to 10 mL 277 .98 1.20 3.98 4.0 | 0.25 6.).8 | 8. and generally.31 1.48 4.01 0. 1954).15 9.04 8. with automatic temperature adjustment.0 |11. Markson Model 1056.90 3. Convert EC reading (mmhos cm-1) to gypsum content (meq L-1) ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ EC | 0.80 2. Summary of Method A soil sample is mixed with water and allowed to stand overnight. Application Salt prediction is used not only to predict which soils have measurable amounts of soluble salts but also to predict the quantity and the appropriate dilutions for salt analyses of those soils.80 4.60 2.06 0. If the temperature deviates significantly. Inc.88 11. Follow standard laboratory safety practices. Exposure to air can cause gains and losses of water and dissolved gases significantly affecting EC readings.15 7.70 6.80 1.35 4.5 | 5.78 7. 25 ± 0.1°C.58 0. Provide airtight storage of KCl solution and samples to prevent soil release of alkaliearth cations. ±1.45 8.05 0.50 10. OR 5.3 | 2.80 0.6 | 6. Interferences Reverse osmosis deionized water is used to zero and flush the conductivity cell.08 0.22 1.7 | 7.25 mmhos cm-1 (dS cm-1) soils are considered nonsalty.95 7.28 0.28 9.30 2.40 9. no other salt analyses are performed on these soils by the SSL.75 5.38 5.50 1. 4.65 7. Eugene.00 0.70 9.32 8.15 1.00 11.38 10.82 6.12 0.10 2.52 7.89 0.58 6.90 8. The electrical conductivity (EC) of the mixture is measured using an electronic bridge.4 | 3.2 Conductivity bridge and conductivity cell.22 4.1 Electronic balance.02 0. 3.10 3.40 0.3 Plastic cups.0-mg sensitivity 5.25 10.12 5.03 0.30 3.2 | 1.18 8. 2.90 0.05 7.40 3.40 7.10 1. The extract temperature is assumed to be 25°C. MD 5.12 10.40 2. Sweetheart Cup Co. <2 mm (4F1a1a1a1) 1. oz.72 0.50 5.04 0.35 6. Owings Mills.50 2.05 9.. Equipment 5.70 4.1 | 0.62 10.85 0.95 9.10 4.60 3.07 0. The EC by this method (4F1a1a1) is used to indicate the presence of soluble salts (U.62 5.60 4. Repipet or equivalent.40 1.60 1.30 Electrical Conductivity and Soluble Salts (4F) Aqueous Extraction (4F1) 1:2 Extraction (4F1a) Conductivity Bridge (4F1a1) Electrical Conductivity (4F1a1a) Salt Prediction (4F1a1a1) Air-Dry.S.20 2.75 10.82 8.25 5. Salinity Laboratory Staff.

2 Use the following relationship to estimate the total soluble cation or anion concentration (meq L-1) in the soil. L. 7. are common in. excessive amounts of soluble salts and/or exchangeable sodium (ES). 11.A. Report Report prediction conductance to the nearest 0.S. 8. air-dry soil in a 30-mL (1-oz) condiment cup.01 mmhos cm-1. References U. Salinity Laboratory Staff. Washington. Govt.0 g of <2-mm.6. cap. i.01 mmhos cm-1 (dS m-1).7456 g of KCl in RODI water and bring to 1-L volume. Richards (ed.S. 160 p.010 N KCl (1. Calculations 8.412 mmhos cm-1. Dry KCl overnight in oven (110°C). 7. These soils are 278 . 60.2 Add 10 mL of RO water to sample using a Repipet dispenser. Procedure 7.2 Potassium chloride (KCl).1 No calculations are required for this procedure.) Diagnosis and improvement of saline and alkali soils.4 Standardize the conductivity bridge using RO water (blank) and 0. 1954. 7.1 Reverse osmosis (RO) water.6 Record conductance to 0. 8.3 Swirl to mix.e. EC (mmhos cm-1) x 20 = Cation (meq g-1 soil) EC (mmhos cm-1) x 20 = Anion (meq g-1 soil) 9.1 Weigh 5. Reagents 6. Office. EC (mmhos cm-1) x 10 = Cation or Anion (meq L-1) 8.3 Use the following relationship to estimate the total soluble cation or anion concentration (meq g-1 oven-dry soil) in the soil. 7.41 mmhos cm-1).010 N.. 10. though not restricted to.5 Read conductance of supernatant solution directly from the bridge. and allow to stand overnight. U. ASTM Type III grade of reagent water 6. Dissolve 0. Conductivity at 25°C is 1. 0. USDA Handb. Electrical Conductivity and Soluble Salts (4F) Saturated Paste (4F2) Salt-affected soils. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. DC. 7. Print. 7. arid and semi-arid regions.

The water-soluble cations of Ca2+. Cl-. the classification of salt-affected soils has been based on the soluble salt concentrations in extracted soil solutions and on the exchangeable sodium percentage (ESP) in the associated soil (Bohn et al. Soil texture and plant species also are factors in this plant response to saline soils. Salinity Laboratory Staff. If salt predictions or conductances are <0. i. Electrical conductivity and soil resistivity of saturated paste are measured in procedures 4F2b1 and 4F2b2. In soil taxonomy. An experienced analyst should be able to repeat the saturated paste preparation to an SP within 5%. and because this soil:water ratio is often related in a predictable manner to field soil water contents (Rhoades. The ESP and SAR are calculated in procedures 4F3a1 and 4F3b.1% or an EC >4 mmhos cm-1. the amount of moisture in the saturated paste. The SP. this ratio is standardized to obtain results that can be applied and interpreted universally. Soil salinity is conventionally defined and measured on aqueous extracts of saturated soil pastes (U...e. 1954). The saturated paste extract is obtained with an automatic extractor (4F2c1). major dissolved inorganic solutes (Rhoades. and generally. the ESP and the Na-adsorption ratio (SAR) have been used as criteria for natric horizons (Soil Survey Staff. and salinealkali soils have properties of both saline and alkali soils (U. Salt composition and distribution in the soil profile affect the plant response. 1982). Soil solutions obtained at lower soil moisture conditions are more labor intensive and require special equipment. F-. CH3COO-.are measured by ion chromatography in procedures 4F2c1b1a1-8... Therefore. 1979). The saturated paste pH is measured in procedure 4C1a1a2. Salinity Laboratory Staff. Estimated total salt is calculated in procedure 4F3c. The SSL measures salinity on aqueous extracts of saturated soil pastes. (U..e. respectively. osmotic stress. over a considerable textural range. i. In general. K+. saline soils have been defined as having a salt content >0. NO3-. 1982).e. Salinity Laboratory Staff. Mg2+.e.S. SP ≈ 4 x 15-bar water SP ≈ 2 x upper end field soil moisture content AWC ≈ SP/4 where: Sp = Saturation percentage AWC = Available water capacity 279 . soils are considered nonsalty. The SP can be related directly to the field moisture range. The SSL also performs a salt prediction test (procedure 4F1a1a1) which is used not only to predict those soils that have measurable amounts of soluble salts but also to predict the quantity and the appropriate dilutions for salt analyses of those soils. no other salt analyses are performed on these soils by the SSL. respectively. respectively. and nutritional imbalances. The measurable absolute and relative amounts of various solutes are influenced by the soil:water ratio at which the soil solution extract is made. 1999). respectively.25 mmhos cm-1. respectively. Measurements on soils. i.usually described and characterized in terms of the soluble salt concentrations. The water-soluble anions of Br. pressure or vacuum. PO43-. The carbonate and bicarbonate concentrations are determined by acid titration procedures 4F2c1c1a1-2. and the saturation percentage (SP) determined (4F2a1). alkali soils have an ESP of >15%. and SO42.S. is an important measurement. The saturated paste is prepared (4F2). 1954). This soil:water ratio is used because it is the lowest reproducible ratio at which the extract for analysis can be readily removed from the soil with common laboratory equipment. specific ion effects.S. 1954) indicate the following general rules of thumb. Traditionally. NO2-. and Na+ are measured by atomic absorption spectrophotometry in procedures 4F2c1a1-4. i.

1954) as follows: Pss ≈ (Psw x SP)/100 The ECs (mmhos cm-1) may be used to estimate the osmotic potential (OP) in atmospheres of a solution (U.25/Rs where: 0. Salinity Laboratory Staff. Salinity Laboratory Staff. The ECs has been related to Rs (U. Salinity Laboratory Staff.25 = Constant for Bureau of Soils electrode cup Historically.e. The unit EC x 103 is called mmhos cm-1.5 6. Salinity Laboratory Staff. i.. preparation of saturated soil paste. as the relationship is markedly influenced by variations in SP. Salinity Laboratory Staff. respectively. at the upper (saturated) and lower (dry) ends of the field moisture range. 1954) as follows: Psw ≈ 0. 1954) as follows: OP ≈ 0.S.S.S. respectively. the preceding SP relationships may be redefined (U. the ECs is adjusted to 60°F (15.0 to 6. The ECs and Rs increase ≈ 2% per °C.S. and soil mineral conductivity. However. 1954) by the equation as follows: ECs ≈ 0.. ECs is more closely related to plant response (U. The SSL determines the ECs and Rs in procedures 8A3a and 8E1.5°C) basis before interpretative use. and the 15-bar water content has been measured. The ECs (mmhos cm-1) may be used to estimate the salt percentage (Psw) in solution (U. If the soil texture is known. 1954) as follows: 15 Bar Water % 2. there is a limited correlation between ECs and Rs. than the Rs measurement.064 x ECs (mmhos cm-1) The preceding equation may be used to estimate the salt percentage in the soil (Pss) (U. i.e. Furthermore. the ECs is the easier measurement from which to make interpretations.Therefore. salinity.36 x ECs (mmhos cm-1) The ECs (mmhos cm-1) may be used to estimate the total cation or anion concentration (meq L ) of the solution (U. Salinity Laboratory Staff. the salt concentration of the soil solution is ≈ 4x and 2x the concentration in the saturation extract. The ECs measurement requires more time.6 to 15 >15 >15 Texture Relationship Coarse Medium Fine Organic SP ≈ 6 1/3 x 15 bar SP ≈ 4 x 15 bar SP ≈ 3 1/4 x 15 bar SP ≈ 3 2/3 x 15 bar The electrical conductivity of the saturated paste (ECs) is measured and is commonly reported as resistivity (Rs). Laboratory Staff. 1954) as follows: -1 Total cations ≈ 10 x ECs (mmhos cm-1) Total anions ≈ 10 x ECs (mmhos cm-1) 280 .S. 1954).S.S.

hydronium. pH and Exchangeable Acidity Significant amounts of exchangeable acidity are indicated if pH <7. and arsenite.5. strontium. aluminum.2. The less commonly analyzed cations and anions include iron. No alkaline-earth CO3. selenite.0. and nitrite. Gypsum has variable solubility in saline solutions (20 to 50 meq L-1). chloride. Bicarbonate concentration is rarely >10 meq L-1 in absence of carbonates. Check for the presence of gypsum if Ca concentration >20 meq L-1 and pH <8. 281 . fluoride. ESP.S. 1954). bicarbonate. silicate. 1954) are as follows: Total Cation and Anion Concentrations Total cations ≈ Total anions. sulfate. selenate. soluble salt composition and concentration. phosphate. cesium. exchangeable cation composition. nitrate. Salinity Laboratory Staff.5. borate. rubidium. ESP <15 may or may not be indicated if pH <8. sodium. The commonly determined soluble cations and anions in the saturation extract include calcium. and Alkaline-Earth Carbonates Alkaline-earth CO3. Some rules of thumb that apply to the saturated paste (U. magnesium. Bicarbonate concentration is seldom >3 or 4 meq L-1 if pH <7. moisture content of the mixture. pH. potassium. expressed on equivalent basis pH and Ca and Mg Concentrations Concentrations of Ca2+ and Mg2+ are seldom >2 meq L-1 at pH >9. bromide.S.2. The saturated paste pH is the apparent pH of the soil:water mixture and is a key indicator in many of these interrelations.where: ECs at 25°C A means of cross-checking chemical analyses for consistency and reliability is provided by the interrelations that exist among the various soil chemical determinations (U. arsenate. pH and Carbonate and Bicarbonate Concentrations Carbonate concentration (meq L-1) is measurable only if pH >9. lithium.5.and ESP >15 are indicated if pH >8. The saturated paste pH is dependent upon the dissolved CO2 concentration. Gypsum Gypsum is rarely present if pH >8. manganese. and the presence and amount of gypsum and alkaline-earth carbonates.are indicated if pH <7. carbonate. Salinity Laboratory Staff.

John Wiley & Sons. Govt. an aqueous extract is obtained. Richards (ed. B. Application The saturated soil paste is a particular mixture of soil and water. The saturation criteria are then rechecked. Salinity Laboratory Staff. and slides freely and cleanly from a spatula except for those soils with high clay content. more water or soil is added until criteria are met.L. 3. References Bohn. 160 p. enough water should be added immediately. After the first wetting. electrical conductivity and concentrations of the major solutes. J.L. the soil paste glistens as it reflects light. 1979. R.H. and slides freely and cleanly from a spatula except for those soils with high clay content. Interferences Special precautions must be taken for peat and muck soils and very fine or very coarsetextured soils (Rhoades.Soluble The presence of alkaline-earth carbonates prevents accurate determination of exchangeable Ca and Mg. This soil:water ratio is used because it is the lowest reproducible ratio for which enough extract for analysis can be readily removed from the soil with pressure or vacuum. p.. G. Rhoades. Therefore. U. the paste usually retains the saturated paste characteristics. With fine-textured soils.e. Part 2. 1954. require an overnight wetting to obtain a definite end point for the saturated paste.D. with a minimum of mixing. 2nd ed.. USDA Handb. flows slightly when the container is tipped. pastes of these soils usually stiffen and lose their glisten. the soluble cations (meq L-1 solution) must be measured separately and the results subtracted from the extractable bases for determination of exchangeable bases as follows: Exchangeable = Extractable . Agron. However. flows slightly when the container is tipped. Print. 167-179. McNeal. 1982. which is used in a series of chemical analyses. Chemical and microbiological properties. saturation percentage (SP) by procedure 4F2a1.The effect of soluble cations upon the exchangeable cation determination is to increase the cation concentration in the extracting solution. i. Refer to procedures 4E3c1a1-4. Washington. especially if coarse textured or woody. Dry peat and muck soils. in soils with soluble salts or carbonates. Soluble salts. U. 1982). In A. the soil paste glistens as it reflects light. 9. 60. and O'Connor.A. The mixture is covered and allowed to stand overnight. WI. i. and D. upon adding water and remixing. Soil chemistry. If the mixture fails to meet these criteria.S. 2. DC. i.) Methods of soil analysis.e.S. Upon preparation of a saturated paste. e. Summary of Method A saturated paste is prepared (4F2) by adding water to a soil sample while stirring the mixture until the soil paste meets the saturation criteria.e..A.L Page. NY.e. Office. Salinity Laboratory Staff. ASA and SSSA. NH4OAc. A saturated paste sub-sample is used to determine the moisture content.0 (procedure 4B1a1b1-4). i. New York. The dissolution of salts by the extractant necessitates an independent determination of soluble cations and a correction to the exchangeable cations.g.. L. Madison. <2 mm (4F2a1a1) 1. Keeney (eds.S. Monogr.) Diagnosis and improvement of saline and alkali soils. to 282 .R.. Miller. and because this ratio is often related in a predictable manner to the field soil water content (U. Electrical Conductivity and Soluble Salts (4F) Saturated Paste (4F2) Gravimetric (4F2a) Water Percentage (4F2a1) Air-Dry. buffered at pH 7. 1954). H.

4 Cover the container and allow the sample to stand overnight. and record the weight to the nearest mg. air-dry. ordinarily. No other significant hazards are associated with this procedure. Reagents 6. Label each moisture can with the appropriate sample number.4 Oven. thermostatically controlled.6 Plastic food containers. 7. Safety Use heat-resistant gloves to remove hot moisture cans from the oven.6 If the paste does not meet the saturation criteria. ±1-mg sensitivity 5.7 Tare a moisture can and cover. 110°C 5. 0° to 200°C 5. 283 .e. stainless steel. 4. 1920 mL (16 fl. Sweetheart Products Group. add more dry soil. Saturation Percentage Determination (4F2a1) 7.1 Place a <2-mm. 7. remix the paste with more RO water or dry soil.. Procedure Saturated Soil Paste Preparation (4F2) 7. and paste should not lose its glisten upon standing. Follow standard laboratory safety practices. Allow to stand for at least 4 h and recheck the saturation criteria. the soil paste glistens as it reflects light. hardwood handles 5. Owings Mills. If the paste becomes too wet. Care also should be taken not to overwet coarse-textured soils. 1982). ASTM Type III grade of reagent water 7.2 Add enough RO water to bring the sample nearly to saturation. This sample size is convenient to handle with the 1920-mL (16-oz) food containers and provides enough extract for most purposes. The presence of free water on the surface of the paste after standing is an indication of oversaturation in the coarse-textured soils (Rhoades.5 Thermometer.bring the sample nearly to saturation. MD 6. 7. Soils puddle easily when worked at a moisture content near field capacity.1 Aluminum cans. To reduce soil puddling and to obtain a more definite end point of the saturation criteria. oz.2 Spatulas. 7. 250-g soil sample in the food container.5 Recheck saturation criteria. paste should not stiffen markedly.) capacities with recessed lids. 5. weigh the can plus sample. At saturation. drying 5. mix with a minimum of stirring. i. flows slightly when the container is tipped.3 Occasionally tap the container on the workbench to consolidate the soil:water mixture. 7. 7. free water should not collect on the soil surface. and slides freely and cleanly off the spatula except for those soils with high clay content. The sample size varies with the number of determinations to be made upon the paste or saturation extract.1 Reverse osmosis (RO) water.3 Electronic balance.8 Add ≈ 20 to 40 g of the saturated soil paste to the moisture can. 7. Equipment 5.9 Cover the can.

Salinity Laboratory Staff. 1954).S.. Washington DC. Salinity Laboratory Staff. L. Calculations SP= [(WtSP . In A.36 ≈ OP in atmospheres (U. The cell constant is set using a standard solution. and D. Govt. Richards (ed. Other uses of this measurement include the estimation of the total cation concentration in the extract. U. 8. 1954. Print Office. the (Psw x SP)/100 ≈ Pss.S. Part 2.e. dilute solutions. R. Before calculating the SP.12 Weigh the oven-dry paste sample and record the weight. salt percentage in soil (Pss). Monogr.S. <2 mm (4F2b1a1) 1. Madison. The ECs (mmhos cm-1) x 0. WI. USDA Handb. 9. 2nd ed. J. For solutions with a low ECs. p. 10. 7. Do not place moist samples in the oven with other samples that are drying.) Methods of soil analysis.11 Remove the cans from the oven and cover immediately. Do not overcrowd the drying oven with samples.1%. 11. 60. Page.L. unless these samples have been in the oven at least 12 to 16 h. Chemical and microbiological properties. Soluble Salts.) Diagnosis and improvement of saline and alkali soils. Salinity Laboratory Staff.WtOD)/ (WtOD)] x 100 where: SP = Saturation percentage WtSP = Weight of saturated paste WtOD = Weight of oven-dry soil 9. Allow the cans to cool for 1 h. 1982. and osmotic pressure (OP). and leave in the oven overnight (12 to 16 h). Electrical Conductivity and Soluble Salts (4F) Saturated Paste (4F2) Conductivity Bridge (4F2b) Electrical Conductivity (4F2b1) Air-Dry.064 ≈ (Psw). 160 p. ASA and SSSA.S. References Rhoades.7. U. The unit EC x 103 is called the mmhos cm-1.R. Summary of Method The ECs of the saturation extract that is prepared in procedure 4F2 is measured using a conductivity cell and a direct reading digital bridge (4F2b1). Report Report the saturation percentage to the nearest 0. place the can in a vented drying oven at 110°C. 1954). Application The electrical conductivity of the saturation extract (ECs) is used as a criterion for classifying a soil as saline. Agron. 167-179. 2. i. salt percentage in solution (Psw). the ECs (mmhos cm-1) x 10 ≈ cation concentration (meq L-1) (U.10 Remove the can cover. 284 . subtract the tare weights from the saturated paste and oven-dry weights. Keeney (eds. Precision and Accuracy Precision and accuracy are available from the SSL upon request.A. Miller.H. A drying period of 24 h or longer is recommended. and the ECs (mmhos cm-1) x 0. Do not use the SP subsample for other analyses. 7.D.

7.1 Reverse osmosis (RODI) water. Markson Model 1096. Office. Reading is started on the "C" Scale.00". with automatic temperature adjustment. for rinse and KCl preparation 6. Calculations No calculations are required for this procedure. U. OR 6. 4. 160 p. 0.) Diagnosis and improvement of saline and alkali soils. 10. 25± 0.S. If the temperature deviates significantly.41". ASTM Type I grade of reagent water. Dissolve 0.5 When the reading has stabilized. Interferences Reverse osmosis deionized water is used to zero and flush the conductivity cell. Print. USDA Handb. Report Report ECs to the nearest 0.010 N. Draw up extract a second time. Amber Science. 11. record the ECs. Reagents 6. Safety No significant hazards are associated with this procedure. 7.4 Read the electrical conductivity of saturation extract (ECs) by drawing up the extract into the cell and flush at least once if the cell has not been dried. a correction may be required. 1954.3 Flush the cell and fill with RODI water.A. Provide airtight storage of KCl solution and samples to prevent soil release of alkaliearth cations. Washington. 7.412 mmhos cm-1.2 Potassium chloride (KCl). Salinity Laboratory Staff. 285 .010 N KCl solution into the cell. References U. 5. Follow standard laboratory safety procedures.1 Conductivity bridge and conductivity cell. 7. Richards (ed. The extract temperature is assumed to be 25°C.7456 g of KCl in RODI water and bring to 1-L volume.1 Calibrate the conductivity meter and cell by drawing the 0.01 mmhos cm-1 (dS m-1). 7.1°C. DC. L.S. Conductivity at 25°C is 1.3. Eugene. 8. Rinse the cell with RODI water and ensure that the conductivity reading falls to zero. Higher readings may require the use of the "D" or "E" Scales. Dry KCl overnight in oven (110°C). Exposure to air can cause gains and losses of water and dissolved gases significantly affecting EC readings. 9. 60. Verify that digital reading is "0.2 Set the meter to "D" Scale and adjust the digital reading to "1. Govt. Equipment 5. Procedure 7. Precision and Accuracy Precision and accuracy data are available from the Soil Survey upon request.

25. cell constant is defined as 0.3 Bureau of Soils electrode cup. 5.1 Fill the electrode cup with the saturated paste that is prepared in procedure 4F2. 3. 5. 286 . 5. Inc. Standard Wheatstone. Industrial Instruments. 7. There is a limited correlation between ECs and Rs. and the results are reproducible. Make sure that the surfaces of the cup and holder are clean and bright.5°C) basis using a fourth order equation (Benham.1 Conductivity bridge. 4. The resistance is measured (procedure 4F2b2). Level the soil paste by striking off the excess with a spatula. Model RC 16B2. The resistance (ohms) is converted to a 60°F (15. The temperature of the paste is measured. soil cup Cel-M. Application The resistivity of the soil paste is mainly used to estimate the salt content in the soil.3 Set the conductivity meter to 1000 cycles s-1 and adjust the multiplier range and the dial control to obtain the most distinct butterfly pattern on the fluorescent tube.4 Thermometer. salinity. Soil Survey Staff.Electrical Conductivity and Soluble Salts (4F) Saturated Paste (4F2) Conductivity Bridge (4F2b) Resistivity (4F2b2) Air-Dry.2 Place the cup in the cell holder. 7. Adjustment of the sensitivity control also may be necessary. as the relationship is markedly influenced by variations in SP. Gently tap the cup to remove air bubbles. 1951). the measurements can be made quickly. Beckman Instruments. Many agencies use the Bureau of Soils electrode cup to estimate the soluble salt content in soils (Davis and Bryan. 7. 5. Equipment 5. <2 mm (4F2b2a1) 1. Follow standard laboratory safety practices. Use steel wool or fine sandpaper to carefully clean the surfaces. and soil mineral conductivity. Safety No significant hazards are associated with this procedure. There is no simple method to convert saturation extract electrical conductivity to soil paste resistivity or vice versa. 2003). 2. 1910. Inc.5 Record the resistivity. Procedure 7. 0 to 100°C 6. Reagents No reagents or consumables are used in this procedure. Summary of Method A saturated paste that is prepared in procedure 4F2 is placed in an electrode cup.4 Measure resistivity.2 Soil cup cell holder. Interferences No significant interferences are known to affect the saturated paste resistivity measurement. 7. 7. The apparatus is simple and rugged.

Precision and Accuracy Precision and accuracy data are available from the SSL upon request.2020657e-08B4) x CxDxE Where: A = Resistance (ohms) corrected to 60oF B = Temperature (oF) at which the resistance was measured C = Resistance (ohms) measured at temperature B D = Electrode cup cell factor E = Scale (range multiplier) 9. Bur.7. 2003. Means. 10. 1951. DC. Alternatively. and H. A = (-0. 287 .5°C). R.H. The electrical bridge for the determination of soluble salts in soils. 36 pp.028627073B .6 Place a thermometer in the saturated paste. Davis. NE. Report Report saturated paste resistivity in units of ohms at 60°F (15. 61.00037976971B2 + 3.5°C) to the nearest whole number. Lincoln..013840786 + 0. Calculations Use Table 1 to convert measured resistance to specific resistance at 60°F (15. An electrical method of determining the soluble salt content of soils.7891593e-06B3 -1. Office. Soil survey manual.C. Resistivity (ohms cm-1) = ohms @ 60° F x electrode cup cell factor.. USDA. Soil resistivity temperature correction.. record the temperature. 8. Soils Bull. and T. Whitney. Washington.0. When the temperature is stabilized. 1910. 11. illus. Soils Bul. References Benham. 1897.O. USDA-SCS. 8. Print. Soil Survey Staff. 30 pp. Div. Govt. Bryan. M. USDA. USDA-NRCS. the following equation may be used reducing soil paste resistance readings to values at 60°F with final results reported to 4 significant figures. E.

1000 2000 3000 4000 5000 6000 7000 8000 9000 40 735 1470 2205 2940 3675 4410 5145 5880 42 763 1526 2289 3052 3815 4578 5341 6104 44 788 1576 2364 3152 3940 4728 5516 6304 46 814 1628 2442 3256 4070 4884 5698 6512 48 843 1686 2529 3372 4215 5058 5901 6744 50 867 1734 2601 3468 4335 5202 6069 6936 52 893 1786 2679 3572 4465 5358 6251 7144 54 917 1834 2751 3668 4585 5502 6419 7336 56 947 1894 2841 3788 4735 5682 6629 7576 58 974 1948 2922 3896 4870 5844 6818 7792 60 1000 2000 3000 4000 5000 6000 7000 8000 62 1027 2054 3081 4108 5135 6162 7189 8216 64 1054 2108 3162 4216 5270 6324 7378 8432 66 1081 2162 3243 4324 5405 6486 7567 8648 68 1110 2220 3330 4440 5550 6660 7770 8880 70 1140 2280 3420 4560 5700 6840 7980 9120 72 1170 2340 3510 4680 5850 7020 8190 9360 74 1201 2402 3603 4804 6005 7206 8407 9608 76 1230 2460 3690 4920 6150 7380 8610 9840 78 1261 2522 3783 5044 6305 7566 8827 10088 80 1294 2588 3882 5176 6470 7764 9058 10352 82 1327 2654 3981 5308 6635 7962 9289 10616 84 1359 2718 4077 5436 6795 8154 9513 10872 86 1393 2786 4179 5572 6965 8358 9751 11144 88 1427 2854 4281 5708 7135 8562 9989 11416 90 1460 2920 4380 5840 7300 8760 10220 11680 92 1495 2990 4485 5980 7475 8970 10465 11960 94 1532 3064 4596 6128 7660 9192 10724 12256 96 1570 3140 4710 6280 7850 9420 10990 12560 98 1611 3222 4833 6444 8055 9666 11277 12888 --------------------------------------------------------------------------------------------------------6615 6867 7092 7326 7587 7803 8037 8253 8523 8766 9000 9243 9486 9729 9990 10260 10530 10809 11070 11349 11646 11943 12231 12537 12843 13140 13455 13788 14130 14499 288 .Table 1. 1897). Bureau of soils data for reducing soil paste resistance readings to values at 60°F (Whitney and Means. ---------------------------------------------------------------------------------------------------------------Temp Ohms ---------------------------------------------------------------------------------------------------------------°F.

soluble salt composition and electrical conductivity.6 Syringe filters..1 Prepare the saturated paste extract cup to receive the saturated paste (procedure 4E3) by placing a 3-cm diameter filter paper circle over the center of the cup followed by two 9-cm diameter filter paper circles. Equipment 5. water-soluble cations (procedure 4F2c1a1-4) and water-soluble anions (procedures 4F2c1b1a1-8 and 4F2c1c1a1-2).g.g. 4. 2.4 Rubber tubing. NJ 5. Cliffton. Interferences Some saturated pastes are difficult to extract. 0. Lincoln. soil dispersion and puddling. MAVCO Industries.2 Paste extraction cups.4 mm (1/8 ID x 1/16 OD x 1 in) 5. Whatman No.1 Reverse osmosis (RO) water. 7. e.2 ID x 1. 3. and the saturated paste is extracted (4F2c1).Electrical Conductivity and Soluble Salts (4F) Saturated Paste (4F2) Saturated Paste Extraction (4F2c) Automatic Extractor (4F2c1) 1. Summary of Method The saturated paste (prepared in 4F2) is transferred to a plastic filter funnel fitted with filter paper.. 3 and 9-cm diameter.7 Filter paper. for mechanical vacuum extractors 5. High speed centrifuging or filtration of the extract also may be necessary.2 Place the extraction syringe on the lower disk of the mechanical vacuum extractor. The funnel is placed on a mechanical vacuum extractor (Holmgren et al. 1954). Procedure 7.3 Syringes. sodium hexametaphosphate may be added to prevent calcium carbonate precipitation in the extract. Co. 40 or equivalent 6. If the extract is to be stored for an extended period. 5. Repeated extractions may be necessary to obtain sufficient extract. 3.6 OD x 6. Follow standard laboratory procedures.e. 1977). These soil properties or characteristics are related in turn to the plant response to salinity (U. SAMPLETEX.1 Mechanical vacuum extractor. 9-cm diameter. i. Salinity Laboratory Staff. The extract is used in subsequent chemical analyses. Safety No significant hazards are associated with this procedure. NE 5.5 Polycons.. The saturated paste extract derived from the saturated paste is an important aqueous solution because many soil properties have been related to the composition of the saturation extract. for extraction 5. Ensure there is no trapped air between the two 9-cm filter paper circles.S. e. 60 mL. Application The saturated paste is operationally defined so that it may be reproduced by a trained analyst using limited equipment. Richards Mfg. Reagents 6.. polypropylene. Slightly moisten the filter paper to ensure that it remains in place.45-µm diameter. 289 . ASTM Type III grade of reagent water 7. Whatman. disposable. 5. 24-place.

Am. Carefully transfer the saturated paste into the extraction cup. Washington. References Holmgren. turn off the power.8 If insufficient extract has been obtained. Richards (ed. 7.5 Turn on the extractor. 7. 1954. Electrical Conductivity and Soluble Salts (4F) Saturated Paste (4F2) Saturated Paste Extraction (4F2c) Automatic Extractor (4F2c1) Atomic Absorption Spectrophotometry (4F2c1a) Calcium. Remove excess air in the syringe and restart the extractor. Soil Sci. U. Mg2+. then store samples at 4°C. R. Report None. USDA Handb. 7. 41:1207-1208. Print. Set the extraction time to ≈ 1 h. 10. Office. Do not pull plunger from the barrel of the syringe. 8. and Sodium (4F2c1a1-4) Air-Dry. Potassium. Carefully remove the syringe containing the extract.C. 11. place a plastic cover over the extraction cup to retard evaporation. 160 p. L. Juve.S. Application The commonly determined soluble cations are Ca2+.3 Use a clamp to close rubber tubing on the bottom of the paste extraction cup. Magnesium.45 µm diameter syringe filter and express the extract into a polycon. and Na+. and R. 1977. If extracts are not to be determined immediately after collection. Salinity Laboratory Staff. Geschwender. J. Gently tap the cup to remove entrapped air in the paste.A. mixing with any "unused" paste.6 When the extractor stops. and re-extracting with a clean extraction cup or centrifuging. 7. measurable amounts of Fe and Al may be present. Govt. 9. 7.4 When all cups are ready to extract. George G. connect the syringe and remove the clamp. Alternate methods are to extract any "unused" saturated paste in a new extraction cup or to reextract by removing the top "moist" paste from the extraction cup. K+. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. pull the plunger of the syringe down. Determination of soluble 290 .L. A mechanically controlled variable rate leaching device. 7. Place cups on the extractor. DC. re-extract by repositioning the extractor to its starting configuration.9 Filtering the saturation extract is recommended to prevent the development of microorganisms.S. Calculations No calculations are required for this procedure.7. U..7 If sufficient extract has been obtained. In soils with a low saturation pH.S. Connect the syringe to a 0. <2 mm (4F2c1a1-4a1) 1.) Diagnosis and improvement of saline and alkali soils. Leave the rubber tubing on the sample tube. Slowing the extraction time to an overnight extraction may be necessary to obtain sufficient extract. 60.

2000 mg L-1. 4. 6 N.3 Autosampler. Cooling the solution is necessary. Norwalk. 291 . Ca2+. Summary of Method The saturation extract from procedure 4F2c1 is diluted with an ionization suppressant (La2O3).3 HCl. Slowly and cautiously add 500 mL of 6 N HCl to dissolve the La2O3. Perkin-Elmer Corp. 2. The analytes are measured by an atomic absorption spectrophotometer (AA). Complete analyses of the soluble ions provide a means to determine total salt content of the soils and salt content at field moisture conditions. Follow standard laboratory procedures when handling compressed gases. The relative concentrations of the various cations in the soil-water extracts also provide information on the composition of the exchangeable cations in the soil. 16 mm x 100.. 1:1 HCl:RODI. chemical. Hamilton Co. acetylene 5. Gas cylinders should be chained or bolted in an upright position. 6. Wet 152. 15-mL. 1954).5 Working lanthanum ionization suppressant solution (WLISS). Store in polyethylene container.7 Plastic test tubes. Dilute 61. and Na+. ASTM Type I grade of reagent water 6. 65. Do not use borosilicate tubes because of potential leaching of analytes.cations is used to obtain the relations between total cation concentration and other properties of saline solutions such as electrical conductivity and osmotic pressure (U. Restrict the use of concentrated HCl to a fume hood. ±1. Dilute to 2 L with RODI water. Perkin-Elmer Corp. Invert to mix thoroughly. K+. NV 5.5 Single-stage regulator. Standard laboratory equipment includes fire blankets and extinguishers for use when necessary.6 Digital diluter/dispenser. CT 5. Mg2+. 3. CT 5.S. PerkinElmer Corp.2 Hydrochloric acid (HCl).9 Peristaltic pump 6. are reported in meq L-1 (mmol (+) L-1) in procedures 4F2c1a1-4. Avoid open flames and sparks..0-mg sensitivity 5. Acetylene is highly flammable.000 mg L-1. concentrated 12 N 6. for sample dilution and sample changer 5. Interferences There are four types of interferences (matrix. depending upon the particular analyte selected. with syringes 10000 and 1000 µL. respectively. Salinity Laboratory Staff. Store in polyethylene container. 6. Filter solution. Equipment 5. AAnalyst 300.4 Computer. Carefully mix 1 part of concentrated HCl to 1 part RODI water. Reno. MicroLab 500.1 Electronic balance.4 Stock lanthanum ionization suppressant solution (SLISS). and ionization) in the analysis of these cations. Safety Wear protective clothing and eye protection.4 g of lanthanum oxide (La2O3) with 100 mL RODI water. The saturation extracted cations. When preparing reagents. with AA WinLab software. Make up to volume with RODI water.5 mL of SLISS with 1800 mL of RODI water (1:10). Reagents 6. polyethylene 5. AS-90.. The data are automatically recorded by a computer and printer.. double-beam. spectral.8 Containers. Norwalk. Many metal salts are extremely toxic and may be fatal if ingested. Thoroughly wash hands after handling these metal salts. Follow the manufacturer's safety precautions when using the AA. gas tight. 5. and printer 5.1 Reverse osmosis deionized (RODI) water. CT. exercise special care. Norwalk.2 Atomic absorption spectrophotometer (AAS). These interferences vary in importance.

Medium. Allow to equilibrate to room temperature before use. Invert to thoroughly mix. Prepare fresh weekly. 25 mL Mg PSSS. Allow to equilibrate to room temperature before use. Dilute 1:100 with WLISS. Store in polyethylene containers. Store in a refrigerator. 1000 mg L-1: Ca. and 200 mg L-1 K. and 2 mg L-1 K.3 MCSS Low Standard (1:400): To a 100-mL volumetric flask. Invert to thoroughly mix.4 6.2 6.5 mg L-1 Mg.5 mg L-1 Na. Invert to mix thoroughly. Invert to mix thoroughly. High. Dilute 1:100 with WLISS. Prepare fresh weekly. Dilute to volume with RODI water. In a 500-mL volumetric flask. Final concentration = 0. 6.8. Store in polyethylene containers. Dilute 1:100 with WLISS. Final concentration = 1. Medium. 0.9. Dilute 1:100 with WLISS.5 mL of PSMSS and bring to volume with RODI water. MCSS Blank = 0 mL of Ca.8. K.125 mg L-1 Mg. and 100 mL K PSSS = 500 mg L-1 Ca. Prepare fresh weekly.9. Store in polyethylene containers. High. Mg.1 6. Store in a refrigerator. Very Low. Store in polyethylene containers. Allow to equilibrate to room temperature before use. 0. add 25 mL of WSMSS and bring to volume with RODI water. Na Calibration Standards Solution (NaCSS). Prepare fresh weekly. add 50 mL of WSMSS and bring to volume with RODI water.9.5 6. Invert to mix thoroughly mix. 6. 6. MCSS Very Low Standard (1:600): To a 100-mL volumetric flask. Final concentration =2.8.9 6. Allow to equilibrate to room temperature before use. Invert to thoroughly mix. Store in polyethylene containers. Store in a refrigerator. Final concentration = 5 mg L-1 Ca. add 12. Prepare fresh weekly.3 292 . Dilute 1:100 with WLISS. Dilute RODI water 1:100 with WLISS. Final concentration = 2. Prepare fresh weekly. and K. and K. Allow to equilibrate to room temperature before use. NaCSS Medium Standard (1:200): In a 50-mL volumetric.1 MCSS High Standard (1:100): Dilute WSMSS 1:100 with WLISS.65 mL of WSMSS and bring to volume with RODI water. Allow to equilibrate to room temperature before use. and Na. Store in a refrigerator. Store in a refrigerator. Mg.5 mg L-1 K.8.25 mg L-1 Ca.25 mg L-1 Mg. Prepare fresh weekly. Store in polyethylene containers. Prepare fresh weekly.6. Low.5 mg L-1 Ca. 0. and Very Low as follows: NaCSS High Standard (1:100): Dilute Na PSMSS (1000 mg L-1) 1:100 with WLISS. Invert to thoroughly mix. and 0. high purity. 0.83 mg L-1 Ca.6 6. Allow to equilibrate to room temperature before use. 50 mg L-1 Mg.08 mg L-1 Mg. Store in polyethylene containers.33 mg L-1 K. Final concentration = 10 mg L-1 Na. Mixed calibration standards solution (MCSS). and Blank as follows: 6. add 16. Store in polyethylene containers. Working stock mixed standards solution (WSMSS) for Ca. Store in the refrigerator. Store in a refrigerator.8. and 0.7 6. Low. Store in a refrigerator. Final concentration = 5 mg L-1 Na. Mg.8 Primary stock standards solution (PSSS).2 MCSS Medium Standard (1:200): To a 100-mL volumetric flask. NaCSS Low Standard (1:400): In a 50-mL volumetric flask. add 25 mL of Na PSMSS and bring to volume with RODI water. add 250 mL Ca PSSS. and 1 mg L-1 K. Invert to mix thoroughly.

0 10 cm @ 30° 589.5 0.9. Prepare fresh weekly. Dilute the saturation extract sample with 100 parts of WLISS (1:100). See regeants for the preparation of the MCSS and the NaCSS.7 1.1 The 10-mL syringe is for diluent (WLISS).35 mL of PSMSS Na (1000 ppm) and bring to volume with RODI water.7 0. If reading is not within 10%. AAS Set-up and Operation 7.10 6. The 1-mL syringe is for the MCSS and saturation sample extracts (procedure 4F2c1).4 NaCSS Very Low Standard (1:600) In a 50-mL volumetric flask. 7.0 Na 10.5/10. Dilute 1:100 with WLISS. Analyte Conc. if R2 <0.5/10. Burner Wavelength Slit Fuel/Oxidant (mg L-1) & angle (nm) (mm) (C2H2/Air) ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ Ca 5.9.0 10 cm @ 0° 422. Allow to equilibrate before use.0 Mg 0. purity 99. Invert to thoroughly mix. etc. with RODI water followed by 1:100 dilution with WLISS.0 7.0 10 cm @ 0° 766.7 1.3 Refer to the manufacturer's manual for operation of the AAS.7 1. 1:20.4 Use the computer and printer to set instrument parameters and to collect and record instrument readings.6. 6.7 Perform one quality control (QC) (Low Standard) for every 12 samples. Procedure Dilution of Calibration Standards and Sample Extracts 7.8 Record analyte readings to 0. Store in a refrigerator. Compressed air with water and oil traps.5/10.99. 1:100.67 mg L-1 Na.5 Calibrate the instrument by using the MCSS and NaCSS.01 mg L-1. AAS Calibration and Analysis 7. Set the digital diluter at a 1:100 dilution. Dilute RODI water 1:100 with WLISS. 293 .. NaCSS Blank = 0 mL Na PSMSS.0 0. The data system will then associate the concentrations with the instrument responses fore each MCSS.6 If sample exceeds calibration standard. The following are only very general guidelines for instrument conditions for the various analytes. Acetylene gas. the sample is diluted 1:5. add 8. 7.6%.2 1.5/10. 7.5 6. Store in polyethylene containers. 7. the instrument is re-calibrated and QC re-analyzed.0 K 2.11 7.2 0. Rejection criteria for MCSS.5 10 cm @ 0° 285.2 Dispense the diluted sample solutions into test tubes which have been placed in the sample holders of the sample changer. Final concentration = 1.

References U. 60. nitrate. Report Report the saturation extraction cations of Ca2+. U. Fluoride. Phosphate. bicarbonate. L. if needed C = Equivalent weight where: Ca+2 = 20. Richards (ed. Calculations The instrument readings for analyte concentration are in mg L-1. Mg2+.) Diagnosis and improvement of saline and alkali soils. and the anions are separated. Application The soluble anions that are commonly determined in saline and alkali soils are carbonate. USDA Handb. phosphate. nitrite. Print. In saline and alkali soils. and nitrite are measured in solution by chromatography. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. and K+ to the nearest 0. fluoride. Na+. Nitrite. nitrate. sulfate. bicarbonate. and chloride are the anions that are found in the greatest abundance.S. In general. Na+) concentration in extract (mg L-1) B = Dilution ratio.04 mg meq-1 Mg+2 = 12. Govt. sulfate. and aluminate are found only occasionally in measurable amounts in soils. DC. soluble sulfate is usually more abundant than soluble chloride. sulfate.15 mg meq-1 Na+1 = 22. Washington. The diluted sample is injected into the ion chromatograph.1 -1 meq L (mmol (+) L-1). Mg2+. Salinity Laboratory Staff. bromide.99 mg meq-1 K+1 = 39. <2 mm (4F2c1b1a1-8a1) 1. Acetate. Phosphate. carbonate.10 mg meq-1 9. 1954).S. 10. and Sulfate (4F2c1b1a1-8) Air-Dry. chloride. U. Nitrate. 11. bromide. Office. 1974. These analyte concentrations are converted to meq L-1 as follows: Analyte Concentration in Soil (meq L-1) = (A x B)/C where: A = Analyte (Ca2+. fluoride. silicate.S. Chloride. and borate (Khym. Summary of Method The soil saturation extract is diluted according to its electrical conductivity (ECs). 160 p. 1954. Electrical Conductivity and Soluble Salts (4F) Saturated Paste (4F2) Saturated Paste Extraction (4F2c) Automatic Extractor (4F2c1) Ion Chromatograph 4F2c1b Conductivity Detector (4F2c1b1) Self-Regeneration Suppressor (4F2c1b1a) Bromide. Salinity Laboratory Staff. Chloride. K+.A.8. Carbonate and bicarbonate are determined by titration. silicate. borate. 2. A 294 .

Many metal salts are extremely toxic and may be fatal if ingested. Sunnyvale. A computer program automates these actions.6 Computer with PeakNet software and printer 5. F. Sunnyvale. CA 5.5 F. IonPac AS14.8 Poly-vials with caps. Br-. Reagents 6.024 M Na2CO3 and 0.1 6. When preparing reagents. (PSSS1000).2 6. Dionex Corp. CH3COO-.4 Primary stock standards solutions. F-.conductivity detector is used to measure the anion species and content.PSSS100 = 25 mL PO43. Dionex Corp. NO2-.5 Primary stock standards solutions (PSSS100). ASTM Type I grade of reagent water 6. ASRS – ULTRA. Make 2 L of eluent solution if chromatograph is to run overnight.3 Eluent solution. Sunnyvale. IonPac AG14.5.PSSS1000 PO43. Sunnyvale. exercise special care.PSSS1000 NO2. NV 5.PSSS1000 Br. NO3-. CH3COO-. Standard anion concentrations are used to calibrate the system. Hamilton Co.1 Ion chromatograph. double-column.are reported in meq L-1 (mmol (-) L-1) in procedures 4F2c1b1a1-8.PSSS100 = 25 mL NO3. Equipment 5. 6. CA 5.PSSS100 = 25 mL NO2.4 6. respectively.PSSS1000 295 . PO43-. Solution A: Mix 5.5. This same method may also be used for water analysis. 5 mL.5. NO3-. 4 x 250 mm. MicroLab 500. Saturation extracts of very high pH may contain organic material which may clog or poison the column. Prepare fresh weekly.PSSS1000 NO3. NO2-. Dionex Corp. Add 35 mL of Solution A and 10 mL of Solution B in a 1-L volumetric and make to volume with RODI water for a final concentration is 0.. Dionex Corp. Dionex Corp.30 g of Na2CO3 with RODI water in a 500-mL volumetric and make to volume with RODI water. Br-. Place eluent in eluent tank and degas with helium 15 min L-1 eluent (30 min total).5 Autosampler. CA 5. AS40. high purity. 3. 4 mm.. Safety Wear protective clothing and safety glasses. CA 5.20 g of NaHCO3 with RODI water in a 500-mL volumetric and make to volume with RODI water. 100 mg L-1: F-...3 Analytical column.. and PO43-. CA 5. SO42-. Low molecular weight organic anions will co-elute with inorganic anions from the column. and SO42. Cl-.2 Helium gas 6. Sunnyvale. Thoroughly wash hands after handling these metal salts. A calibration curve is determined.2 Guard column. 4 x 50 mm.. Dionex DX-120. with syringes 10000 and 1000 µL. 5.025 M NaHCO3. and the anion concentrations are calculated. 1000 mg L-1: Cl-.. Make fresh daily. NO2-.PSSS100 = 25 mL of Br. Reno. conductivity detection. Solution B: Mix 4. gas tight. Filtering after dilution removes the particles. Br-. Follow the manufacturer's safety precautions when using the chromatograph. The saturation extract anions. CA 6.1 Reverse osmosis deionized filtered (RODI). 6.PSSS100 = 25 mL F.5. Interferences Some saturation extracts contain suspended solids. Dionex Corp. NO3-. and PO43-.3 6. Saturation extracts of acid soils that contain Fe and/or Al may precipitate and clog the separator column.4 Self-regeneration suppressor. Sunnyvale. In five 250-mL volumetric flasks add as follows: 6. 4.5.7 Digital diluter/dispenser.

5 mL F. NO3-. and PO43-.6. and PO43-. and 3. 6. multiply the ECs (procedure 4F2b1) by 10. 2. Store in glass containers.76.6. Prepare fresh weekly. 30.and HCO3. 6. 0. 7.2. add 5 mL MCSSA and dilute to volume with RODI water. Store in glass containers. and PO43-..6 MCSS Blank = 0 mL of Cl-. add 20 mL MCSSA and dilute to volume with RODI water. 0. Br-. 7.4 MCSSD = In a 250-mL volumetric flask.8 mg L-1 20 mL CH3COO.52. 3. 1.5 mL Cl.176.176 mg L-1 Cl-. NO3-. Br-. add 40 mL MCSSA and dilute to volume with RODI water. SO42-.16.PSSS100 = 8. respectively.2. Store in the refrigerator.6. respectively. 0. NO3-. 0. 1.6. 3.PSSS1000 = 50 mg L-1 25 mL SO42 PSSS1000 = 100 mg L-1 12.52. Store in the refrigerator. 40. 0.6. Store in the refrigerator. NO2-. Store in the refrigerator.6. Final concentration = 20. NO3-. 6. and PO43-. F. CH3COO-. 2. Invert to thoroughly mix.+ CO32-) 296 . Invert to thoroughly mix. NO3-.3 MCSSC = In a 100-mL volumetric flask.PSSS100 = 9.PSSS100 = 8 mg L-1 20 mL NO2.4. Store in the refrigerator.(HCO3.6 Mixed calibration standards solutions (MCSS). add 25 mL MCSSA and dilute to volume with RODI water. Dilute RODI water to volume. and Blank as follows: 6.6. Prepare fresh weekly.76 mg L-1 Cl-. Prepare fresh weekly. Store in glass containers.concentrations (procedures 4F2c1c1a1-2) from the total anion concentration. F. SO42-. A. Invert to thoroughly mix.PSSS1000 = 80 mg L-1 24 mL PO43. and 1. Prepare fresh weekly. Subtract the CO32. Anion concentration (meq L-1) = ECs x 10 .PSSS100 = 8 mg L-1 22 mL Br. NO2-. 15. SO42-. Final concentration = 10. Store in glass containers. Br-. respectively. NO2-. and PO43-. SO42-.2. 3. C. 0.6 mg L-1 Dilute to volume with RODI water and invert to thoroughly mix. F-. F-. Br-. Final concentration = 5.. and 0. F-. Store in the refrigerator. 6.6. 0. add as follows 12.5. 1. B. Final concentration = 1. 1. CH3COO-.8. NO2-. 20. D. CH3COO-.88. respectively. Invert to thoroughly mix.1 To estimate the total soluble anion concentration (meq L-1).1 MCSSA = In a 250-mL volumetric flask. 6. 0. 6. SO42-.1. Prepare fresh weekly. NO2-.6.16. E. 1.PSSS100 = 5 mg L-1 20 mL NO3. Procedure Dilution of sample extracts 7. CH3COO-.52 mg L-1 Cl-. 10. CH3COO-.Dilute each PSSS100 to volume with RODI water and invert to thoroughly mix. Br-.88 mg L-1 Cl-. and 0. Store in glass containers.5 MCSSE = In a 250-mL volumetric flask.8.2 MCSSB = In a 100-mL volumetric flask. The remainder is the ≈ concentration (meq L-1) of anions to be separated by ion chromatography.

80 1.30 2.00 2.01 to 9.50 1.10 3.21 to 5.00 27.61 to 5.60 1.61 to 1.01 to 11.76 to 0.00 20.01 to 21.31 to 2.20 5.00 17.96 to 1.60 2.50 11.56 to 4.01 to 32.65 0.01 to 2.55 6.01 to 14.00 9.05 4.66 to 0.01 to 27.00 30.00 18.00 13.00 21.30 7.01 to 44.00 10.00 23.00 to 0.50 14.01 to 40.01 to 18.11 to 3.01 to 30.05 1.01 to 17.2 Dilute the saturation extract with the RODI water as follows: ECs (dS cm-1) 0.06 to 1.56 to 0.95 0.40 1.01 to 20.60 4.51 to 16.01 to 10.01 to 24.00 16.7.00 25.00 24.75 0.55 0.00 33.31 to 8.20 1.41 to 1.55 3.56 to 7.01 to 25.00 28.00 8.85 0.61 to 3.00 Dilution Factor 4 5 6 7 8 9 10 15 25 30 40 50 60 70 80 90 100 120 140 150 160 180 200 225 240 270 280 300 320 360 400 450 480 500 540 560 600 640 680 700 720 800 900 1000 297 .00 36.86 to 6.00 40.86 to 0.01 to 33.51 to 1.01 to 28.51 to 13.06 to 4.81 to 2.21 to 1.85 5.01 to 36.01 to 23.00 32.

9 µS (ON) 7. E. SO42-) concentration in extract (mg L-1) B = Dilution ratio. Calculations The instrument readings for analyte concentration are in mg L-1. These analyte concentrations are converted to meq L-1 as follows: Analyte Concentration in Soil (meq L-1) = (A x B)/C where: A = Analyte (Br-. NO3-. if needed C = Equivalent weight where: ClSO42= 35. dilute sample extracts with RODI water solution and reanalyze. Rejection criteria for MCSS. D. PO43-.4 Refer to the Manufacturer's manual for the operation of chromatograph. CH3COO-.7 Calibrate the instrument by using the MCSS (B. based on analyte). and check samples.9 to 999.63 mL min-1) 0 to 4000 psi (2200 to 2400 psi) Suppressed conductivity 0 to 999. NO2-. standards. Cl-.99. only a general set-up of the Dionex DX-120 ion chromatograph is presented. Set-up and Operation of Ion Chromatograph (IC) 7. 7.45 mg meq-1 = 48. Blank) and diluted extract samples in the Poly-vials and cap with filtercaps.5 Load the sample holder cassettes with the capped samples. C. E.5 to 4. D. If reading is not within tolerance limits (10 to 15%. Blank). The data system will then associate the concentrations with the instrument responses for each MCSS. the instrument is recalibrated and QC re-analyzed. Ranges and/or (typical settings) are as follows: Parameter Calibration Flow Setting Pressure Detection Total Conductivity Injection Volume Auto Offset Range and/or (Typical Setting) Peak Height or (Area) 0. Standard C) for every 12 samples. 7. Individual analysts may modify some or all of the operating conditions to achieve satisfactory results. 7. C.3 Place the MCSS (B.6 Use the computer and printer to set instrument parameters and to collect and record instrument readings.5 mL min-1 (1. F-.10 Record analyte readings to 0.01 mg L-1. IC Calibration and Analysis 7.9 Perform one quality control (QC) (Low Standard MCSS.9 µS 10 µL -999. R2 <0. 7.03 mg meq-1 298 .8 If samples are outside calibration. 8. Because any number of factors may cause a change in IC operating conditions.7.

Br-. silicate. nitrate. 11.1 meq L-1 (mmol (-) L-1). Englewood Cliffs. 1954). References Khym. DC. USDA Agric. < 2 mm (4F2c1c1a1-2a1) 1. In saturation extracts. carbonate is measurable if the pH >9 (U. 10. Carbonate and bicarbonate are reported in meq L-1 (mmol (+) L-1). techniques. Salinity Laboratory Staff. Therefore. and acid normality (procedures 4F2c1c1a1-2. The total dissolved ion amounts generally increase with increasing soil moisture content. Office. phosphate. NO3-. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.90 mg meq-1 CH3COO = 59. Analytical ion-exchange procedures in chemistry and biology: Theory. 1954).S. CH3COO-.F= 19.S. bicarbonate.66 mg meq-1 9. U. 1974. Print. Govt. Application The water soluble anions that usually are determined in saturation extracts are carbonate. Carbonate and bicarbonate are analyzed by titration.S. Electrical Conductivity and Soluble Salts (4F) Saturated Paste (4F2) Saturated Paste Extraction (4F2c) Automatic Extractor (4F2c1) Automatic Titrator (4F2c1c) Combination pH-Reference Electrode (4F2c1c1) Acid Titration.X. Salinity Laboratory Staff. U.25 and pH 4. some ions may decrease. and borate. While some ions increase. The carbonate and bicarbonate anions are among those ions which are most dependent upon soil moisture. equipment. 2.00 mg meq-1 NO3 = 62. in making interpretations about carbonate and bicarbonate in soil solution. Salinity Laboratory Staff. Handb. Prentice-Hall. 299 . Richards (ed. 1954. J..00 mg meq-1 Br = 79. F-. respectively). Report Report the saturation extraction anions (Cl-. 1954). chloride. The bicarbonate concentration is seldom >10 meq L-1 in the absence of carbonate anions (U.05 mg meq-1 PO43= 31. Inc. fluoride. 60. Summary of Method An aliquot of the saturation extract (procedure 4F2c) is titrated on an automatic titrator to pH 8. sulfate. there must be careful consideration about the chemistry of the soil and the soil solution. Washington.) Diagnosis and improvement of saline and alkali soils.S. The bicarbonate concentration at pH <7 seldom exceeds 3 or 4 meq L1 (U. H2SO4 (4F2c1c1a) Carbonate and Bicarbonate (4F2c1c1a1-2) Air-Dry. blank titer.60 end points. NJ.00 mg meq-1 NO2 = 46. The carbonate and bicarbonate are calculated from the titers.A. aliquot volume. and 3PO4 ) to the nearest 0. bromide. L. Salinity Laboratory Staff. nitrite. NO2-.S. SO42-.

Blanks may not titrate properly because some sources of reverse osmosis (RO) water have a low pH.18. 5.3. CA. and pH 9.00.00 and 4.4 Calibrate automatic titrator with 9.18. Equipment 5. Inc. electronic digital.1 Automatic titrator. Beckman.3 H2SO4.. Reagents 6. pH 7. Safety Wear protective clothing and eye protection. Brinkmann Instruments. Wiping the electrode dry with a cloth. concentrated. exercise care.0240 N standardized.2 Combination pH-reference electrode. changing the electrode generally solves the problem. Metrohm Ltd.67 mL of concentrated H2SO4 in 4 L of RODI degassed water (≈ 15 min). 5. or similar material may cause electrode polarization. for titrator calibration. 36 N 6. 7.2 Helium gas 6.5 units 0. sample changer.2 Add 72 mL of RO water into a titration beaker. pH 4. Use sodium bicarbonate and water to neutralize and dilute spilled acids.00 pH buffers. Final volume is 75 mL for blanks and samples.4 mV s-1 300 . Use showers and eyewash stations to dilute spilled acids.3 Refer to manufacturer's manual for operation of the automatic titrator.5 units 0. Slow electrode response time may cause over shooting the end point. If all else fails. 6.4 mV s-1 10 s pH 4. laboratory tissue. Fullerton.3 Pipettes.1 Pipet 3 mL of the fresh saturation extract (procedure 4E3c) into a 250-mL titration beaker.00. When preparing reagents. Metrohm Ltd. Interfernces Clean the electrode by rinsing with distilled water and patting it dry with tissue. with tips.. The "Set" pH parameters are listed as follows: Parameter Ep1 Dyn change pH Drift Time delay Ep2 Dyn change pH Drift Value pH 8. 7. Thoroughly wash hands after handling reagents. Set-up the automatic titrator to set end point titration mode. 5. Restrict the use of concentrated H2SO4 to the fume hood. Run 8 to 12 blanks of RO water through the titration procedure. Refer to the procedure for standardization of acids. Cleaning the electrode with detergent may decrease the response time. Carefully dilute 2. 2500 µL and 10 mL 6. with control unit. Inc. Procedure 7. ASTM Type III grade of reagent water 6. Follow the manufacturer's safety precautions when operating the automatic titrator. 2500 µL and 10 mL.4 Borax pH buffers. A combination of slowing the buret speed and increasing the time delay may help. 7. 4.3 Sulfuric acid (H2SO4). and dispenser.60 1. 7. Brinkmann Instruments. Re-standardize the acid at regular intervals. Metrohm 670 Titroprocessor. 7.1 Reverse osmosis (RO) water. 0.25 1.

(mL) = Titer of HCO3. 8. Ratios and Estimates Related to Soluble Salts (4F3) Exchangeable Sodium Percentage (ESP). In soil taxonomy. 7. Salinity Laboratory Staff. Richards (ed.A.Blank – (2 x T1) x N x 1000]/Aliquot where: T1 T2 N Blank Aliquot 1000 = Titer of CO32.S.S.Temp Stop Volume 25°C 35 mL 7.1 meq L-1 (mmol (-) L-1). 1954). pH 7. 301 . pH 7. 60. the ESP is calculated as follows: ESP = (ES/CEC-7) x 100 where: ESP = Exchangeable sodium percentage ES = Extractable sodium (NH4OAc extractable Na+. USDA Handb. pH 7. Calculated without Saturated Paste Extraction (4F3a1) Compute the exchangeable sodium percentage (ESP) by dividing the exchangeable sodium (ES) by the CEC by NH4OAc. Govt. 11. 1954. NH4OAc. References U. 10.2 HCO3. no other analyst intervention is required.0(4F3a) ESP. an ESP >15% is a criterion for natric horizons (Soil Survey Staff.0 (cmol (+) kg-1). The titers and other titration parameters are recorded on the Titroprocessor printer. L.1 CO32. Washington. Print.to the nearest 0. 1999). U.) Diagnosis and improvement of saline and alkali soils. CEC-7 = CEC by NH4OAc. The ES is calculated by subtracting the water soluble Na+ determined in procedure 4E3c1a4 from the NH4OAc extractable Na+ determined in procedure 4B1a1b4 (U.0 (CEC-7) and multiplying by 100 (procedure 4F3a1). The CEC-7 is determined in procedure 4B1a1a1a1.S.5 Place the 250-mL titration beakers in the sample changer. Office.6 Press "Start".(meq L-1) = [(T2 + T1) .7 If the titrator is operating properly. Calculations 8. When the saturation extract is not prepared.(meq L-1) =(2 T1 x N x 1000)/Aliquot 8. Report Report saturation extract CO32. 7. (cmol (+) kg-1)). DC.and HCO3. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.(mL) = Normality of H2SO4 = Average titer of blank solutions (mL) = Volume of saturation extract titrated (mL) = Conversion factor to meq L-1 9. Salinity Laboratory Staff.

a SAR >13 is a criterion for natric horizons (Soil Survey Staff. When the saturation extract is prepared.(Naws x (H2Ows/1000))]/CEC-7 where: ESP Naex Naws H2Ows CEC-7 1000 100 = Exchangeable sodium percentage = Extractable Na (NH4OAc extractable Na+. The SAR is calculated as follows: SAR = [Ca SAR Na+ Ca2+ Mg2+ ++ [ Na ] ] + [ Mg ] + ++ 2 = Sodium Adsorption Ratio = Water soluble Na+ (mmol (+) L-1). 1954). In soil taxonomy. (cmol (+) kg-1)) = Water-soluble Na (mmol (+) L-1) = Water saturation percentage = CEC by NH4OAc. The water soluble Ca2+. Mg2+. Exchangeable Na equals extractable Na minus saturation extract Na multiplied by saturation percentage.0) minus exchangeable Na. The SSL calculates the SAR by procedure 4F3b. 302 . Salinity Laboratory Staff. NH4OAc. 1954). The SAR was developed as a measurement of the quality of irrigation water.S. = Water soluble Ca2+ (mmol (+) L-1). = water soluble Mg2+ (mmol (+) L-1). Exchangeable Na can be determined with greater accuracy than the other cations in the presence of gypsum or carbonates. Calculated with Saturated Paste Extraction (4F3a2) Exchangeable Na is computed with acceptable accuracy unless salt contents > 20 mmhos cm-1 (dS m-1) at 25 C. and Na+ are determined in procedures 4F2c1a1. 1999). If exchangeable K is negligible compared to exchangeable Ca and Mg then exchangeable Ca plus Mg equals CEC (NH4OAc. and 4F2c1a4. Results are not so satisfactory for exchangeable Ca when computed in the presence of carbonates or large amounts of gypsum. This approximation is suitably reproducible for comparison between soils and for soil classification. respectively.Ratios and Estimates Related to Soluble Salts (4F3) Exchangeable Sodium Percentage (ESP). pH 7. pH 7. the SSL calculates the ESP by procedure 4F3a2 as follows: ESP = 100 x [Naex . Exchangeable Na can be computed in the same manner as exchangeable Na.0(4F3a) ESP. Salinity Laboratory Staff.0 (cmol (+) kg-1) = Conversion factor to (cmol (+) kg-1) = Conversion factor to percent Ratios and Estimates Related to Soluble Salts (4F3) Sodium Adsorption Ratio (SAR) (4F3b) Compute the sodium adsorption ratio (SAR) by dividing the molar concentration of the monovalent cation Na+ by the square root of the molar concentration of the divalent cations Ca2+ and Mg2+ (U.S. Saturation percentage is the water percentage in the saturated paste divided by 1000. pH 7. 4F2c1a2. particularly when the water is used for irrigating soils that are salt or Na affected (U.

Handb. L.000064 x SP where: ECs = Electrical conductivity of saturation extract SP = Saturation percentage of saturation extract Previous equations used to estimate total salt content are as follows: Log total salt in soil (ppm) = 0.. imogolite. etc (Jackson.g. Govt.2333 + (12. Washington. Some of these analytical procedures include X-ray diffraction analysis and selective chemical dissolutions. amorphous. of Agric. in part. Office. 160 p. poorly crystalline.S. Washington. 436. Office. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. U. 1999. Richards (ed. Washington. crystalline phyllosilicates. 60. Ratios and Estimates Related to Soluble Salts (4F3) Estimated Total Salt (4F3c) Use the charts and graphs available in U. Selective Dissolutions (4G) Background: Over the years. Handb. USDA Agric..g. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. 60. U. U.References Soil Survey Staff. L. and thereby. Print.058 x Ecs2 ) . Richards (ed.(0.81 + 1. Print. These groupings have been related. sodium pyrophosphate. Govt. and short-range-order minerals (SROMs). 1954.S. References Soil Survey Staff. e. Salinity Laboratory Staff.S. Salinity Laboratory Staff.2347 X Ecs) + (0. U. In addition.) Diagnosis and improvement of saline and alkali soils.S. Office.08 x Log ECs (mmhos cm-1) + Log SP where: ECs = Electrical conductivity of saturation extract SP = Saturation percentage of saturation extract Total salt in soil (%) = Total salt (ppm) x 10-4 These equations are applicable to saturation extracts with an ECs <20 mmhos cm-1. For more detailed discussion of these 303 . 1986). dithionite-citrate. allophane. DC. 1954.0003 x Ecs3)) x 0. DC. either conceptually or operationally. U. 436. Govt. USDA-NRCS Agric. noncrystalline. 2nd ed. DC. paracrystalline.A.S.) Diagnosis and improvement of saline and alkali soils.S.S. various terms have been used to describe broad groupings of soil components. Govt. Dept. Print.A. and ammonium oxalate extractions. The essential relations are summarized in the equations as follows: Total Salt in soil (ppm) = (-4. to various laboratory analyses. Office. 1999. U. DC. Handb. Print. Deviations occur at higher salt concentrations. Salinity Laboratory Staff (1954) to estimate total salt content (4F3c) from the electrical conductivity (ECs) of the saturation extract (procedure 4F2b1). have been operationally defined quantitatively and semiquantitatively by these analyses (Jackson. there is not always a clear delineation between dissolution data. U. USDA-NRCS Agric. 1986). These terms have not been used consistently in the literature. 2nd ed. e. Washington.S. Handb.

Higashi and Ikeda. dithionite-citrate. 1989) for the dissolution of Al. 1965). e. The use of sodium pyrophosphate extract data in conjunction with dithionite-citrate data as chemical requirements for spodic horizons have been replaced by other criteria (Soil Survey Staff. 1983. Dithionite-citrate extractable Fe (Fed) is considered a measure of "free iron" in soils and. Those soils containing hydroxyls (-OH groups). Fey and LeRoux. 1980).. Kassim et al. and some caution is required in the interpretation of these analytical data (van Wambeke. e. as such. and thermogravimetric analysis (TGA). kaolinite. Jackson et al. Refer to additional discussion on X-ray diffraction and thermal analysis in the mineralogy section (7) of this manual. it cannot be expected that chemical methods are able to perfectly distinguish the degrees of crystallinity. At one time. 1989) as commonly thought (Schwertmann and Taylor. 1992). and clay minerals (Weaver et al. In general. differential scanning colorimetry (DCS). Sodium Pyrophosphate Extraction: Sodium pyrophosphate extracting solutions tend to selectively extract mainly Fe and Al associated with organic compounds while the dithionitecitrate extractions tend to extract these compounds plus the free oxides (McKeague et al.. sodium pyrophosphate. at one time.. Selective dissolution data have been used extensively in the study of the noncrystalline material content of soils and sediments.various soil terms and the application of selective chemical extractions. However. and its effect on soil colors (Schwertmann. Parfitt and Childs. 1986). 1988. sediments. the crystalline free oxides and phyllosilicates of soils can be identified qualitatively and estimated semiquantitatively by X-ray diffraction analysis. and goethite. there exists a continuum of crystalline order. 1966. Refer to (Wada. 1993). there are limitations in using these data. sodium pyrophosphate extractable Fe and Al in conjunction with dithionite-citrate data were used to help identify translocated Al and Fe humus complexes in spodic horizons (Soil Survey Staff. Dithionite-citrate extractable Fe data are of interest in soil genesis-classification studies because of its increasing concentration with increasing weathering. With selective chemical dissolution data. Parfitt and Childs. ammonium oxalate (4G2a1a1-5). 1986). Birkeland et al. refer to Wada (1989) and Soil Survey Staff (1995). In general. there are difficulties in the adequate assessment of the portion that is extracted by particular reagents..... The ammonium oxalate procedure removes most noncrystalline and paracrystalline materials (allophane and imogolite) from soils (Higashi and Ikeda. 1984. acting as cementing agents. and sodium pyrophosphate (4G3a1-3). Selective dissolution data are necessary for independent determinations of various inorganic constituents of soils because of the difficulty with many physical analytical methods in estimating or even recognizing the presence of noncrystalline and paracrystalline free oxides or aluminosilicates mixed with crystalline soil components (Jackson et al.g. 1988). In principle. gibbsite. 1989. 1999) and. The SSL routinely performs three selective chemical dissolutions as follows: dithionite-citrate (4G1a1-3). 1968.. Schwertmann and Taylor. is pedogenically significant. 1971). Jackson. were referred to as spodic horizon criteria on the SSL data sheets. Fe. Hodges and Zelazny.g. ranging from no long-range order to paracrystalline to poorly crystalline to well crystalline (Follet et al. 1974. Hodges and Zelazny. Ammonium Oxalate Extraction: In general.. 1974. ammonium oxalate allowed to react in darkness has been considered to be a selective dissolution for noncrystalline materials (McKeague and Day. 1980) as well as short-range-ordered oxides and 304 . "Free iron" is also considered an important factor in P-fixation and soil aggregate stability. 1969. Dithionite-Citrate Extraction: The original objectives of the dithionite-citrate extraction were to determine the free Fe oxides and to remove the amorphous coatings and crystals of free Fe oxide. and Si in various clay constituents and organic complexes by treatment with different reagents.. for subsequent physical and chemical analysis of soils. Pyrophosphate not only extracts organic-bound Fe but also peptizes solid particles of ferrihydrite and in some instances even goethite (Yuan et al. and ammonium oxalate. 1975). 1992). 1977.. can sometimes be determined quantitatively by differential thermal analysis (DTA). Numerous evaluations of pyrophosphate extracts have indicated that the pyrophosphate extraction does not necessarily correlate with organicbound Fe and Al (Schuppli et al. 1976.

Al + Fe humus complexes.. 305 . In evaluating the relative proportion of Fe and Al atoms solubilized by ammonium oxalate. Childs et al. hematite. ammonium oxalate Fe and Si for the amorphic and ferrihydritic mineralogy classes and dithionite-citrate Fe for the ferritic mineralogy class. The Alo minus the Alp gives an estimate of the Al in allophane and imogolite. 1982. 1971. The Mnd is considered the "easily reducible Mn". The ammonium oxalate extraction is assumed to dissolve selectively "active" Al and Fe components that are present in noncrystalline materials as well as associated or independent poorly crystalline silica. The Feo/Fed ratio is often calculated because it is considered an approximation of the relative proportion of ferrihydrite in soils (Schwertmann. and chemical tests (Jackson. Birkeland et al. Allophane in soils can be estimated from the Alo and Sio and the pyrophosphate extractable Al (Alp) (Parfitt and Henmi. Ratios. 1992). 1990). Unlike Fed. 1989) and so does not necessarily represent the total pedogenic Al (Wada. However. Fe.. The optical density of ammonium oxalate extract (ODOE) of >0. while the ammonium oxalate extractable Fe (Feo) (probably ferrihydrite) is a measure of the paracrystalline Fe (Birkeland et al. Fey and LeRoux. Refer to the Soil Survey Staff (1995. imogolite. Schwertmann and Taylor.. Selective chemical dissolution data are used as taxonomic criteria for mineralogy classes. 1989). 1999) for more detailed discussion of these taxonomic criteria. goethite. 1989).. Ammonium oxalate extractable Alo plus 0. imogolite.. and Estimates: In a general way. 1989). and Al-humus complexes. whereas the Sio gives an estimate of the Si in allophane and imogolite. The intent of the ammonium oxalate procedure is to measure the quantities of poorly crystalline materials in the soil. 1983). 1964.g. 1985. lepidocrocite. Application. There have been conflicting data on the effect of this procedure on clay minerals. 1969. and amorphous or poorly crystallized oxides and hydroxides. and Mn (Schwertmann. e. 1985).5 Feo is also used as a taxonomic criterion for andic soil properties (Soil Survey Staff. 1999). 1977). Parfitt and Wilson. but in general. the Fed is considered to be a measure of the total pedogenic Fe. Opaline Si is not dissolved by this method (Wada. and organically-bound Al (Wada.Alp)/Sio times the molar ratio (28/27) is an estimate of the Al/Si ratio of allophane and imogolite in the soil. Walker.. the weight percent of Fe must be divided by two.. An increase in ODOE is used as an indicator of the accumulation of translocated organic materials in an illuvial horizon (Soil Survey Staff..e. 1977. McKeague et al. McKeague and Day. 1999). 1976). montmorillonite. the Ald extract is commonly less than the Alo (Childs et al. The method also extracts allophane. This procedure has been reported to dissolve very little hematite and goethite and small amounts of magnetite (Baril and Bitton.. the ammonium oxalate treatment is considered to have very little effect on phyllosilicates (kaolinite. 1983). Alo + 1⁄2 Feo. 1983. McKeague et al. The Ald and Alo are pedogenically significant. A more reliable and accurate estimation of soil properties and a better understanding of noncrystallinity are provided when ammonium oxalate extraction is used in conjunction with other selective dissolution procedures. 1986). 1977. The values of 28 and 27 represent the atomic weights of Si and Al. 1971. respectively. thermal techniques. In addition. in principle it cannot be expected that chemical methods are able to perfectly distinguish degrees of crystallinity. which can have an upper limit of thirty-three mole percent substitution (Schwertmann et al. 1977). 1999). The Alo is generally an estimate of the total pedogenic Al in soils dominated by allophane. this method is assumed to extract Al + Fe humus. The Alo represents the Al dissolved from allophane. The (Alo .. and the Alp is the Al from the Al-humus complexes alone (Parfitt and Kimble. 1959. The Ald represents the Al substituted in Fe oxides. The weight of Fe atoms is approximately twice that of Al atoms. e. and some caution is to be exercised in the interpretation of the analytical data (van Wambeke. Parfitt. and ferrihydrite.g.hydroxides of Al. 1966. the ammonium oxalate extraction is considered the most precise chemical method for measuring these soil components.25 is used as a chemical criterion for spodic materials (Soil Survey Staff. illite) or gibbsite. imogolite. At the present time. i.

1969. Benedict. Univ. Taylor. and L. In J. T.. Childs. No. Ikeda. and R.A. Bodenkd. Quat.M. Soil Sci. S. Dithionite. S. soil color. J.J. 2nd ed. and G.A. Lim. 19:99-106. 1989. and J. Bigham and E. Ltd. 172-200. M.B. Taylor. Pflanzenernaehr. IL.W. R. Minerals in soil environment. Publ. Day. 1992. Dixon and S. and W. Soc. Clay Miner. Soil Sci. Ferrihydrite in pyrophosphate extracts of podzol B horizons. Am. Can. 28:183-190. McKeague.).. 25:373-374. In J. Am. Zelazny. J. Al substitution and differential disorder in soil hematites. 1985. Bitton. Parfitt. No. R. Am. Soc. 1984. 1989.. Soil Sci. 47:1026-1032. Soc. B. Schuppli. P.. Bodenk. Z. Soc. Soil. Klute (ed. and J. U. Wilson. Soil Sci.B. and C. Allophane in New Zealand . J. Nutr.B. R.L. Teneurs elevees de fer libre et identification taxonomique de certain sols due Quebec contenant de la magnetite.. Wilmette. Weed (eds. New Zealand. 1959. 35:33-38. U. Soc. 1969. Brydon. Soil color. Relations between iron oxides. Soc.M. Fey. Can. Soil Sci. and H. In A. Higashi. Soil Sci. Schwertmann.. J. and J.H. Miles.L.D. Conditions for formation of allophane in soils. McKeague. 46:13-22.. ihre mineralogischen Formen und ihre Entstehungsweisen. and N.. 1:370-438. Soil Sci. 53:971-977. W. and B. and J.) Methods of soil analysis. 1985. Kimble. 1977. The effect of pedogenic environments on iron oxide minerals. Parfitt. Schwertmann. WI. 1964. and A.A. i.F. U.M. Dixon and S. P.. The differentiation of iron oxides in soil by extraction with ammonium oxalate solution. Aust. 5:451-463. J.. and J.. E.LeRoux. McKeague. 1975 (Mexico City). G. Z. J. Schwertmann. Birkeland. 31. No. Am. Estimation of forms of Fe and Al: a review of and analysis of contrasting soils by dissolution and Moessbauer methods. 2nd ed. 1976.. Adams. J. 49:1-9.H. and R. Res. R. Soil Res. Schwertmann. Proc.L. R. Weed (eds.M. Part 1.W. Quantitative determinations of allophane in soil clays. Publ.M. Madison. 2nd ed.B.. Dueng. Estimation of allophone and halloysite in three sequences of volcanic soils. Catena Suppl. Parfitt. Soil Sci. 306 .L. SSSA Spec. Smith.L.A. 6:23-43. 9:101-150. Adv. Clays Clay Miner. LeRoux. 1:145-180. 4:205-212. Pflanzenernahr. Parfitt. Kassim.J.C. Fitzpatrick. and soil formation. Res. Hodges. McHardy. Am. J.A. 28:343-360. 1986.L. U.. J. 28:35-42. Soil chemical analysis. Schwertmann. Wisconsin. Aust.J. 32:193-204.V. R. U. 1988.W. Am. 1980. Jackson. 1965.. Ross.K. Soil Sci. and L. WI. Dissolution of allophane by acid oxalate solution.. Clays Clay Miner.W. 1977. Jackson. Zelazny. 1974. and J. Comparison of an oxalate-extraction method and an infrared spectroscopic method for determining allophane in soil clays. Clay Conf. 1971. Differentiation of forms of extractable iron and aluminum in soils. 84:194-204.M.A. Henmi.). & II. and aluminosilicates. Proc. M. 1983. Adv.B. Burke. R.and oxalate-extractable Fe and Al as aids in differentiating various classes of soils.). 7:1-9. 1989. Clay Miner. J.A review. Parfitt. R.L. C. Iron oxides. Gafoor. The effective removal of suspended materials from pyrophosphate extracts of soils from tropical and temperate regions. 26:121-144. Oxides.W. I. Chemical dissolution techniques in the study of soil clays.L.. Appl.E.. hydroxides. U.D. Follet. Schwertmann. Mitchell. Iron oxides. Agron.N. 1966. Die fraktionierte Extraktion der freien Eisenoxide in Boden. and T. Int. Madison. 105:194-202. In J. 1982. Physical and mineralogical methods. Schwertmann. Ciolkosz (eds. Soil Sci.References: Baril. Clay Sci. Pedogenic gradients of iron and aluminum accumulation and phosphorus depletion in arctic and alpine soils as a function of time and climate.. M. Minerals in soil environment. Determination of noncrystalline soil components by weight difference after selective dissolution. U.C. 1990.

The method (4G1a1-3) described herein is not the same extraction as described in the Soil Survey Investigations Report (SSIR) No. NY. Fe.M. G. 1968. The analytes are measured by an atomic absorption spectrophotometer (AAS). J. U. K. A. Commun. Interferences There are four types of interferences (matrix. 1 (1972). 436. Inc. and C. The CD solution is a poor extractant of crystalline hydrous oxides of Al. and a clear extract obtained. The percent CD extractable Al. Soc. Soil survey laboratory information manual. Office. commonly referred to as the CBD method. 1:603-638.B. 1977. Solution is centrifuged. 42. Dixon and S. Washington. Handb. Walker. <2 mm (4G1a1-3a-b1) 1. Am.). resulting in a buffered neutral citrate-bicarbonate-dithionite (Aguilera and Jackson. and reverse osmosis deionized (RODI) water. DC. Application Dithionite-citrate (CD) is used as a selective dissolution extractant for organically complexed Fe and Al.0. Mehra and Jackson. 1989). Manganese (4G1a1-3) Air-Dry or Field Moist. Am. 3. Wada. Soil Sci. Soil Sci.S. In J. 1333-1343. Allophane and imogolite. No. depending upon the particular analyte selected.K. R. Si.L. USDA-SCS Agric. van Wambeke. sodium citrate. L. and Jackson. In soil taxonomy. 1989). Soil Survey Staff. These interferences vary in importance. A. 1999). Soil Survey Investigations Report No. Determination of silica in citratebicarbonate-dithionite extracts of soils. The CD solution does not extract opal. Govt. allophane. Print. 1989. 1995.B. Proc. and M. Summary of Method A soil sample is mixed with sodium dithionite. 1999. U.and dithionite-extractable iron. Handb. Version No. 1960. 2. Soil Sci. Am. 1953. Soils of the tropics: properties and appraisal. Soc. Minerals in soil environment. chemical. Am. No. Wang. U. Jackson.L. and ionization) in the AA analyses of these elements. 1993. the CD extractable Fe and Al are criteria for spodic placement (Soil Survey Staff. Soil Survey Staff. 47:1022-1025. Soil Sci. 32:497-501. The effects of magnetite on oxalate. Weed (eds.Survey Staff. 1.M. USDA-NRCS Agric. and amorphous aluminosilicates (Wada. or other constituents of crystalline silicate minerals (Wada. Allophane and imogolite. and Mn are reported in procedures 4G1a1-3. 1975. In J. A method for estimating organic-bound iron and aluminum contents in soils. The CD extract is diluted with RODI water. 436. 24(11&12). Office. and imogolite. Lavkulich. Weaver. Govt. 1983. Office. DC. respectively. 1: 1051-1087.S. McGraw-Hill. Yuan. DC.. 2nd ed. USDANRCS.). Washington. Print. 1969). Selective Dissolutions (4G) Dithionite-Citrate Extraction (4G1) Atomic Absorption Spectrophotometer (4G1a) Aluminum. noncrystalline hydrous oxides of Fe and Al. spectral. Plant Anal.B. 1st ed. This obsolete SSL method (6C3) incorporated sodium bicarbonate as a buffer (pH 7. and shaken overnight. This extraction is also sometimes referred to as citrate-dithionite or sodium citratedithionite.. Minerals in soil environment. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. J. Wada. Soc. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. 2nd ed.S. Syers. method 6C3. K. Soc. Print. The AAS converts absorption to analyte concentration. Soil Sci. Weed (eds. Washington. No. The data are automatically recorded by a computer and printer.B.. Dixon and S.3) in the dithionite-citrate method. 1992. Govt. 307 . Iron.

Acetylene gas is highly flammable. reagent. and 1000-mL 5. A diluting solution for Fe analysis (for a final concentration of 0.4 Sulfuric acid (H2SO4). 6. 1 1⁄2 in strokes. Gas cylinders should be chained or bolted in an upright position. Perkin-Elmer Corp. Reno. ASTM Type I grade of reagent water 6.3 Atomic absorption spectrophotometer (AAS). 15-mL. 0.2 Mechanical reciprocating shaker. 250.7 Centrifuge. for sample dilution and sample changer 5. Eberbach Corp..13 Measuring scoop. sleeve guards.0-mg sensitivity 5. purified powder 6.4 Autosampler.8 Digital diluter/dispenser. concentrated (85%).3 Sodium citrate dihydrate (Na3C6H507·2H2O).. handmade.5 to 7. Class A.1 Reverse osmosis deionized (RODI) water. MicroLab 500. MA 5. NV 5. acetylene and nitrous oxide 5. crystal. Safety Wear protective clothing (coats. 1000 mg L-1: Fe. samples are diluted 1:50 prior to analysis. polypropylene 5. Mn. 4. 100. add 25 mL of the following matrix matching mixture. ±1. Follow the manufacturer's safety precautions when using the AA..10 Test tubes. double-beam optical system. followed by diluting to 2 L with RODI water. Follow standard laboratory practices when handling compressed gases. For Fe analysis. diluting to 1000 mL and mixing thoroughly. with computer and printer 5. Hamilton Co. eye protection (face shields. Centra. Thermo IEC.4 g calibrated 5. GP-8. Needham Heights. AAnalyst.6 Single-stage regulators.9 Dispenser. Dissolve 336 g sodium citrate in approximately 1 L RODI water. resulting in the precipitation of Fe sulfides. (Note: 1:5 sample dilutions for Al and Mn are in RODI water. and gloves). Filtered extracts can yield different recoveries of Fe. Keep dithionite in a fume hood. Norwalk. MI 5. and 6 mL H3PO4 and diluting to 250 mL volume with RODI 308 . 50-mL 6. concentrated. Standard laboratory equipment includes fire blankets and extinguishers for use when necessary.12 Volumetrics. CT.11 Containers.7 Calibration standards for Fe (Section 6. with syringes 10000 and 1000 µL. even by atmospheric moisture. 6. and a breathing filter when handling dry sodium dithionite. Sodium dithionite may spontaneously ignite if allowed to become moist. Some soils may lower the pH. Perkin-Elmer Corp.5% H3PO4 in samples) may be made by adding 6. AS-90. and quality control (QC) standards. Sodium citrate complexes the reduced Fe and usually buffers the system to a pH of 6. This mixture is made by combining 20 mL Na citrate extracting solution.57 M sodium citrate. Avoid open flames and sparks. 16 mm x 100. gas tight. Equipment 5. and Al. aprons.12 mL of concentrated H3PO4 to 500 mL volume of RODI water. high purity.. 300.14 Centrifuge tubes.5 Peristaltic pump 5.5 Phosphoric acid (H3PO4).8): To each 100 mL volume of blank. Eberbach 6000.21 mL H2SO4. goggles.The redox potential of the extractant is dependent upon the pH of the extracting solution and the soil system.1 Electronic balance. or safety glasses).6 Primary Stock Standard Solution (PSSS). 6. calibration. 200 oscillations min-1. 0. CT 5. relative to unfiltered extracts.2 Sodium dithionite (Na2S2O4). Final concentration is 0. Ann Arbor. 30 mL 5. and Al. Reagents 6.3. 5.) 6. Mn. Norwalk.

10 6. H2SO4 substitutes for dithionite). 5. H2SO4 substitutes for dithionite).10. 2. add 25 mL of the following matrix matching mixture.0 mL PSSSMn 5.8.12): To each 100 mL volume of blank.5 mg Mn L-1 = 0.11 Calibration standards for Al (Section 6. 10.2 6.6 6. Also.5 mL PSSSMn 10. and then diluting to 250-mL volume with RODI water.2 80.25 mL PSSSMn 1.5 mL PSSSFe 6. Also. 20.5 mg L-1). This mixture is made by combining 200 mL Na citrate extracting solution.0 mg Fe L-1 = 2.5 mg Mn L-1 = 0. (Note: Matrix of standards is prepared to match a 1:5 dilution of samples (same as with Mn). (Note: Matrix of standards is prepared to match a 1:50 dilution of samples.0 mL PSSSMn (blank) 6.12 6.8.0 mL PSSSAl 6.5 mL PSSSMn 2. In six 100-mL volumetric flasks add as follows: 15.0 mg Fe L-1 = 0.8.0. calibration. and quality control (QC) standards.5 mg Mn L-1 = 0. After dissolution.0 mg Mn L-1 = 0.0 mg Mn L-1 = 1.9 Calibration standards for Mn (Section 6. and 0.0 mL PSSSFe 6. 1. 6.0 mg Al L-1 = 6. and 0.4 10. calibration.8 12. In seven 100-mL volumetric flasks add as follows: 6.3 15. After dissolution.6. 80. H2SO4 substitutes for dithionite).1 mL H2SO4. 2.0.0.0.0 mg L-1).1 mL H2SO4. transfer solution to a plastic bottle.4 6.25 mL PSSSFe (QC) Fill to volume with RODI water and invert to mix thoroughly.10. 15.0. 6.1 mL PSSSFe 6.0 mg Al L-1 = 10. transfer solution to a plastic bottle.0 mL PSSSFe 6.8 water.2 20.10.0 mg Al L-1) and QC (50.3 6.10): To each 100 mL volume of blank.10. In seven 100mL volumetric flasks add as follows: 6.12.10. Invert to mix thoroughly. 1.0 mg Al L-1 = 8. Prepare fresh weekly.8. 2.0 mg Fe L-1) and QC (12.5 mL PSSSFe 6.0.15 mL PSSSMn 0. This mixture is made by combining 200 mL Na citrate extracting solution.12.5.8. 20.10. Standard Fe calibration solutions (SFeCS) or working standards (25. Standard Al calibration solutions (SAlCS) or working standards (100.5 mg L-1).0.1 100.0 mL PSSSFe (blank) 6. and diluting to 250-mL volume with RODI water.5 5. add 25 mL of the following matrix matching mixture.0 mg Mn L-1 = 1.0 mg Fe L-1 = 1.10.65 mL PSSSMn (QC) 6. Invert to mix thoroughly.0 mg Mn L-1 = 0.0. and quality control (QC) standards.7 0. Prepare fresh weekly.0.0 mL PSSSAl 309 .8.3 60.0.12. 60.0.7 Fill to volume with RODI water and invert to mix thoroughly.0 mL PSSSAl 6.0 mg Fe L-1 = 1. (Note: Matrix of standards is prepared to match a 1:5 dilution of samples.0.0.5 m Fe L-1 = 1.0 mg Fe L-1 = 2.5 mL PSSSFe 6.0 mg Mn L-1) and QC (6.8.8. Standard Mn calibration solutions (SMnCS) or working standards (15.0.0.5 6. Invert to mix thoroughly.6 1. and 0.1 6.0 mg Fe L-1 = 0. 5. 40. Prepare fresh weekly. 10. Also.0 mg Fe L-1 = 0.5.1 25. 10.

The Fe.9 Dispense the diluted sample solutions into test tubes that have been placed in the holders of the sample changer. centrifuge at 4000 rpm for 15 min.13 6.0 mL PSSSAl (QC) Fill to volume with RODI water and invert to mix thoroughly.4 Place rack in shaker and shake overnight (12 to 16 h) at 200 oscillations min-1 at room temperature (20°C ± 2°C). For a 1:50 dilution of samples for Fe analysis.75 g of air-dry soil. Dilute 1 part CD sample extract with 49 parts of H3PO4 diluting solution (1:50 dilution).12.6 6.0 mL PSSSAl (blank) 50.0 mg Al L-1 = 2. transfer solution to a plastic bottle.8 A 1:5 dilution in RODI water is used for Al and Mn.1 Weigh 0. Dilute 1 part CD sample extract with 4 parts RODI water. Allow samples to sit overnight.0 mL PSSSAl 10. Dilution of Sample Extracts 7. use the H3PO4 diluting solution (see Section 6.0 mg Al L-1 = 0. 6. 7.0 mg Al L-1 = 1. 7.12.0 mg Al L-1 = 4. After dissolution.12. Place tubes in rack. If sample is moist.7 No ionization suppressant is required as the Na in the extractant is present in sufficient quantity.8 40.4 g of sodium dithionite (use one calibrated scoop) and 25 mL of sodium citrate solution. 310 .6 The following day.2 Add 0.0 mL PSSSAl 20. weigh enough soil to achieve ≈ 0.5 6.6.15 Acetylene gas. Fe.12. 7.6% Nitrous oxide. 7. and Al are determined on the AA from a clear aliquot of solution. air-dry soil sample to the nearest mg and place in an 50-mL centrifuge tube.5% H3PO4.0 mL PSSSAl 0. Mn. and Mn 7. 7. 7.75 g of <2-mm or fine-grind. AAS Set-up and Operation 7. The dilution of Fe results in a final solution concentration of 0. The following are only very general guidelines for instrument conditions for the various analytes. Procedure Extraction of Al.5 Remove tubes from shaker and manually shake tubes to dislodge any soil from cap. 7.12.4 6.10 Refer to the manufacturer’s manual for operation of the AAS. purity 99.14 6.3 Cap tubes and shake briefly by hand to dislodge soil from tube bottom.7 6.5). USP Compressed air with water and oil traps 7.0 mg Al L-1 = 5.

Calibrations are linear with calculated intercept.0 248. Mn (%) = (A x B x C x R x 100)/ (E x 1000) where: A = Sample extract reading (mg L–1) B = Extract Volume (L) C = Dilution.2 3.7 Air Mn 15. Al.0 279. followed by the typical dilution (1:5 dilution with RODI water for Al and Mn. Wavelength Burner Head Slit Fuel/Oxidant (mg L-1) (nm) (mm) ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ Fe 25. Three replicates are average for each sample. 10.1 of a percent. required R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) E = Sample weight (g) 100 = Conversion factor to 100-g basis 1000 = mg g-1 9. 7. AAS Calibration and Analysis 7. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.8 10-cm parallel 0. 7.7 N2O Typical read delay is 3 s.0 C2H2/15. and Mn to the nearest 0. 8.0 C2H2/15.7 Air Al 100.5 C2H2/15. recalibrate and reread the QC. Calculations Convert analyte concentrations (mg L-1) to percent in soil as follows: Soil Fe.2 3.7 8. It must pass within 15% to continue. a serial dilution is performed.15 If samples are outside the calibration range. 7. and integration time is 3 s but can vary depending on soil type. Report Report percent CD extractable Al.8 10-cm parallel 0.14 Use the QC after every 12th sample.0 309. Fe.11 Use the computer and printer to set instrument parameters and to collect and record instrument readings. A 1:5 dilution of the sample using the calibration blank. The QC is also read at the end of each run. Maintain matrix match between standards and diluted samples by performing this extra dilution with calibration blank. Analyte 311 .12 The instrument readings are programmed to display analyte concentration in mg L-1 (ppm). 7.Conc.13 Each element is analyzed during separate runs on the AAS. and 1:50 dilution with the H3PO4 diluting solution for Fe). If it fails. 7.16 Record analyte readings to 0.3 5-cm parallel 0.01 unit. Use the calibration reagent blank and calibration standards to calibrate the AAS.

opal. 1989).25. Interferences There are four types of interferences (matrix. acid oxalate. The ammonium oxalate extractable Al. <2 mm (4G2a2a1a-b1) 1. Data are automatically recorded by a computer and printer. and amorphous aluminosilicates (Wada. Summary of Method A soil sample is extracted with a mechanical vacuum extractor (Holmgren et al. The analytes are measured by a inductively coupled plasma atomic emission spectrophotometer (ICP-AES). oxalate-oxalic acid. Soil Sci. 1989). ammonium oxalate extractable Fe and Al are criteria for andic soil properties (Soil Survey Staff. The ammonium oxalate extract is weighed.B. Manganese. Phosphorus. The ammonium oxalate extract is diluted with reverse osmosis deionized water. Weed (eds.. If the sample contains large amounts of amorphous material (>2% Al). Dixon and S. This extraction is also sometimes referred to as acid ammonium oxalate. <2 mm (4G2a1a1-5a-b1) UV-Visible Spectrophotometer. and chemical tests. WI. 312 . i. 1989. Fe. respectively. Ammonium oxalate is a poor extractant of imogolite and layer silicates and does not extract crystalline hydrous oxides of Fe and Al. Book Series No.. 2nd ed. 2. In procedure 4G2a2a1. 1977) in a 0. References Wada. 1999. The exclusion of light reduces the dissolution effect of crystalline oxides and clay minerals.275 M ammonium oxalate. Madison. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. Selective Dissolutions (4G) Ammonium Oxalate Extraction (4G2) Automatic Extractor (4G2a) Inductively Coupled Plasma Atomic Emission Spectrophotometer (4G2a1) Radial Mode (4G2a1a) Aluminum.). 2nd ed. depending upon the particular analyte chosen. Soil Survey Staff. All these data are reported in percent except Mn and P.2 M ammonium oxalate solution buffered at pH 3. U. 436. Minerals in soil environment. Dual Beam (4G2a2) Transmittance (4G2a2a) Optical Density (4G2a2a1) Air-Dry or Field-Moist. chemical. Allophane and imogolite.e. These interferences vary in importance. thermal techniques. shaking with 0. and Si are reported in procedures 4G2a1a15. and Silicon (4G2a1a1-5) Air-Dry or Field-Moist. noncrystalline hydrous oxides of Fe and Al.S. p. Am. 1. or crystalline silicate (Wada. 1:100 soil:extractant. 3. Mn. spectral. In J.0 under darkness. Handb. 1051-1087. especially UV light. or oxalic acid-ammonium oxalate. DC. an alternate method should be used. K. USDA-NRCS Agric. Iron. The ammonium oxalate buffer extraction is sensitive to light. 1999). ASA and SSSA. In soil taxonomy. Washington. Print. P. pH 3.11. which are reported in mg kg-1. A more reliable and accurate estimation of soil properties and a better understanding of soil exchange complex is provided when ammonium oxalate extraction is used in conjunction with other selective dissolution procedures. and ionization) in the ICP analyses of these elements.B. the optical density of the extract is measured with a UV spectrophotometer at 430 nm. Application Ammonium oxalate is used as a selective dissolution extractant for organically complexed Fe and Al. allophane. Govt. Office.

6.6 Primary Si standard.8 Inductively coupled plasma atomic emission spectrophotometer (ICP-AES). 1000 mg L-1. 5. and printer 5. reservoir.J. Mix 60 mL of each primary standard (Si. polypropylene. 1000 mg L-1.5 Dispenser.. Mn.9 Automsampler.7 Containers. plastic.8 Primary P standard. 5. Fairlawn. Fisher Chemical Scientific Co.. 0.11 Single-stage regulator. mini. Equipment 5.16 Cuvettes. UV-Visible. 6. Fairlawn. Certified Reference Solution. for extraction (0. with WinLab32TM software.3 Borax pH buffers. N. Certified Reference Solution. and Al. MV1. 4. 1000 mg L-1. N. 3. NE 5. electronic digital. Solution B (acid): Dissolve 252 g of H2C2O4·H2O in 10 L of DDI water.45-µm filter).4 Primary Fe standard. Optima 4300 DV. pH 3. Fisher Chemical Scientific Co.18 for electrode calibration. The elements are added in the order (Si.6 Pipettes. polyethylene 5. Cary 50 Conc. Varian. 1000 mg L-1. Follow standard laboratory practices when handling compressed gases.J.2 Mechanical vacuum extractor.1 Electronic balance. exercise special care.10 Computer. and printer 5. Certified Reference Solution.0-mg sensitivity 5.. Fairlawn. Norwalk.4 Rubber tubing. argon 5. P) to avoid element precipitation. CT.12 Test tubes. MAVCO Industries. Fisher Chemical Scientific Co. ±1. Perkin-Elmer Corp. Fisher Scientific 5. pH 4. 10 mg L-1 313 . 6.J.15 Computer with Cary WinUV software. Mix 4 parts solution A with 3 parts solution B. N. Al.2 Ammonium oxalate buffer solution. high-flow.00. Solution A (base): Dissolve 284 g of (NH4)2C2O4·2H2O in 10 L of DDI water. Certified Reference Solution. Safety Wear protective clothing and eye protection.5 Primary Al standard. 1-cm light path. CA. 30-mL 5.. 6. Beckman. Varian Australia Pty Ltd. 6.J.4. 6.3 Tubes.2 M. 16 mm x 100. N. Gas cylinders should be chained or bolted in an upright position.2 M ammonium oxalate solution and make to 1-L volume with RODI water. Lincoln. alumina or quartz injector. SAMPLETEX. Store in a polypropylene bottle. CT 5. Fisher Chemical Scientific Co.2 ID x 1.0. 1000 mg L-1. 15-mL. and Al) with 10 mL of primary Mn standard and 20 mL of primary P standard in 1 L volumetric flask.. with high-solids nebulizer. 7. 6. Fairlawn. 24 place. When preparing reagents.00.J. Fisher Chemical Scientific Co. Follow the manufacturer's safety precautions when using the UV spectrophotometer and ICP. dual-view. ASTM Type I grade of reagent water 6. Varian Australia Pty Ltd. VWR Scientific Products 5.5-mL. Fairlawn. Perkin-Elmer Corp.. Daigger Scientific 6. Fe. Resulting solution contains 60 mg L-1 each of Si. Certified Reference Solution.. N. Fe.14 Spectrophotometer.9 High mixed calibration standard. Adjust ammonium oxalate solution pH by adding either acid or base solution.6 OD x 6. with tips 10000 and 1000 µL 5.. 5. and tared extraction tubes 5. (1/8 ID x 1/16 OD x 1 in) for connecting syringe barrels 5.13 Vortexer. for sample dilution and sample changer. high-purity.1 Reverse osmosis deionized (RODI) water. 60-mL. Add 100 mL of 0. Norwalk.4 mm. Fe.7 Primary Mn standard. 10000 and 1000 µL. AS-93. Fullerton. and 9. Reagents 6.

purity 99.14 6. Add 100 mL of 0. Al. Turn off extractor. Fe. Make fresh weekly.2 Place labeled ET on extractor and connect to corresponding tared extraction tube (TETOxalate) with rubber tubing. and 3 mL primary P standard in 1 L volumetric flask.4 Secure reservoir tube (RT) to top of ET tube. Store in a refrigerator. air-dry or fine-grind soil the nearest mg and place in sample tube. Store in polyethylene bottle. Set extractor for 30-min extraction rate and extract until the ammonium oxalate buffer solution is at a 0. Resulting solution contains 10 mg L-1 each of Si. Medium mixed calibration standard. Mix 2 mL of Si primary standard in 1-L volumetric flask. Mix 10 mL of each primary standard (Si.9% 7. or stirring may be required to wet organic samples. The elements are added in the order (Si. 2 mg L-1 Mn. Make fresh weekly. and 10 mg L-1 P. Store in polyethylene bottle. Si. Make sure that the sample is thoroughly wetted. Invert to mix thoroughly.13 6. Resulting solution contains 5 mg L-1 Si. Store in a refrigerator.15 6. P) to avoid element precipitation.5 Add 35 mL of ammonium oxalate buffer to the RT. Mix 5 mL of Si primary standard in 1-L volumetric flask. Store in polyethylene bottle. 7. 5 mg L-1 Mn. Shaking. Add 100 mL of 0. Adjust the extraction rate for a 12-h extraction. Invert to mix thoroughly.6 Cover the extractor with a black plastic bag to exclude light. Fe. Cover samples with black plastic bag to exclude light. 314 . Mn. Low Si calibration standard.2 M ammonium oxalate solution and make to 1-L volume with RODI water. 7. 7. Procedure Extraction of Fe. Fe. Invert to mix thoroughly. Store in a polyethylene bottle. Fe.2 M ammonium oxalate solution and make to 1-L volume with RODI water. and Al. Store in a refrigerator. Store in a refrigerator. Add 100 mL of 0. Al. P) to avoid element precipitation.5 g of <2-mm. Resulting solution contains 2 mg L-1 Si. Make fresh weekly. wash sides of the tube and wet the sample. weigh enough soil to achieve ≈ 0.5 g.1 Weigh 0.9% Nitrogen. Mn. and 3 mg L-1 P. Store in a polyethylene bottle.5 to 1. Make fresh weekly. Low mixed calibration standard.11 6. Mix 30 mL of each primary standard (Si. Store in a refrigerator. Invert to mix thoroughly.10 6.2 M ammonium oxalate solution and make to 1-L volume with RODI water. Prepare two reagent blanks (no sample in tube) per set of 48 samples.0-cm height above sample. If sample is moist. and Al.16 Mn. Allow sample to stand for at least 30 min.2 M ammonium oxalate solution and make to 1-L volume with RODI water. Make fresh weekly. Add 100 mL of 0. Fe.2 M ammonium oxalate solution and make to 1-L volume with RODI water. Store in a refrigerator. and 20 mg L-1 P. Fe. The elements are added in the order (Si. Invert to mix thoroughly. During the addition. 7. Make fresh weekly. swirling.6.00 mL of ammonium oxalate buffer to the ET. Resulting solution contains 30 mg L-1 each of Si. Mn.3 Use a dispenser to add 15. and Al) with 5 mL of primary Mn standard and 10 mL of primary P standard in 1 L volumetric flask. and P 7. Store in a polyethylene bottle. purity 99. and Al) with 2 mL of primary Mn standard. Add 100 mL of 0. Calibration reagent blank solution.12 6. Argon gas. 7. Al. Very Low Si calibration standard.

and P. 7.00 L min-1 35 sec 315 .17 Refer to the manufacturer's manual for operation of the ICP-AES. Refer to manufacturer’s manual for operation of the spectrophotometer. Calibration reagent blanks and calibration standards are not diluted.12 On the spectrophotometer. If optical density is to be measured. ICP-AES Set-up and Operation 7.5 L min-1 0. Add 1 part ammonium oxalate sample extract with 9 parts dilution solution. Determination of Optical Density of Extract 7. Vortex. Si.7 mL of extract and 6.3 mL RODI water. 7. This solution is reserved for determinations of Fe. Leave the rubber tubing on the ET.0 Radial 2.85 L min-1 1450 Watts 15. Discard excess solution properly.10 Place 4 mL of ammonium oxalate extract in disposable cuvette.000 unit. Parameter Plasma Source Equilibration Delay Plasma Aerosol Type Nebulizer Start-up Conditions Plasma Auxiliary Nebulizer Power View Dist Plasma View Peristaltic Pump Sample Flow Rate Sample Flush Time Value 20 sec Wet Gradual 15 L min-1 0.15 Dilute ammonium oxalate extracts (1:10) with RODI water.7. 7. select a 430-nm wavelength. Dilution of Sample Extracts and Standards 7.14 Record optical density of ammonium oxalate extract to nearest 0. Pipet 0.8 Weigh each syringe containing ammonium oxalate extract to the nearest mg. Al.13 Use the ammonium oxalate extract reagent blank to zero spectrophotometer.7 After the extraction. 7. Select normal slit width and height.9 Mix extract in each TETOxalate by manually shaking. 7. 7. then store samples at 4°C. Fill a disposable tube with extract solution. Mn. If extracts are not to be determined immediately after collection. 7. shut off the extractor. fill a disposable cuvette with extract solution.11 Place 4 mL of ammonium oxalate reagent blank in disposable cuvette.16 Dispense the diluted solutions into test tubes that have been placed in the sample holder of the sample changer. Carefully remove TETOxalate. The following parameters are only very general guidelines for instrument conditions for the various analytes.

the instrument restandardizes.01 unit. The ICP calibrates the blank first.02 M ammonium oxalate extracting solution).61 213. low flow nebulizer requires a higher nebulizer pressure whereas a higher flow nebulizer requires a lower nebulizer pressure.18 Analyte data are reported at the following wavelengths. and P).e.Wash Parameters Wash Rate Wash Time Background Correction Read Delay Replicates Between samples 2. Al.0 mg L-1 yttrium. Al. and Si and mg kg-1 for Mn and P as follows: 8. aspirate with 1000. 7.00 mL min-1 30 sec 2 point (all elements) 2 sec 2 Nebulizer pressure depends on the type of nebulizer that is being used.61 257. Use these values to calculate the analyte concentration in percent in the soil for Fe. Fe. followed by a 1:10 (1 mL of 1:5 solution with 9 mL RODI water). Element Fe Al Si Mn P Wavelength ----------. If the QC is outside the range. low standard.20 Use a multipoint calibration for ICP-AES analysis of ammonium oxalate extracts. i. Si) The instrument readings are the analyte concentration (mg L-1 Fe. Calculations (Al. 7. This makes for a 1:50 dilution. If the QC falls within the range set by operator (±10%). Si (%) = [A x [(B1 – B2)/B3] x C1 x C2 x R x 100]/(E x 1000 x 1000) where: A = Sample extract reading (mg L-1) 316 . Al. ICP-AES Calibration and Analysis 7. 8. medium standard.. dilute 1:5 (1 mL of sample extract with 4 mL 0. Mn.19 Use the computer and printer to set instrument parameters and to collect and record instrument readings. Prepare a quality control (QC) standard with analyte concentration between the high and low calibration standards. To check for correct nebulizer pressure.94 308.nm --------259. Si.22 251. The QC is analyzed approximately every 12 samples. the instrument proceeds to analyze the unknowns.61 7. The ICP reads the QC after the high standard. followed by the high standard. The instrument readings are programmed in mg L-1. 7. Adjust pressure to correct yttrium bullet.1 Soil Fe.22 Record analyte readings to the nearest 0.21 If sample exceeds calibration standard.

11th Printing. 1. Washington DC. USDA-NRCS. Jackson. 1960. 317 . Govt. Madison.007 g mL-1) = Dilution. 1989. WI. In J. 41:1207-1208. Report Report the percent ammonium oxalate extractable Al. required = Dilution.L.L. Soil Sci. Jackson. 1977. R. J. Fe. Proc. Report the optical density of the ammonium oxalate extract to the nearest 0. required C2 = Dilution. 1999.2 M ammonium oxalate solution at 20° C (1. G. 1979.. Dixon and S. Jackson. if performed R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) 1000 = Conversion factor in numerator to kg-basis 1000 = Factor in denominator (mL L-1) E = Sample weight (g) 9. 1953. Holmgren. and Si to the nearest 0. Soc. 17:359-364. Iron oxide removal from soils and clays by a dithionite-citrate system buffered with sodium bicarbonate. Book Series No. and M. Iron oxide removal from soils and clays. A mechanically controlled variable rate leaching device. Am. Minerals in soil environment. Juve. 2nd ed.C. Published by author. Geschwender.01%.007 g mL-1) C1 = Dilution. Soil chemical analysis-advance course.. and R. A basic system of soil classification for making and interpreting soil surveys.2 M ammonium oxalate solution at 20° C (1.. Mehra.H.. 1051-1087. Office.P.B. Soil Sci.2 Soil Mn. 10.).L.S. O. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. M. 10. ASA and SSSA. References Aguilera. Madison. Weed (eds. Am. p. Soc. Soil taxonomy.B. Am.G. 2nd ed. if performed = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) = Sample weight (g) = Conversion factor to 100-g basis = Factor in denominator (mL L-1) = Factor in denominator (mg g-1) 8. Report the concentration of ammonium oxalate extractable Mn and P to the nearest mg kg-1 soil. N. Allophane and imogolite.L. Clays Clay Miner. and M.01 unit. Wada. K. P (mg kg-1) = [ A x [(B1 – B2)/B3] x C1 x C2 x R x 1000]/(E x 1000) where: A = Sample extract reading (mg L-1) B1 = Weight of syringe + extract (g) B2 = Tare weight of syringe (g) B3 = Density of 0. 7:317327.B1 B2 B3 C1 C2 R E 100 1000 1000 = Weight of syringe + extract (g) = Tare weight of syringe (g) = Density of 0. Print. Soil Sci. Soil Survey Staff. 2nd ed.

Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. imogolite. 436. These interferences vary in importance. Percent sodium pyrophosphate extractable Al. 1. depending upon the particular analyte selected. 1984). USDANRCS. The Na4P2O7 solution does not extract opal. USDA-NRCS Agric. crystalline silicates. Version No. There are several problems with this procedure. The analytes (Al.1 M Na4P2O7 and shaken overnight. 1983. especially the peptization and dispersion of microcrystalline iron oxide by pyrophosphate (Jeanroy and Guilet. Sodium 318 . layer silicates.. The AAS converts absorption to analyte concentration. 1999. The organic C in the sodium pyrophosphate extract is wet oxidized in a fume hood and gravimetrically measured in procedure 4G3b1a1. Sodium pyrophosphate extractable organic C. Application Sodium pyrophosphate (0. Selective Dissolutions (4G) Sodium Pyrophosphate Extraction (4G3) Atomic Absorption Spectrophotometry (4G3a) Aluminum. and crystalline hydrous oxides of Fe and Al (Wada. chemical. Washington. 1999) for more detailed information on the application of this ratio.S. The quantity of Fe extracted with pyrophosphate decreases with increasing centrifugation (McKeague and Schuppli. and Mn are reported in procedures 4G3a1-3. therefore uniform high-speed centrifugation or micropore filtration treatments are required (Schuppli et al. Handb. U. Fe. Interferences There are four types of interferences (matrix. 2nd ed. amorphous aluminosilicates. DC. 1981). Office. and Manganese (4G3a1-3) Air-Dry or Field-Moist. 1989). Washington. Print. Print. The Na4P2O7 solution is a poor extractant for allophane. The solution is then allowed to settle overnight before centrifuging and filtering to obtain a clear extract. Soil Survey Investigations Report No. Gravimetric (4G3b1a) Organic Carbon (4G3b1a1) Air-Dry or Field-Moist. Soil Survey Staff.Selective Dissolutions (4G) Ammonium Oxalate (4G2) Ratios and Estimates Related to Ammonium Oxalate Extraction (4G2b) Al + ½ Fe (4G2b1) The ratio using ammonium oxalate extractable Al plus 1⁄2 Fe determined in procedure 4G2a1a1-5 are used as taxonomic criterion for andic soil properties. 42. 1982). Iron. Mn) are measured by an atomic absorption spectrophotometer (AAS). 1975). 3. Loveland and Digby. and ionization) in the AA analyses of these elements. The data are automatically recorded by a computer and printer. <2 mm (4G3b1a1a-b1) 1. spectral. and Al were former criteria for spodic placement in soil taxonomy (Soil Survey Staff. Summary of Method The soil sample is mixed with 0.1 M Na4P2O7) is used as a selective dissolution extractant for organically complexed Fe and Al (Wada. Fe. 2. Govt. Govt. and noncrystalline hydrous oxides of Fe and Al. Soil survey laboratory information manual. 1995. Fe. Refer to Soil Survey Staff (1995. 1989). respectively. Office. <2 mm (4G3a1-3a-b1) Acid Digestion (4G3b) K2Cr2O7 + (H2SO4 + H3PO4 Digestion)(4G3b1) CO2 Evolution.S.0. U. References Soil Survey Staff. DC.

with syringes 10000 and 1000 µL.J. ±0. Acetylene is highly flammable. 6.5 Primary Al standard. double-beam optical system. To six 250-mL volumetrics. Certified Reference Solution.10 Test tubes. Fairlawn. drying. Follow the manufacturer's safety precautions when using the atomic absorption spectrophotometer (AAS). short neck 5. concentrated. Safety Wear protective clothing and eye protection.18 Flask. 6. N.2 Mechanical reciprocating shaker. Avoid open flames and sparks.. AAnalyst 300. Reno.20 Funnel.19 Condenser. 50-mL 5. Perkin-Elmer Corp... 1996).8 Digital diluter/dispenser.15 Filter paper. 50-mm diameter 5. Variable amounts of Fe. Fisher Chemical Scientific Co. Fisher Chemical Scientific Co. N.4 Autosampler. 12 N 6. 5. CT 5. 16 mm x 100. exercise special care. separatory. 40 mL 5. 1000 mg L-1.1 Electronic balance.2 Hydrochloric acid (HCl). N. round bottom. 250. 1000 mg L-1. Mn. Class A.4 Primary Fe standard.5 Peristaltic pump 5. Dissolve 446. AS-90.05 g of Na4P2O7·10H2O in 10 L of RODI water. Reagents 6. Follow standard laboratory procedures when handling compressed gases. Ann Arbor. GP-8. Al. Mn) to avoid element precipitation. Fe. 4.. with stopcock 5. 60° angle. Nesbitt with stopper 5. Eberbach 6000.7 Mixed Calibration Standards (MCS). 100.0 with either HCl or NaOH. Many metal salts are extremely toxic and may be fatal if ingested.J. Fisher Chemical Scientific Co.6 Single-stage regulators. 6. and organic C may be extracted by varying the pyrophosphate concentration. MicroLab 500.1 Reverse osmosis deionized (RODI) water 6. Certified Reference Solution. The concentration of Na4P2O7 solution must be close to 0.16 Absorption bulb.pyrophosphate extraction works best at pH 10 (Loeppert and Inskeep. Norwalk. 319 . Fairlawn. 15-mL. pH solution to 10.J. Restrict the use of concentrated HCl to a fume hood. Centra.11 Containers. Hamilton Co. Mn. 1000 mg L-1. 0. for sample dilution and sample changer 5.17 Absorption bulb. polypropylene 5.21 Tube.1 M. Schwartz 6.14 Funnel.13 Centrifuge tubes. Eberbach Corp. MI 5..12 Volumetrics. Al. Perkin-Elmer Corp. Allihn 5. long stem. open top. and 1000-mL 5. Fairlawn. 150 mm 5. add the following amounts of Primary Standards (1000 mg L-1) as follows. The elements are added in the order (Fe. Needham Heights. cylindrical. NV 5. Certified Reference Solution. Standard laboratory equipment includes fire blankets and extinguishers for use when necessary.1 M. Equipment 5.6 Primary Mn standard. Norwalk. Whatman 42.1-mg sensitivity 5.9 Dispenser.. When preparing reagents. Thoroughly wash hands after handling these metal salts. 6. acetylene and nitrous oxide 5. Al. CT 5..3 Atomic absorption spectrophotometer (AAS). boiling.7 Centrifuge. gas tight. Stetser-Norton 5.3 Sodium pyrophosphate solution. Thermo IEC. 1 1⁄2 in strokes. Gas cylinders should be chained or bolted in an upright position. MA 5. 200 oscillations min-1.

6. 0. respectively. and 5 mg L-1 Fe.14 6.00. 7.5 Remove tubes from shaker and manually shake tubes to dislodge any soil from cap. purity 99.50. 20. and Mn 7. 7. respectively.1 Weigh 0. and 15 mg L-1 Fe. Potassium iodide solution. and 10 mg L-1 Fe.625 mL Fe. Al. If sample is moist.16 6. Add 50 mL of 0.1 M Na4P2O7 to each MCS and make to volume with RODI water.8 6.5 g of air-dry soil.7.1 M Na4P2O7.7. air-dry soil to the nearest mg sample and place in a 50mL centrifuge tube. and Mn. 100. 6. 7. 10.50 mL Fe.4 20. pH 10.00. Al.0 solution to centrifuge tube. 6.6% Nitrous oxide gas. 40. Al.25. and 1. 2. Filter if necessary.9 6.00.2 Add 30-mL of 0. Al. and Al are determined from a clear aliquot of solution. Al.75 mL Fe. Dissolve 100 g of KI in 100 mL of RODI water. The Fe. Al. and 2.3 6. Al. compressed Compressed air with water and oil traps 7. saturate aqueous solution Digestion acid mixture: Mix 600 mL of concentrated H2SO4 and 400 mL of 85% H3PO4 Indicarb or Mikohibite Soda lime Zinc granules. and Mn = 0. 7. 6.5 g <2-mm or fine-grind.375 mL Fe.7.00.00. and 5 mg L-1 Fe.2 6. and Mn = 0.6 0. respectively. respectively. 0. and Mn = 5. 320 .5 1. and Mn = 6.10 6. 5.50 mg L-1 Fe.17 6.02 M Na4P2O7.5 mg L-1 Fe.25 mL Fe. and Mn. Allow samples to sit overnight. and 0. Al.15 6. 20.6. and 3. and 2. 7. 5. 25. 40. and Mn. and 0. weigh enough soil to achieve ≈ 0. Silver sulfate. Final concentration of MCS is 0.6 Next day centrifuge sample at 4000 rpm for 15 min. and 1. Quality control (QC) is the MCS with 10.13 6.7. and Mn = 2. and Mn. and Mn = 1. and Mn.11 6. and 0 mg L-1 Fe.0. Fe. 10. respectively.3 Cap tube and shake briefly by hand to dislodge soil from tube bottom. Mn.25. and Mn. 0. 10.1 25.25.18 Potassium dichromate (K2Cr2O7) reagent. respectively. Al. 300 mesh Anhydrone Acetylene gas.50.4 Place rack in shaker and shake overnight (12 to 16 h) at 200 oscillations min-1 at room temperature (20°C ± 2°C).0. Al. Procedure Extraction of Al. 80. Al. Place tube in rack.12 6. Al.7. Al. respectively. and Mn.7.0 mL Fe.

0 C2H2/15.0 309.2 3.12 Each element is analyzed during separate runs on the AAS.3 5-cm parallel 0.16 Pipet 100 mL of the extract into a 100-ml flask.18 Construct the wet combustion apparatus.0 C2H2/15. The QC is also read at the end of each run.17 Evaporate the extract to near dryness using a 50°C water bath and a gentle stream of clean. Wavelength Burner Head Slit Fuel/Oxidant (mg L-1) (nm) (mm) ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ Fe 25. Refer to Fig. filtered air.14 If samples are outside the calibration range.02 M Na4P2O7.0 279. Calibrations are linear with calculated intercept.11 If sample exceeds calibration standard.8 Dispense the MCS and diluted sample solutions into test tubes that have been placed in the sample holder of the sample changer. Organic C Determination 7. 7. 1 for the apparatus for gravimetric organic C determination. Samples have a final concentration of 0.15 Record analyte readings to 0.1 M Na4P2O7 and then 1:5 with RODI water.10 Use the computer and printer to set instrument parameters and to collect and record instrument readings.7 7.0 248. 7. 7. If it fails.8 10-cm parallel 0. Dilute samples 1:5 with RODI water. 7.2 3.9 The following are only very general guidelines for instrument conditions for the various analytes.7 Air Al 100. 7. AAS Calibration 7. 7. Use the calibration reagent blank and calibration standards to calibrate the AAS. Conc.13 Use the QC after every 12th sample. 7.20 Wash the neck of the flask with 3 mL of RODI H2O and connect to condenser.0 C2H2/3. 7.5 N2O Typical read delay is 3 s and integration time is 3 s but can vary depending on soil type. 7.Dilution of Sample Extracts and Standards 7.7 No ionization suppressant is required as the Na in the extractant is present in sufficient quantity. dilute the sample 1:10 with 0. recalibrate and reread the QC.01 unit. dilute 7.19 Add 1 to 2 g of potassium dichromate.3 10-cm parallel 0.2 Air Mn 15. 321 Analyte . AAS Set-up and Operation 7. Three replicates are averaged for each sample. It must pass within 15% to continue.

disconnect the bulb from the system. 7. if performed 322 .25 Remove the heat and allow to aerate for 10 additional min at a rate of 6 to 8 bubbles s-1. Continue a gentle boiling for 10 min.7. Adjust the flow of the "carrier stream" to maintain 1 to 2 bubble s-1 rate throughout the digestion.5 cm below the digestion-acid mixture. Use the digestion-acid mixture to lubricate the stopcock. 7. 7. Mn (%) = (A x B x C1 x C2 x R x 100)/(E x 1000 x 1000) where: A = Analyte concentration reading (mg L-1) B = Extract volume (L) C1 = Dilution. Add the mixture to the flask and immediately close the stopcock. 7.23 The tip of the air-delivery tube should be ≈ 0.21 Attach a weighed Nesbitt bulb to the system and open the valve at the top.26 Close the stopcock on the Nesbitt bulb. gently heat the flask until the mixture boils (≈ 3 to 4 min). 8.1 Soil Fe. Al.24 With a gas flame or a variable power-heating mantle. Apply suction on the outlet side of the Nesbitt bulb. Gentle air pressure and needle valve on the air-pressure line aids flow-adjustment.22 Pour 25 mL of digestion-acid mixture into the funnel.0001g. required C2 = Dilution. Calculations 8. and weigh to the nearest 0. Heating is too rapid if white fumes of SO2 are visible above the second bulb of the reflux condenser. 7.

Madison. Soil Survey Staff. P.) Methods of Soil Analysis.A.WtI) x 27. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. R. Am. 1996..P. Changes in concentration of iron and aluminum in pyrophosphate extracts of soil and composition of sediment resulting from ultracentrifugation in relation to spodic horizon criteria.). and B. and W. J. Report Report sodium pyrophosphate extractable Fe. p..2 Organic C (%) = [(WtF . 1981.A. Soil Sci. U. Book Series No. 134:265-270. Soc. 35:243-250. 47:1026-1032. 1983. Weed (eds. G. In J. The effective removal of suspended materials from pyrophosphate extracts of soils from tropical and temperate regions.. and Al to the nearest 0. J. DC. K. Loeppert. 1982. Soil Sci. In D. Office. Handb.6 = Nesbitt bulb weight after digestion (g) = Nesbitt bulb weight before digestion (g) = Extract volume digested (mL) = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) = Conversion factor = Total extract volume (mL) 9. Inskeep. The extraction of Fe and Al by 0. 1989. Minerals in soil environment. Book Series No. H. E. and J. References Jeanroy.B. ASA and SSSA.3 236.6) where: WtF WtI Volume R 27.. Soil Sci. Schuppli.B. P. 1. Soil Sci. Iron. 1051-1087. and P. Am. Mn. Ross.A.J. Allophane and imogolite.J. The occurrence of suspended ferruginous particles in pyrophosphate extracts of some soil horizons. p. Soil Sci. Print. 436. 2nd ed.R = Air-dry/oven-dry ratio (procedure 3D1) or field-moist/oven-dry ratio (procedure 3D2) E = Sample weight (g) 100 = Conversion factor to 100-g basis 1000 = Factor in denominator (mg g-1) 1000 = Factor in denominator (mL L-1) 8. P. Madison.3 x Volume x R]/(Sample Weight (g) x 236. Schuppli. 5. WI. 11. 639-664. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.1 of a percent.A. WI. 1984. 10. Loveland. USDA-SCS Agric.. 1975. 323 .A.S. Dixon and S. Part 3 – Chemical methods. Am. McKeague.1M pyrophosphate solutions: A comparison of some techniques. Washington. ASA and SSSA. Guillet. Digby. Geoderma 26:95-105. McKeague. and P. J. Sparks (ed.L. Govt. Wada.

mining. The volumetrics are allowed to stand overnight.g. Nickel. Manganese. and Zinc (4H1a1a1a1-20) Air-Dry. W. 1992). Summary of Method The approach of this digestion methodology is to maximize the extractable concentration of elements in digested soils while minimizing the matrix interferences such as found in digestion procedures that use HF acid. Knowledge of these levels is important in understanding the consequences of increasing levels of trace elements in ecosystems (Tiller.. feldspars) are not soluble in HNO3 + HCl. Cobalt. Arsenic. pesticides. Phosphorus. Tl.. Antimony. This method (4H1a1) follows EPA Method 3051A. Thallium. 1998).. and Zn are determined using an inductively coupled plasma atomic emission spectrophotometer (ICP-AES) in axial mode by procedures 4H1a1a1a1-20. 1994. Vanadium. respectively. Sn. 324 . 3. Mercury is analyzed by a cold-vapor atomic absorption spectrophotometer (CVASS) (4H1a1c1).Total Analysis (4H) Acid Digestion (4H1) HNO3 + HCl Digestion (4H1a) Microwave (4H1a1) Inductively Coupled Plasma Atomic Emission Spectrophotometer (4H1a1a) Axial Mode (4H1a1a1) Ultrasonic Nebulizer (4H1a1a1a) Silver. manufacturing).0 mL HNO3 and 3. 1993. 1989. P. and samples transferred into appropriate acid-washed polypropylene containers for analysis. organic concentrations. Sb. Sr. Knowledge of the elemental amounts and distribution in soils and their relationships with other soil properties can enhance the understanding of the fate and transport of anthropogenic elements. The concentration of Ag. Beryllium. Cr. filled to volume. thereby expanding the utility and application of soil survey knowledge in areas of environmental concern such as urban. A 500-mg <2-mm soil separate which has been air-dried and ground to < 200 mesh (75 µm) is weighed into a 100-ml Teflon (PFA) sample digestion vessel. Holmgren et al. respectively. Molybdenum. 1997) to human-induced distributions (Wilcke et al.g. mine spoil reclamation. 2003). Strontium. These elements may become elevated in concentration due to natural (e. V. Mo. quartz. 1994. Uses of elemental data in soil survey applications are broad and diverse. Application The term of trace elements is widely applied to a variety of elements that are generally present in plants. Jersak et al. Co. <2 mm (4H1a1a1a1-20a1) 1.g. Cd. and placed into a rotor with temperature control. To the vessel. Ni. 2. smelting. Tin. Certain soil minerals (e. Cu. and digestate quantitatively transferred into a 50-ml glass volumetric high purity reverse osmosis deionized water. 2002).. Mn. and water in low concentrations or what is termed background levels. Pb. Lead.. Copper. ranging from understanding natural (Wilcke and Amelung. and As and Se are determined by flow through hydride-generation and atomic absorption spectrophotometer (HGAAS) (4H1a1b1a1-2). and agricultural waste applications (Burt et al. Gambrell. Interferences Organic constituents may contain metals and are difficult to digest if present in high concentrations. smelter emissions.. Tungsten. Burt et al. Certain elements are subject to volatile losses during digestion and transfer.0 mL HCl are added. Keller and Vedy. Ba. and oxides (Pierzynski and Schwab. 1996. As. Be. translocation through the soil or landscape) or through human-induced activities (e.. Cadmium. The vessel is inserted into a protection shield and covered. the rotor and samples are cooled. mineral weathering. magmatic activity. soils. The relative reactivity or bioavailability of these elements in soils is governed by a variety of chemical factors such as pH. Barium. Following microwave digestion. redox potential. Chromium.. 9.

Neslab.2 Pipet(s) capable of delivering 3 and 9 mL.1.1 mg sensitivity) 5. Part No.7 Primary standards: 1000 mg L-1.1 Reverse osmosis deionized (RODI) water. 50 mL 5.. Perkin-Elmer Optima 3300 Dual View (DV). class A glass..0 mm id). Rainin Instrument Co..10 Inductively coupled plasma atomic emission spectrophotometer (ICP-AES).14 Compressed gasses. (±0. Omnifit Corp. CT.16 Quartz torch.8 Containers.5 Concentrated hydrochloric acid (HCl). 250. Norwalk. Equipment 5. HNO3 + HF. AS-90.4 Reverse osmosis deionized (RODI) water. ±1. 5. with cap 5. Norwalk. Perkin-Elmer Corp.0-mg sensitivity 5. 5... Omaha. 5. 14 position-HP500 Plus vessel and rotor (vessels composed of PFA. floor mounted power unit. Charleston. 45 MHz free running.3 Volumetric flasks. Single elemental standards are manufactured in dilute HNO3. CT. 4. Woburn. Perkin-Elmer Corp. argon (minimum purity = 99. Wash hands thoroughly after handling reagents.. alumina injector (2. Part No. 60 mL. CETAC Corp. 16 N. sleeves composed of advanced composite) 5. or H2O 325 . with WinLab software ver.15 Autosampler. 4. SC. Also. trace pure grade 6.11 RF generator. trace pure grade 6.Spectral and matrix interferences exist.5 Electronic balance.3 Concentrated nitric acid (HNO3). 250 µL and 10 mL. NE 5. 12 N. Reagents 6.9 Pipettes. 500-mL. Samples and standards are matrix-matched to help reduce interferences. CT.999%) 5. Model U-5000AT+ . electronic digital. Norwalk.12 Computer. Perkin-Elmer Corp.1 Electronic balance.4 Polypropylene bottles. 16 N. Filling the digestion vessel to greater than 25 percent of the free volume or adding organic reagents or oxidizing agents to the cup may result in explosion of the digestion microwave system.18 Peristaltic pump (for automatic injection of internal standard) 6. trace pure grade 6. Norwalk. careful selection of specific wavelengths for data reporting is important.6 Concentrated nitric acid (HNO3).5 L bottles 5.6 Microwave oven. 12 N. 500. manufacturers variable volume. trace pure grade 6.996%) and nitrogen (minimum purity = 99. Restrict the use of concentrated acids to the fume hood. Safety Wear protective clothing and eye protection.7 Volumetrics. Interferences are corrected or minimized by using both an internal standard and inter-elemental correction factors. polypropylene.17 Ultrasonic nebulizer. from High Purity Standards. and 50-mL class A glass 5. N069-1662. CT 5. CFT Series 5. exercise special care. When preparing reagents. (10-ml maximum) pipettes suitable for HNO3 and HCl delivery from 2.13 Recirculating chiller. Background corrections are made by ICP software.2 Concentrated hydrochloric acid (HCl). ASTM Type I grade of reagent water 6. Perkin-Elmer Corp. with screw caps 5. N069-5362 5. MA 5. and printer 5. ASTM Type I grade of reagent water 6. CEM Mars 5.

and blank by the same digestion method.13 A primary mixed calibration standard (PMCS) is prepared from the respective primary elemental standards (1000 mg L-1) to a 500-mL final volume.0 mL HNO3 and 3. Procedure Microwave Acid Digestion 7. perform a preliminary digestion in the muffle furnace in an digestion crucible: 250°C for 15 min. Run two of these standards or blank with each set of 14 samples. 7. reference soil sample from the SSL repository. Connect the pressure monitor to the vessel. cover and place into rotor.6 Microwave settings are as follows: 1200 watts at 100% power for 5.3 Pipet 9. 7.2 Note: If sample is principally composed of organic materials (organic C > 15%).7 After cooling. 7. Allow acids to react and vent in uncovered vessels for about 30 min.9 Open each vessel carefully and then quantitatively transfer contents of vessel to a 50-mL volumetric flask with RODI water. Allow to stand overnight.8 Remove rotor from oven. 7. 7. prior to diluting to volume. three working calibration standards (WCS) are prepared. Add acids in the fume hood.1 mg in a 100-mL digestion vessel. Attach the probe cable into the fitting in the top of the microwave. NIST or other standard reference material. From this PMCS.12 Prepare working standards of a blank. disconnect temperature probe and pressure sensor from microwave. 7.5 Place digestion rotor in the microwave oven and insert the temperature probe into the reference vessel.5 min until 175°C Hold at 175°C for 4.1 About 500 mg of fine-earth (<2-mm) or a specific particle size separate ground to <200mesh (75 µm) is weighed to the nearest 0.7.10 Cap flask and mix well by inverting. Also. ICP-AES Calibration Standards. 7. 7. a single element standard for Tl (STl1) is prepared separately from a 1000 µg L-1 stock standard to a 50-mL final volume. 450°C for 15 min.5 min Cool for 5 min 7. followed by 550°C for 1 h.11 Decant contents into a labeled 60-mL polypropylene container. add 90 mL HNO3 and 30 mL HCl to the PMCS and 9 mL HNO3 and 3 326 . and Operation 7. and place in fume hood. 7. In addition. 7. Finish filling to volume with RODI water.0 mL HCl into the sample and allow to completely wet. Set-Up.4 Place covered vessels in protective sleeve.

The amount of the primary standards (1000 mg L-1) to make the PMCS.63.25 mL HCl to the WCS (Low. respectively. and 62.89.5.000 2 Co 4. Invert to mix thoroughly. prior to diluting to volume.2 Ba 120.1 mL HNO3 and 2.2 V 20.14 The WCS are made from dilution of the PMCS with the exception of single element Tl (STl2). Use RODI water to dilute to final volume for WCS and STl2. add 44. Invert to mix thoroughly. 43. Medium.7 mL HCl for the Low and Medium ST12. The elemental concentrations of the Low. 14. amount of the1000 µg L-1 Tl stock standard to make the STl1 and the final elemental concentrations of the PMCS and STl1 are as follows: ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ Element Concentration Primary Standard Required ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ -µg L-1---.91 and 8.000 20 Cu 20. and 50 mL of the STl1 diluted to a 50-mL final volume. Also. Medium.3 Sb 400 0. Make fresh on a routine basis.000 1 ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ 7. and 11.625.25. add 8.88.97 and 2.000 2 Ag 400 0. 6. Store in polyethylene container in a refrigerator. The three WCS (Low.mL HCl to the STl1. High. and 33.000 10 Cd 2.2 Sr 60. respectively. prior to diluting to volume.000 30 Cr 4.96. which is made up separately. Medium.000 1 Pb 4.000 30 Mo 400 0. Use RODI water to dilute to final volume for PMCS and STl1.000 1 Ni 4.mL ---As 2.000 10 Zn 20.75 mL HNO3 and 14. The STl2 requires 0. 5. Store in polyethylene container in refrigerator.000 2 P 60. Make fresh on a routine basis. and High) require 0.000 10 Sn 8.000 60 Be 600 0. Also. and High WCS and the ST12 are as follows: 327 .5 ml PMCS diluted to 250-mL final volume.000 4 Tl 500 25 W 2.000 2 Mn 40. respectively).

V. respectively. add 45 and 15 mL HNO3 and HCl. 328 . Make fresh on routine basis.000 Mo 1 10 100 V 50 500 5000 Sn 20 200 2000 Tl 5 50 500 W 5 50 500 As 5 50 500 ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ 7.25 2.µg L-1 -------------------Ni 10 100 1000 P 150 1500 15000 Cr 10 100 1000 Mn 100 1000 10000 Cu 50 500 5000 Zn 50 500 5000 Cd 5 50 500 Pb 10 100 1000 Co 10 100 1000 Ag 1 10 100 Ba 300 300 3000 Be 1.0 10 100 Sr 150 1500 15. Use RODI water to dilute to final volume for MIECS and SEIECS.00 25.⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ ---------------.Concentration -------------Element Low Medium High ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ ------------------. Mo. add 9 and 3 mL HNO3 and HCl. Fe.0 5. These are prepared in the matrix of the digests and are combined into one solution for routine calibration. To SEIECS.00 1. Store in polyethylene container in a refrigerator.5 15 150 Sb 1. The SEIECS is based on a 50-mL final volume and the MIECS is based a 250-mL final volume. respectively. Mn) are required to create the inter-elemental correction (IEC) factors. The mixed IEC standard (MIECS) is required for routine calibration.16 To MIECS.50 5. The single element IEC standards (SEIECS) are required to determine the IEC’s.25 0. Invert to mix thoroughly. Al.50 0.50 Al Fe Mo V Mn 7.50 2.15 Single element primary standards (1000 mg L-1. Use RODI water to dilute to final volume for SEIECS and MIECS.0 0. The amount of the primary standard (1000 mg L-1) to make the SEIECS and MIECS solutions and the final elemental concentration of these IEC solutions are as follows: Element IEC Solution --------Primary Standard-------Concentration --------------Required -----------MIECS SEIECS --mg L-1-------------------mL--------------100 100 5 10 10 25.

979 328.221. 224.710.844 178.604.402 260. all calibration standards.20 Analyses are generally performed at two or more wavelengths for each element.733.568 329 . 7.312 308. IEC factors are established via a procedure in the WinLab software in which the amount of interference on the analyte (in µg L-1) is measured for each mg L-1 of interferent concentration in the digest.912. 7.203 260. 407. Check instrument alignment and gas pressures to obtain optimum readings with maximum signal to noise ratio. 206.787 291. 203.44 mm id.230 189.003. The SEIECS should initially be prepared in separate 50-mL volumetrics for establishment of IEC factors and then prepared (MIECS) in a single 250-mL volumetric for routine analysis.nm --------237.197 228. 231.402.582.353.620 267.0 mL Lu primary standard (1000 mg L-1) and 10 ml conc.570 203.287 202.312 302. 7. 216.7. BEC and %RSD of 1 mg L-1 Mn solution) prior to analysis as discussed in operation manual of instrument.857. 235. 213. 226.525. 455.485 207.801. 327.19 Use the ICP-AES in axial mode and ultrasonic nebulization to analyze sample.558 324.215 302. HNO3 to 500-mL volumetric flask. Internal standard and samples or standards are mixed via a mixing block and coil prior to entering the ultrasonic nebulizer. 206.107 202.104. 338.507 313. The selected wavelengths are as follows: (reported wavelength listed first and in boldface): Element Al Fe Mn P Cr Cu Ni Zn Cd Pb Co Sb Sr Ba Be As Ag Mo V Sn W Tl Lu Al (IEC) Fe (IEC) Mo (IEC) V (IEC) Mn (IEC) Wavelength ----------. 313.802. 276.031. 205. and diluting to volume with RODI water.068. It is prepared by adding 5. No initial dilutions of samples are necessary prior to analysis.614 217.18 A 10 mg L-1 Lu internal standard (read at 291.771 233. and samples.138 nm) is added to the blank.107 238.Perform instrument checks (Hg alignment. 310.845 292.031 292.927.046 188.753. 213.396 232. pump tubing.876 190.Internal standard is automatically injected via the peristaltic pump and mixing block. Internal standard is added via an external peristaltic pump at 15% pump speed using 0.501 220.138 (Internal Standard) 237.17 The elements chosen for IEC factors are based on established spectral interferences with chosen analyte wavelengths.833 460.998 228.

J. Heavy metals in soils and their environmental significance. 23:987-999. and J. Keck. Strom.M. Environ. Adv.. and nickel in agricultural soils of the United States of America. J. Mays. Montana. R. 9:113-142. 26:551-521. Qual.21 Use the blank standard solution to dilute those samples with concentrations greater than the high standard. In B. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. Pierzynski. R. Lee. 1994. 7. G. 10. Environ. 60:1490-1495. Tiller.P.C. cadmium. The particle-size fraction digested needs to be identified with each sample. 1993. Am. copper. Qual. R. Gambrell. Qual. Report Analyses are generally performed at two or more wavelengths for each element. Jersak. 23:883-891.E.A. Trace and toxic metals in wetlands–A review. References Burt. R.22 Establish detection limits using the blank standard solution. Schwab.B. 2002. Bioavailability of zinc.D. lead. Wilson. Soc.W.23 The extract obtained in this procedure (4H1a1) is used in procedure 4H1a1c1 for Hg analysis and in procedures 4H1a1b1a1-2 for As and Se analysis. zinc. 22:247-254.A. respectively. The instrumental detection limits are calculated by using 3 times the standard deviation of 10 readings of the blank. USA. Daniels. M. 1996..L. 32:2109-2121.D. Rerun all elements and use only the data needed from the diluted analysis.. if performed R = Air-dry/oven-dry ratio (procedure 3D1) 1000 = Conversion factor in numerator to kg-basis E = Sample weight (g) 1000 = Factor in denominator (µg mg-1) 9.G.. 1989. Res. 10. Qual.) Adv. 8.. K. 2003. Environ. These values establish the lower detection limits for each element. and C. C. Distribution of copper and cadmium fractions in two forest soils. Dougherty.G. Trace element speciation in selected smelter-contaminated soils in Anaconda and Deer Lodge Valley. M. Soil Sci. Analyzed values lower than the detection limits are reported as "ND" or non-detected. R. Keller.S. and J. and lead in a metal-contaminated alluvial soil. Environ.W. G. J. 1993. 1994. Stewart (ed.01 mg kg-1. Brimhall. and A. Small-scale heterogeneity of aluminum and heavy metals in aggregates along a climatic transect. Jr. Data are reported to the nearest 0. Wilson. Lindhal. with the one selected wavelength for reporting purposes. 22:335-348. 7. Proc.7. Wilcke. Chaney. Meyer.. M. and W. Major and trace elements of selected pedons in the USA. J.A. 8:51-67. Vedy. 330 . D. B. Environ. Calculations The calculation of mg kg-1 of an element in the soil from µg L-1 in solution is as follows: Analyte concentration in soil (mg kg-1) = [A x B x C x R x 1000]/E x 1000 A = Sample extract reading (µg L-1) B = Extract volume (L) C = Dilution. Burt. and G. and R. Qual. Holmgren. W. J. Qual. M. J. Environ. Trace metal geochemistry in Spodosols of the Northeastern United States. Amelung.A. 1997. P. Soil Sci. T. Cadmium. J.J.. Environ. Amundson.

. Concerns exist for both short-term (acute) and long-term (chronic) soil exposure. The bioavailability and toxicity is related to speciation. with a final concentration of 1% in analysis solutions. i. Data from As measurements in groundwater by U. soaps. 1998. sodium borohydride (NaBH4) reduces As and Se to form gaseous products that can be detected by atomic adsorption. but has been widely applied to soils as a component in pesticides and herbicides and also via industrial pollution and smelting operations. is in the form of the oxyanion. such as Mancos Shale in Colorado and Wyoming and in the shales of the Moreno and Kreyenhagen Formations of California (Martens and Suarez. Zech. the extract is combined with 14 mL of water and 20 mL of concentrated HCl and boiled for 30 min. Potassium iodide is added as a pre-reduction step for As analysis... It is typically found in low concentrations. Under acidic conditions. 2. elemental Se (Se0). 2001). The element occurs as arsenate (As5+) and arsenite (As3+). AsO43-. Geological Survey and Environmental Protection Agency has suggested that most As in groundwater is related to natural sources (Ryker. N. Application Arsenic is an extremely toxic element that is occurs in both organic and inorganic forms in soils. The element is used in drugs. Soil applied As is generally immobile. <2 mm (4H1a1b1a1-2a1) 1. The element is important due to both deficiency (forages for animals) and toxicity (bioaccumulation) concerns (Huang and Fujii. S. A 6-mL aliquot of the digestate is combined with 6 mL concentrated H2SO4 and heated at 180 C for 5 min in the microwave oven to eliminate the HNO3.S. Sample extracts are allowed to cool. The weathering of limestone and biological accumulation of the element by aquatic organisms is responsible for the high levels in wetland soils of Florida (Chen et.S. though 90% of industrial As in the U. 1996). and selenide (Se2-). For example.Wilcke. Solutions are allowed to stand 1 h before analyzed for total As and/or Se. 1997). Urban soil contamination in Bangkok: Heavy metal and aluminum partitioning in topsoils. Kanchanakool. Following extraction. Summary of Method A soil sample is digested with HNO3 and HCl in a microwave oven (procedure 4H1a1). For example: 3NaBH4 + 4H2SeO3 4H2Se(g) + 3H3BO4 + 3NaOH 331 . Selenium occurs in four species (related to valance states): selenate (Se6+). and metals. Geoderma 86:211228. from mineral dissolution from minerals in geologic formations and soils. using flow through hydride-generation and atomic absorption spectrophotometer (HGAAS). Then. 2002) Selenium is a naturally occurring element in rocks. Muller. Primary route for exposure is via soil ingestion or inhalation of air-borne particles. but is especially concentrated in certain geologic formations. Total Analysis (4H) Acid Digestion (4H1) HNO3 + HCl Digestion (4H1a) Microwave (4H1a1) HCl Digestion (4H1a1b) Water Bath (4H1a1b1) Flow Through Hydride-Generation and Atomic Absorption Spectrophotometer (4H1a1b1) Arsenic and Selenium (4H1a1b1a1-2) Air-Dry. dyes. selenite (Se4+). and in soils. with soil chemistry similar to phosphorus. W. As released via pyrite oxidation is in part responsible for groundwater As levels in Bangladesh ranging between 50 and 2. al. 2001). and W. The oxidized species are more commonly found in soils and water. is used in wood preservatives (Pinsker. samples are diluted with water to a final 50-mL volume.e.500 ug/L in many wells.

CT 5. CT 5. Dell Computer Corp. or safety glasses). Allentown. In general. 16 mm x 100. argon service 5. Reagents 6..g. and 1000-mL volumetrics.. CT 5. Gas cylinders should be chained or bolted in an upright position. ±0. Ni.1. Cu. Pb.. acetylene service. respectively.14 100.1-mg sensitivity 5. nitric) can produce interferences.3% w/v. affecting the signal. Interferences Oxidizing acids (e. erratic absorbance signals and low recoveries. the quantity of nitric acid can be sufficiently reduced to eliminate the need for urea. Follow standard laboratory practices when handling compressed gases.4 Autosampler. 95°C-capability 6. 25-mL. and gloves). Co) can affect determinations. The As and Se concentrations are reported as mg kg-1 in the soil by procedure 4H1a1b1a1-2. Dell Optiplex GXM 333 MHz Pentium. more so for As than Se. Perkin-Elmer Corp.2 Sulfuric acid (H2SO4). Alternatively. Avoid open flames and sparks. 4. Sn.. Fe.3 System 2 Electrodeless Discharge Lamp (EDL) Power Supply. 36 M. Acetylene gas is highly flammable. This interference can be effectively eliminated with either (1) addition of urea before the potassium iodide pre-reduction step. and inter-element interferences (e. Even small amounts of nitric acid produce suppressed. Perkin-Elmer Corp. Model VGA-77 5.6 Computer. if samples are boiled in HCl.15 Containers. Air Products and Chemicals. Equipment 5. CT 5. Corning Pyrex. Inter-element inteferences can be reduced by using the lowest possible concentration of sodium borohydride.12 Test tubes. 17 in color monitor 5. and a breathing filter when handling As and Se solutions. 50-mL.The data are automatically recorded by a computer and printer. PA 5.1 Electronic balance. Cr. Safety Wear protective clothing (coats.. trace metal purity 6.1 Reverse osmosis deionized (RODI) water. Hydride-forming elements may exist in more than one oxidation-state. Norwalk. for sample dilution and autosampler 5. 4. 3.8 Single-stage regulator. class A. 5. Norwalk.. These elements are extremely toxic. Box 538.3 Sodium hydroxide (NaOH⋅3H20) 332 . PE Model Analyst 300. polypropylene and glass 5. Follow the manufacturer's safety precautions when using the AA.g.9 Double-stage regulator. goggles. 50-mL for calibration standards 5. aprons. Best results can be obtained for difficult samples containing high concentrations of metals if the sodium borohydride concentration is reduced to 0. for sample digestion 5. Ver.7 Printer. with lamps for As and Se. eye protection (face shields. Perkin-Elmer Corp.. Norwalk.5 WinLab Software.11 Tubes. Norwalk. Perkin-Elmer Corp.2 Atomic absorption spectrophotometer (AAS). or (2) boiling the samples with H2SO4. There are typically more inter-element interferences for As5+ methods than for As3+. Standard laboratory equipment includes fire blankets and extinguishers for use when necessary. 5. 250. As5+ methods produce a signal that may be 20 to 50% of that produced by As3+.10 Varian Vapor Generation Accessory.13 Test tubes. Hewlett-Packard LaserJet 880A 5.16 Water bath. Inc. sleeve guards. part number E11-0-N511A.. ASTM Type I grade of reagent water 6. Model 90A.

maximum of 3 beakers. 12 M.4 Sodium borohydride (NaBH4) pellets 6. Final concentration of MCS and QC check is ≈ 6 M HCl. Quality Control (QC) check is MCS 100 µg L-1. Dissolve 50 g of KI and 50 g of ascorbic acid and dilute to volume with RODI water. mix until dissolved. 1000 mg L-1As and 1000 mg L-1 Se.5 Hydrochloric acid (HCl). Invert to mix thoroughly. 25. soil standards. Fill to volume with RODI water. Make fresh daily. Add 2. Standard Reference Material). Store in polyethylene container in a refrigerator. add PMWS and concentrated HCl as follows: 6.11.6 Acetylene gas.5 mL PMWS + 106 mL HCl 100 µg L-1 = 25.13 Acid Carrier.0 mL PMWS + 113 mL HCl 75 µg L-1 = 18.11. Heating program for microwave is as follows: 333 .11. Make fresh daily.6. assay 35-38% 6.1 6. Inc. purchased from High purity Standards) and NIST SRM 2710 (National Institute of Standards and Technology.16 Diluent. and spikes prepared in procedure 4H1a1 as follows: Pipette 6mL of acid (HNO3 + HCl) extract and 6mL concentrated H2SO4 into a 50-mL Pyrex tube. Invert to mix thoroughly.11.0 mL PMWS + 124 mL HCl 0 µg L-1 = 0 mL PMWS + 125 mL HCl 6.10 Primary mixed working standard (PMWS). add 250 mL of RODI water.14 Reductant. Standards will keep for 2 to 3 days with refrigeration.11.5% NaOH .6 6. for samples: Add 400 mL RODI water to a 1-L volumetric.) 6.2 6. and 10 mL concentrated HCl . Store in polyethylene container in a refrigerator. 6 M HCl: Add 200 mL RODI water to a 500-mL volumetric. Add 1.3 6. 6 M HCl. Carefully add 250 mL concentrated HCl and fill to volume with RODI water.12 Bring to volume with RODI water and invert to mix thoroughly. trace metal purity. 12 samples.8 Compressed Argon 6. Degas for 10 min. purity 99. 50.3% NaBH4: Add 200 mL RODI water to a 500-mL volumetric. and 0 µg L-1: To seven 250mL volumetrics.9 Primary standards. Always stabilize the solution by first adding the NaOH. 6.e. 12. 6.15 Potassium iodide (KI) (10%) – ascorbic acid solution (10%): To a 500-mL volumetric. 100. Invert to mix thoroughly. Place in a glass beaker (4 tubes into each 250-mL beaker. blanks.7 Compressed air with water and oil traps 6.7 150 µg L-1 = 37. 6. Final concentration is ≈ 1% HCl. 1 mL of 1000 mg L-1 Se.25 mL PMWS + 122 mL HCl 12 µg L-1 = 3.5 g NaOH and mix until dissolved.11. High Purity Standards. i.11. 6.5 g of NaBH4. 1000 µg L-1 As and Se: Add 500 mL RODI water to a 1-L volumetric. Invert to mix thoroughly.5 mL PMWS + 119 mL HCl 25 µg L-1 = 6. in microwave at one time). 6. Add 1 mL of 1000 mg L-1 As.0. 75. Procedure Digestion of acid (HNO3 + HCl) extract 7. 7.6%. all prepared to < 200 mesh (75 µm).75 mL PMWS + 116 mL HCl 50 µg L-1 = 12.1 Prepare soil samples. 150. and fill to volume. (Procedure requires 1-mL per sample. Make fresh weekly. 6.5 6.11 Mixed Calibration Standards (MCS). Invert to mix thoroughly. 6.4 6. 0.17 QC Soil Standards: Loam C (certified reference material. Carefully add 500 mL concentrated HCl and fill to volume with RODI water..

) For As analysis.8 Each element is analyzed separately on the atomic absorption spectrometer. 7. do a set of MCS. 7. Do not allow MCS to stand greater than 2 h before As analysis. 7. (Note: digested soil samples and QC soil standards can be analyzed the same day.3.Digest the open tubes (do not cover) in a sample rack by submerging up to the neck of the tubes in a water bath (95° C).7 Selenium (sample extracts and MCS): Pour sample extract and MCS (without KI-ascorbic acid solution) into test tubes that have been placed in the sample holder of the sample changer.0 2.4 Remove tubes. proceed to Section 7.7 380 Selenium 196.7 0.2 To the microwave digested soil samples and MCS. fuming (loss of HNO3) should cease. Power (watts) Heating Power (%) Program Ramp (min) Pressure (psi) Temperature (°C) Hold (min) Value 1 600 100 5:00 800 180 30:00 Place thermocouple (in thermowell) into one sample. Heat microwave until 180° C is reached for 5 minutes.0 250 334 . Heat for 30 min and remove to cool. Include one QC soil standard and blank in each sample rack. pipette 15 mL of RODI water + 20 mL of concentrated HCl. cool. Mix well by inverting. Follow the manufacturer’s operating procedures for appropriate gas and liquid flow.5 Arsenic (MCS): Pipette 36 mL of digested MCS + 4 mL of KI-ascorbic acid solution into test tubes that have been placed in the sample holder of the sample changer.7. and adjustments to settings.6 Arsenic (sample extracts): Pipette 9 mL of sample extract + 1 mL of KI-ascorbic acid solution into test tubes that have been placed in the sample holder of the sample changer. Refer to manufacturer's manual for operation of AAS. HGAAS Set-up and Operation 7. Soil samples and QC soil standards have a final concentration of ≈ 6 M HCl.5. Do not allow samples to stand longer than 2 h before As analysis.Parameter Stage Max. At that time. 7. or placed into the refrigerator overnight for subsequent analysis the following day. Allow to stand 1 h before As analysis. Allow to stand 1 h before As analysis. 7. 7. Allow samples to cool and vent in the microwave for 5 minutes prior to removal. warm-up. Connect vapor generation accessory to AA. For Se analysis. Follow the manufacturer’s operating procedures for AA EDL settings. fill to volume and cap. Instrumental parameters for each element are as follows: ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ Element Wavelength Slit Width EDL Current nm mA ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ Arsenic 193. For every sample extract rack. Allow EDL to warm up 20 to 30 minutes. proceed to Section 7. Connect EDL power supply to AAS.

9 For automated analysis (using the autosampler). and allow to dry. respectively. 7. 7.14 If samples are outside the calibration range. as consensus/certified values. with a read delay of 48 s. 7. respectively. 7. Use the calibration reagent blank and calibration standards to calibrate the AAS. time average mode. The sodium thiosulfate solution must be removed by pumping RODI water through the system for 10 min. 7. BOC time of 5 s. The QC soil standards (Loam C and SRM 2710) have As contents of 47±3 and 626±38. Detection limits are 5 and 10 µg L-1 for As and Se. HGAAS Calibration 7.12 Each element is analyzed during separate runs on the AA.11 The instrument readings are programmed to display analyte concentration in µg L-1 (ppb).5) 335 . pump RODI water through the system for 10 min.17 If gas/liquid separator and tubing have not been exposed to contamination with KI. respectively. If QC fails after three attempts. The QC is 100 µg L-1 for As and Se.15 Soak the absorption cell in dilute HNO3 acid (0. Rinse for 30 s between samples. and read time of 2 s. 7. recalibrate and reread the QC. Clean-up and Maintenance 7.2 L min-1.1% w/v) for 30 min. respectively.5 and 0. a 1:5 serial dilution is performed using 6 M HCl. if performed 1000 = Conversion factor in numerator to kg-basis 1000 = Factor in denominator (µg mg-1) R = Air-dry/oven-dry ratio (procedure 3D1) E = Sample weight (g) (0. mg kg-1 soil.05) C = Dilution. pump a freshly prepared 1% sodium thiosulfate solution through the system for 10 min.10 Use the computer and printer to set instrument parameters and to collect and record instrument readings. the analysis is performed using atomic absorption with background correction. with + 30% rejection criteria.The flame is required only for heating the gas flow tube and is maintained as a low temperature as possible. Use an air/C2H2 mixture of 6.16 If gas/liquid separator and tubing (including autosampler sipper) has been exposed to contamination with KI. 8. 7. rinse thoroughly with RODI water. Calculations Convert extract As and Se (µg L-1) to soil As and Se (mg kg-1) as follows: Soil As (mg kg -1) = [A x B x C x R x 1000]/E x 1000 where: A = Sample extract reading (µg L-1) B = Extract volume (L) (0. Reported values are the average of five replications. These QC soil standards have automatic dilutions of 1:10 and 1:100. The QC is read at the end of each run.13 Use the QC standards after every 12th sample.

Am. Suarez. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 26:424-432. Akai. alluvial soils.05) C = Dilution. Martens.M. 2001..7 nm wavelength by Hg vapor. Yin et al. Health hazards: Arsenic. 1997.M. The digest is mixed with stannous chloride to reduce Hg to 336 .5) 9. Report Report As and Se to the nearest 0. L. Geotimes. In D. Ryker. if performed 1000 = Conversion factor in numerator to kg-basis 1000 = Factor in denominator (µg mg-1) R = Air-dry/oven-dry ratio (procedure 3D1) E = Sample weight (g) (0. Inacio et al. WI. WA. Selenium speciation of marine shales.. Sparks (ed. Safiullah. coal combustion. Barrow and Cox. Huang. 1997). J. and R. 2002. 27:597-604. Pinsker.M. ASA and SSSA.) Methods of soil analysis.G. M. Office of Environmental Health Assessment Services. 1987. 1992. Summary of Method Soil digests (HNO3 + HCl) from procedure 4H1a1 are analyzed for Hg using cold-vapor atomic absorption spectroscopy (CVAAS).. Ma. and enters the food chain primarily through atmospheric deposition (smelting.1 mg kg-1 soil. Soil Sci. 11. and S. 1999. Soil Sci. S. J. Mostofa.A. 2001. <2-mm (4H1a1c1a1) 1.. 1974. 793-831. Harris. 2002. 5. Int. 1996. Qual. and evaporation basin soils of California..L. 66:632-640. This method is based on absorption of radiation at 253. 2. but a hard problem. many studies have been performed which have examined soil-Hg interactions (MacNaughton and James.. Arsenic poisoning in groundwater: Health risk and geochemical sources in Bangladesh. Environ. Nov. H. L.G. Chen. Environ.L. Olympia. Geotimes. Tareq. Soc.M. Fujii. 1996) and ecosystem distributions (Hall et al. References Anawar. P. Madison. Nov.Q. p.J. Selenium and arsenic. D. p. Hazards of short-term exposure to arsenic contaminated soil. J. volcanic activity) and pesticide usage (Pais and Jones. Soc. State of Washington. Application Mercury is highly toxic to both plants and animals. K. Mapping arsenic in groundwater: a real need.. and W. Am.M. Arsenic concentrations in Florida surface soils: influence of soil type and properties. S. 34-36. Book Series No. and D. p. Total Analysis (4H) Acid Digestion (4H1) HNO3 + HCl Digestion (4H1a) Microwave (4H1a1) Cold Vapor Atomic Absorption Spectrophotometer (4H1a1c) Mercury (4H1a1c1) Air-Dry. Part 3 – Chemical Analysis. 10.Soil Se (mg kg -1) = [A x B x C x R x 1000]/E x 1000 where: A = Sample extract reading (µg L-1) B = Extract volume (L) (0. Due to the absorption of Hg by both organic and inorganic soil components. 32-33. 1998).

CETAC ASX-500 Model 510. Mercury data are reported as µg kg-1 soil by procedure 4H1a1c1. Safety Soil digests contain acid and must be handled appropriately. 1. and printer 5.5 ug L-1 = 0. Omaha. Microsoft Windows 97.3 Concentrated nitric acid (HNO3). CETAC Corp.the elemental state. 2. NE 5. NE 5. 2500 µL and 10 mL 5.0 ug L-1 = 0. 6. 500 µg L-1: Add 0.4 mL stock standard + 9 mL HNO3 + 3 mL HCl Dilute each working standard to mark with RODI water and invert to mix thoroughly.6.6 Computer.0 ug L-1 = 0...9 Calcium sulfate (anhydrous) or equivalent desiccant 6. Invert to mix thoroughly. Omaha. CETAC ADX-500.5 ug L-1 = 0. These working standards are used for Normal and High Throughput Ranges. Absorbance (peak height) is measured as a function of mercury concentration. Woburn. NE 5. Omaha. 16 N.1 Reverse osmosis deionized (RODI) water. Procedure uses a primary Hg standard that is diluted for working standards.5 Stock standard. the solution is passed over a gas-liquid separator in a closed system to separate the gaseous Hg from solution. Omaha.2 mL concentrated HCl to 500 mL volumetric and dilute to mark with RODI water. The Hg vapor passes through a cell positioned in the light path of an atomic absorption spectrophotometer.4 Primary standard: 1000 mg L-1 Hg.5 3. 12 N.0 ug L-1 = 9 mL HNO3 + 3 mL HCl 6. Omaha. CETAC Corp. Equipment 5.5.6 Standard Hg calibration solutions or working standards are 4.25 mL primary standard to 500 mL volumetric and dilute to mark with RODI water and invert to mix thoroughly.1 Cold-vapor atomic absorption spectrophotometer (CVAAS). and 0.1 mL stock standard + 9 mL HNO3 + 3 mL HCl 6. Use gloves and avoid skin contact. 6.0. CETAC.5 Peristaltic Pump. Use trace pure HNO3..7 Stannous chloride.. electronic digital. MA.0 ug L-1. Reagents 6. CETAC Corp.0..3 Autodilutor Accessory. NE 5.6. CETAC M-6000A Mercury Analyzer. prior to passing through the Hg vapor trap may contain Hg vapor. CETAC Corp. Rainin Instrument Co. 3. Do not run the instrument unless the exhaust gas is properly scrubbed or removed. Omaha. Use trace pure HCl. reducing agent 10% stannous chloride solution (SnCl2 in 7% HCl). CETAC Corp. Corp.3 1. and certain volatile organic materials may be interferences.6. CETAC M-6000A Software. 6. 6.2 Concentrated hydrochloric acid (HCl).2 0. 5.25 mL stock standard + 9 mL HNO3 + 3 mL HCl 6.6 4. Interferences Copper.4 2.8 Compressed argon gas 5.6. Gasses exhausting from the Hg analyzer cabinet. Charleston.. SC.4 Nafion drying tube.2 Autosampler.. Using argon as a carrier gas. ASTM Type I grade of reagent water 6.7 Pipettors. 3.6.0 ug L-1 = 0. 0. High-Purity Standards. Add 50 g of stannous chloride and 97.0. 6. 337 . chlorides. 4.1 0.5. NE. To six 50-mL volumetric flasks add as follows: 6.6. NE 5.3 mL stock standard + 9 mL HNO3 + 3 mL HCl 6.05 mL stock standard + 9 mL HNO3 + 3 mL HCl 6.

Ensure integrity of lamp (there is some loss of performance at 13 mA but replace at 15 mA). Three ranges of analysis (Highest Sensitivity.4 mL HNO3 to 1-L volumetric and dilute to mark with RODI water.1.3. 7.8 mL min-1 (reagent). 6. solid.050 µg L-1 Baseline Correction: 1 point Normal Range: Sampling Times: Integration 1 s Read Delay 50 s Auto-Adjust Integration Replicates 4 338 . Argon gas carrier must be supplied at 100 psig (6.0 mL min-1 (sample) and 0.10 Potassium permanganate. 7. Liquid flow is always set at fixed flow of 4.6.9 Rinse (5% HNO3): Add 71. General parameters are as follows: High Throughput Range: Sampling Times: Integration 1 s Read Delay 35 s Auto-Adjust Integration Replicates 4 Instrument Control Gas Flow 300 mL min-1 Autosampler Setup Sip Duration 20 s Rinse Time 20 s Repeats 1 Sample Matrix: Liquid Reslope Frequency: 0 Reslope Standard: Standard No.9 bar). 3 (check standard) Detection Limit: 0. and High Throughput) have been developed on the CETAC Mercury Analyzer. Fine glass wool only. Method parameters for each of these ranges are saved on a different Worksheet Template. 6. Procedure 7. Oven radiator temperature must be at 125°C to maintain the actual gas temperature of 50° C.11 Glass wool.2. 7. Turn mercury analyzer and mercury lamp for warm-up (90 min) prior to analysis. Normal. Invert to mix thoroughly. Turn on computer and choose Worksheet Template appropriate to range of analysis. 6. Invert to mix thoroughly.8 Diluent: Add 90 mL concentrated HNO3 and 30 mL concentrated HCl to 500 mL volumetric and dilute to mark with RODI water. crystalline. fills safety trap for Hg vapor exhaust.

001 µg L-1 Baseline Correction: 2 point 7.4.4.7 Do not let liquid level overflow GLS into Nafion drying tube.4 With drain pump tubes unclamped. 3 (check standard) Detection Limit: 0.Instrument Control Gas Flow 85 mL min-1 Autosampler Setup Sip Duration 30 s Rinse Time 45 s Repeats 1 Sample Matrix: Liquid Reslope Frequency: 0 Reslope Standard: Standard No.4. respectively.1 Check the bottle supplying the ASX-500 rinse station is full of 5% HNO3. immediately reengage quick-release clamps on drain pump tubes.6 Upon wetting. 7. 7.015 µg L-1 Baseline Correction: 1 point Highest Sensitivity Range: Sampling Times: Integration 1 Read Delay 50 Auto-Adjust Integration Replicates 4 Instrument Control Gas Flow 40 mL min-1 Autosampler Setup Sip Duration 60 s Rinse Time 140 s Repeats 1 Sample Matrix: Liquid Reslope Frequency: 0 Reslope Standard: Standard No.3 Use sample and reagent tubes and pump 5% HNO3 and stannous chloride reagent.2 Use quick release mechanism and fully release clamp tension on lower two tube channels of peristaltic pump (drain channels).4. 7. 7. 3 (check standard) Detection Limit: 0. including apex.4.5 Allow GLS to fill until liquid level reaches top of GLS center post or until gas bubble propels a meniscus upward to wet post all along its length. 7.4.4.4. GLS should begin to fill with 5% HNO3.Prior to analysis ensure that the gas-liquid separator (GLS) post is fully wetted as follows: 7. 339 . 7.

8 Run calibration and analysis in “Analysis”. 7.6.6.10 Perform shutdown: turn off mercury lamp. Pump all lines dry after rinsing.6. final volume. 7.6 Define Time Profile using Signal Profile Chart (sample time. 7.6. 340 . 7. and turn off the computer. pump. run RODI water through sample sipper tube and stannous chloride reagent lines. change point times by clicking on chart and dragging to right.10 Release shift and mouse key and chart will update baseline times in worksheet.6.9 Once GLS has emptied. 7.2 Using mouse. define sample time by clicking on chart and dragging to right.12 Use mouse and control key.6. liquid level normally stops rising and goes back down 7.9 After completion of analytical run.3 Integration times will automatically be recalculated based on new total sample time.8 With drain tube clamps properly reengaged and pump running. 7. ASX-500.5 Use mouse and shift key and change point times by clicking on chart and dragging to right. dirty sample windows.7 Enter sample numbers.6. press and hold shift key. and thermal drift). M-6000 main power.5 Zero analyzer to compensate for baseline offsets (due to microscopic dust buildup on the optics. 7. 7.6 To do this. 7.4. and 1st and 2nd baseline correction points) as follows: 7. 7. 7.8 Light blue vertical cursor line will appear.4. 7.6. argon gas. close the M-6000A Software.6. drag mouse to right until portion of signal to be used as baseline correction point is between light blue and dark red cursor lines. and weights in “Labels”.9 Without releasing shift key or left mouse button.11 Current 2nd baseline correction point on chart will start at light green vertical line and stop at purple line. 7. 7.6.7.7 Click with left mouse button on left limit of part of signal to be used on baseline correction point.1 Current sample time on chart will start at dark green vertical line and stop at light red vertical line.6.6. 7. leave pump running (keep liquid flowing) 7. 7.4 Current 1st baseline correction point will start at light blue vertical line and stop at dark red line.

Sanders. 1992. X-ray diffraction and thermal analysis. Allen.F. 11.. Report Hg data are reported to the nearest 0. Lucie Press. 10. 1996. M. Sodium. FL. if performed 1000 = Conversion factor in numerator to kg-basis R = Air-dry/oven-dry ratio (procedure 3D1) E = Sample weight (g) 9. and M. References Barrow. Duarte. and R. C.. Sci. James..M.B. Sources and sinks of mercury in the coastal lagoon of Aveiro. Huang. By goethite.F. The effects of pH and chloride concentration on mercury sorption: I.g. 1994). Jr. Manganese. M. 1974. Total Analysis (4H) Acid Digestion (4H1) HF + HNO3 + HCl Digestion (4H1b) Microwave (4H1b1) Boric Acid (4H1b1a) Inductively Coupled Plasma Atomic Emission Spectrophotometer (4H1b1a1a1-11) Aluminum. and J. Zirconium. 47:431-440. chloride. Bain and Smith. Y. Adsorption of aqueous mercury (II) complexes at the oxide/water interface. Pais. The handbook of trace elements. 1997. Lucas. and organic matter. Boca Raton. Magnesium.E. and V. Cox.F. Colloid Interface Sci. and P. Hall.. Silicon. Total Environ. Pinto.T. Inacio. Portugal). identification of minerals was based on elemental analysis and optical properties (Washington. Li. J. Application Prior to the development of modern analytical techniques.J.8. and Titanium (4H1b1a1a1-11) Air-Dry.C. and M. A. Chemical analysis is still essential to determine mineral structural formulas and to identify and quantify specific mineral species through elemental allocation to minerals. Potassium. 43:295-304.S. Many clay mineral groups are subdivided based on composition. Y.P. 1930. Calculations Analytical data is reported by the instrument in µg mL-1 in solution. 1998. V. M. Istvan. e. Geoderma 85:325-339. Pereira. Jones. It is converted to µg kg-1 in soil as follows: Hg in soil (µg kg-1) = [A x B x C x R x 1000]/E where: A = Sample extract reading (µg L-1) B = Extract volume (mL) C = Dilution. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 64:75-87.O. <2 µm (4H1b1a1a1-11b2) 1. J. Iron. St. Portugal. <2 mm (4H1b1a1a1-11a1) Oven-Dry. Caldeeira. H. J. Mercury contamination in sandy soils surrounding an industrial emission source (Estarreja.G. 341 . Calcium. M.. Phosphorus. Soil Sci. N.C. A. 1987. Adsorption of mercury(II) by soil: Effects of pH. 223 pp. Yin.. MacNaughton.1 µg kg-1.

Careful selection of specific wavelengths for data reporting is important. the rotor and samples are cooled. K. HNO3 + HCl aids in the digestion of soil components. Safety Wear protective clothing and eye protection. 3. P. When preparing reagents. and mineral weathering within or between pedons. Elemental concentration of the digestate is determined using an inductively coupled plasma atomic emission spectrometer (ICP-AES). The digestate then quantitatively transferred onto a 100-ml polypropylene volumetric with boric acid solution to achieve a final boric acid concentration of 2. Procedure 4H1b1 follows EPA method 3052. Keep HF acid refrigerated and avoid contact with skin of all acids. Mg.1%.002 mm) may be used or a clay suspension (procedure 7A1a1) containing approximately 250 mg of clay material is pipeted into a digestion container and dried at 110°C. The P and Na content of the clay fraction is not measurable when the soil is dispersed in sodium hexametaphosphate (procedure 7A1a1). The vessel is inserted into a protection shield and covered. Interferences Insoluble fluorides of various metals may form. 2. Samples and standards are matrix matched to reduce interferences where possible. dried clay (<0. The volumetrics are allowed to stand overnight. Fe. or Ti/Zr. the fine-earth (<2-mm) fraction. 3. and Zr are determined by ICP-AES by procedures 4H1b1a1a1-11. 4.0-mg sensitivity 342 .0 mL HNO3. and 20 ml of 4.5% boric acid solution is added (4H1b1a). 5. This interpretation is determined from differences between horizons or pedons in elemental concentrations. Procedure 4H1b1a is a digestion of 100 mg of dried clay suspension. The concentration of Al. such as water-soluble or Bray-1 extractable P. Ca. To the vessel. The samples are then covered and heated in the microwave. Equipment 5.1 Electronic balance. Mn. A equal amount of suspension is pipeted into a tared aluminum-weighing dish and dried at 110°C to obtain a dried sample weight. 1968. 1994). elemental ratios such as Si/Al. Phosphorus fertility of a soil and potential water quality problems can be better understood by measurements of total P. and placed into a rotor with temperature control. especially the organic fraction. Hydrofluoric acid (HF) is efficient in the digestion and dissolution of silicate minerals for elemental dissolution (Bernas. Si/Al+Fe. Ti. especially when compared to other P measurements.0 mL HCl. Si. Spectral and matrix interferences exist. Filling the digestion vessel to greater than 25 percent of the free volume or adding organic reagents or oxidizing agents to the cup may result in explosion of the digestion microwave system.Analysis of the entire fine-earth (<2-mm) fraction or specific particle-size separates provides information on parent material uniformity. Sawhney and Stilwell. Formation of SiF4 results in gaseous losses of Si. Samples are placed in Teflon digestion vessels and heated in a microwave. The inherent fertility of a soil derived from its parent material can be examined by determination of the basic cations relative to the Si or Al content. Restrict the use of concentrated acids to the fume hood. 9. Wash hands thoroughly after handling reagents. or from differences in total elemental concentrations compared to concentrations determined by selective dissolution techniques. exercise special care. pedon development. Na. In addition. filled to volume. Following microwave digestion. but additions of boric acid retards formation of this molecule as well as dissolves other metal fluorides. or other particle size separate with HF + HNO3 + HCl. and approximately 60 mL saved for analysis. Background corrections are made by ICP-AES software. ±1. Summary of Method A 250-mg <2-mm or other particle-size soil separate which has been oven-dried and ground to < 200 mesh (75 µm) is weighed into a 100-ml Teflon (PFA) sample digestion vessel. respectively. and 4 mL HF are added.

CFT Series Compressed gasses. Part No. Computer.6. If sample is principally composed of organic materials (organic C > 15%). (±0. Quartz torch. (10-ml maximum) pipettes suitable for HNO3 and HCl delivery from 2. Ryton 6. CT. Perkin-Elmer Corp. Perkin-Elmer Corp. Desiccator Disposable aluminum-weighing dishes Volumetrics. ver. (Note: samples are typically prepared in sets of 14. electronic digital.5. HNO3 + HF. Charleston.7 Boric acid solution.8 5.7 5. Procedure Microwave Acid Digestion 7.4 Concentrated hydrochloric acid (HCl).5 Concentrated nitric acid (HNO3). with WinLab software.9 percent. 45 MHz free running. from High Purity Standards. AS-90. 7. or H2O 7. If a clay suspension is used. argon (minimum purity = 99. proceed to section 7. If using dried specimen. SC.2 5. Perkin-Elmer Optima 3300 Dual View (DV).3 5.0 g low trace metal. with screw caps Pipettes. (Preparation of Clay Suspension. Norwalk. 16 N. Single elemental standards in dilute HNO3.. perform a preliminary digestion in the muffle furnace in an digestion crucible: 250°C for 15 min.1 mg in a 100-ml TFM vessel. Perkin-Elmer Corp. as the digestion rotor accommodates that number of samples. 450°C for 15 min.6 5.5. Clay dispersion by this method eliminates quantitative analysis of Na and P in the clay due to dispersion by sodium hexametaphosphate.11 5. 1.1.12 5. ASTM Type I grade of reagent water 6.1 Reverse osmosis deionized (RODI) water. granular boric acid (H3BO3) in 1000 mL RODI water. 500-mL. A 250 mg sample is weighed to the nearest 0. 100 mL Polypropylene bottles.4 5.15 5. nalgene. proceed to section 7.999%) Autosampler.996%) and nitrogen(minimum purity = 99.5 percent..10 5. 4.2 Prepare Na-saturated clay as in procedure 7A1a1.. CEM Mars 5. sleeves composed of advanced composite).0 mm id). trace pure grade 6.. Part No.2 Calcium sulfate (anhydrous) or equivalent desiccant 6. manufacturers variable volume.5 L bottles. with cap Electronic balance.18 Pipet(s) capable of delivering 3. RF generator. MA Inductively coupled plasma atomic emission spectrophotometer (ICP-AES).0 g low trace metal. 14 position-HP500 Plus vessel and rotor (vessels composed of PFA. low trace metal content 6. 6. Norwalk.8 Primary standards: 1000 mg L-1.. followed by 550°C for 1 h. polypropylene. N069-1662. Rainin Instrument Co. Digestion of the entire fine earth (<2-mm) fraction or any fraction not derived by dispersion with sodium hexametaphosphate (or other Na and P-containing dispersing agents) can be quantitatively 343 .9 5. 4. 500-mL. CT. polypropylene Containers.1 mg sensitivity) Microwave. N069-5362. trace pure grade 6. and 9 ml. Volumetric flasks. granular boric acid (H3BO3) in 1000 mL RODI water.17 5. 4.6 Boric acid solution.16 5.3 Hydrofluoric acid (HF). Norwalk. Norwalk.19). Perkin-Elmer Corp. 48%. floor mounted power unit.1 Fine-earth (<2-mm) or a specific particle size separate ground to <200-mesh (75 µm) is used. 2500 µL and 10 mL. 60 mL. Neslab.13 5. Reagents 6. CT. 6. Omnifit Corp.14 5.2 to 7. CT. and printer Recirculating chiller.8 to 7. 12 N. Dissolve 19. Woburn.5 5. alumina injector (2. Dissolve 45. Sections 7.

70% power for 9.15 Invert the volumetric flask to mix and decant approximately 60 mL into a labeled polypropylene container. holding at 180°C Cool (Vent) for 15 min 7. then cover vessels and re-digest in microwave at: 1200 Watts. 7. Use this value as the sample weight in the calculations. reference soil sample from the SSL repository. Add acids in the fume hood.5 min (350 psi). More dilute suspensions should be partially evaporated under a fume hood to concentrate the clay prior to transfer to the Teflon container. Allow to stand overnight to dissolve any metal fluorides.5 Dry the Teflon container and clay suspension in an oven for 4 h or until the aqueous portion of the suspension is completely evaporated. 344 . Remove from oven and cool on the bench top or in a fume hood. achieving a final concentration of 2. 7.8 Place digestion rotor in the microwave oven and insert the temperature probe into the reference vessel.0 mL HCl into the sample and allow to completely wet and then pipet 4 mL HF into sample.9 Microwave settings are as follows: 1200 Watts. dry at 110°C.13 Transfer contents of digestion vessel to a 100-mL nalgene volumetric flask and adjust to near volume with 1. 100% power for 10 min (350 psi) to approximately 180°C 1200 Watts. and a National Institute of Standards and Technology (NIST) standard reference or other reference material by the same digestion method. Attach the probe cable into the fitting in the top of the microwave.6 Pipet 9. 7. 7. 7.12 Open each vessel carefully. Finish filling to volume with 1. Run one of these standards with each set of 14 samples. 7. Dispersion of clays and cleaning of test tubes and dishware should be with RODI water. 7. cool in a desiccator. add 20 mL 4.5 percent boric acid (H3BO3) solution.10 After venting. 7.11 Remove rotor from oven and place in fume hood.9% boric acid. 7. Connect the pressure monitor to the vessel. disconnect temperature probe from microwave.analyzed for Na and P.1 percent H3BO3. The volume of required suspension depends on the clay concentration in the suspension.1 mg. cover. Cooling in a desiccator is not required. Cool (vent) for 15 min.0 mL HNO3 and 3.3 Pipet a known aliquot of clay suspension containing approximately 250 mg clay into a 100mL TFM vessel.16 Prepare working standards of a blank. at 160°C for 10 min.4 Pipet a duplicate aliquot of suspension (as used in section 7. 7. 7. 7.14 Cap flask and mix well by inverting.9% boric acid.7 Place covered Teflon digestion vessels in protective sleeve. and weigh to the nearest 0.3) into a tared Al weighing dish. and place into rotor. but is generally from 6 to 10 mL. 100% power (350 psi) to 160°C. 7.

592.995 178. 25. Fe. No initial dilutions of samples are necessary prior to analysis. Mg.5 of the Al.mL volumetic flask. Ti. Na. for ICP-AES analysis are as follows: 7. Check instrument alignment and gas pressures to obtain optimum readings with maximum signal to noise ratio. Each working standard is used in two concentrations. and Na primary standards (1000 mg L-1). 20. The concentrations of elements in the low standards (CALO. The selected wavelengths are as follows: (reported wavelength listed first and in bold): Element Al Ca Fe K Mg Mn Na P Si Ti Zr Wavelength ----------. high and low. add 112.5. 40. 7.0. and 25 mg L-1 of Al. 238.0.nm --------308.610. BEC. and Mn.620 212. 150. add 225. 7. and SIHI). and Operation 7. and 10. respectively. at the specified concentrations.17. respectively. %RSD of Mn solution) prior to analysis as discussed in operation manual of instrument. respectively. 5. Zr. and 12.490 280.0. 343.570 589. add 75. 7. Mg.0 mL HNO3. 2. respectivley. K.20 Analyses are generally performed at two or more wavelengths for each element. respectively.0. respectively. and 5. 37. Fe. respectively.5 mL of the Si and P primary standards (1000 mg L-1). and Mn. 317. and Mn primary standards (1000 mg L-1). 213. 396. 260.939.5. Zr.5. 7. P. 368. Si.157 315. Fe.197. and Na. and Na. 10. add 50. 12.17.0 mL of the Al.5. To a 500mL volumetric flask.075 257. 75. respectively. 5.271. ALLO. 7.5. add 37.0 mL of the Si and P primary standards (1000 mg L-1). 50. Mn. 75. K. 588. 5.887. 7.0. and 10.940. To a 500-mL volumetric flask.0. 251.0 and 5. To a 500-mL volumetric flask. ALHI. Fe. and SILO) are 50 percent of the concentrations in the high standards (CAHI.0 mL HF.221. Mg.17.19 Use the ICP-AES in radial mode and analyze for the following elements: Fe.2 CAHI is 150. 25.215.0 mL HCl. add 100. 15. Mg. Make all standards and the blank to a final 500-mL volume with RODI water. 7.818 345 . and Mn primary standards (1000 mg L-1).412. Zr. Ti. Perform instrument checks (Hg alignment.3 ALLO is 100. and 50 mg L-1 of Al. 5. Ca. 10.17. and Na primary standards (1000 mg L-1). and 25. Mg. The amounts of primary standards (1000 mg L-1) to make 500-mL volume of the low and high calibration standards. To a 500-mL volumetric flask. respectivley. 7. Zr. respectively.0. respectively.5 SILO is 225 and 5 mg L-1 of Si and P. and 10 mg L-1 of Ca.0. 20. Set-up. and 20 mg L-1 of Ca.0 mL of the Ca. 279.932 259. respectively.205 766. Zr.1 CALO is 75.5 and 2. 10. To a 500.17.4 ALHI is 200.ICP-AES Calibration Standards. 45. Ti. K. To a 500-mL volumetric flask. 2.522 339.0.17 Instrument calibration standards for analysis are limited to specific combinations of elements because of chemical incompatibilities of certain elements. Ti.6 SIHI is 450 and 10 mg L-1 of Si and P. K. and Ti.612 334.0 mL of the Ca. Al. K. also add the following chemicals: 20.18 To the calibration standards and a blank.17.90 g granular Boric Acid.

2 Data are recorded on an elemental basis. if performed R = Air-dry/oven-dry ratio (procedure 3D1) 1000 = Conversion factor in numerator to kg-basis E = Sample weight (g) 8. oxide form.22 Establish detection limits using the blank standard solution.1 The calculation of mg kg-1 of an element in the soil from mg L-1 in solution is as follows: Analyte concentration in soil (mg kg-1) = [A x B x C x R x 1000]/E A = Sample extract reading (mg L-1) B = Extract volume (L) C = Dilution.000 to convert from mg kg-1 to %.21 Use the blank standard solution to dilute those samples with concentrations greater than the high standard. These instrumental detection limits are calculated by using 3 times the standard deviation of 10 readings of the blank. and the elemental percent in the oxide form are as follows: Element Oxide Form SiO2 Al2O3 Fe2O3 MgO MnO K2O TiO2 CaO ZrO2 P2O5 Na2O Elemental % 46. Rerun all elements and use only the data needed from the diluted analysis.0 43. An example is as follows: Atomic weight Si = 28. The element.09) x 100 = 46. Analyzed values lower than the detection limits are set equal to zero.0 Molecular weight SiO2= 60.09 Atomic Weight O = 16.7 52. 8.7.09 Calculate percent Si in SiO2 as follows: Si (%) = (28. The factor for converting from an elemental form to an oxide form is based on the atomic weights of the element and oxygen. 7.2 346 Si Al Fe Mg Mn K Ti Ca Zr P Na .0 59.9 69.3 77.9 71.4 83.6 74. Often users request data in an oxide form. To convert from mg/kg Si to percent Si oxide (SiO2) in the soil.7 % There is 46. then divide the percent Si by 0. These values establish the lower detection limits for each element. Calculations 8.7 percent Si in SiO2.09/60. divide by 10.5 74.9 60.467 or multiply by the inverse of this value.

. charcoal. 1982). and D.F.W. 1996). automatic titrator (6A1c.724 to calculate organic matter. 1994. a measurement of organic C can serve as an indirect determination of organic matter. Surface soils rarely have a factor <1. Report Analyses are generally performed at two or more wavelengths for each element. Dissolution and elemental analysis of minerals.5. 11.0. Chemical analysis. extractable bases. soils.9. H. Any constant factor that is selected is only an approximation. The particle-size fraction digested needs to be identified with each sample. Zelazny (eds. B.C. the soil organic matter generally includes only those organic materials that accompany soil particles through a 2-mm sieve (Nelson and Sommers. Soc. stability of soil aggregates. WI. 347 . Chapman and Hall. Inc. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. The subsoil factor may average ≈ 2. Misc. and Sulfur (4H2a1-3) Air-Dry. Organic C consists of the cells of microorganisms. Soil Survey Staff. water retention capacity. Am. Amonette and L. Stilwell. e.8 to 2. Wilson (ed. and micronutrients. The preference is to report organic C rather than to convert the organic C to organic matter through use of an approximate correction factor. Smith. stable "humus" synthesized from residues. London. the SSL used the wet combustion method. 1982). Total Analysis (4H) Dry Combustion (4H2) Thermal Conductivity Detector (4H2a) Total Carbon. Nitrogen. Organic C determination is either by wet or dry combustion.S. B. The proportion of organic C in soil organic matter for a range of soils is highly variable. England. Chem. Anal. Values for organic C are multiplied by the "Van Bemmelen factor" of 1.) Clay mineralogy: Spectroscopic and chemical determinative methods. 1987).) Quantitative methods in soil mineralogy..E. P. 1953). capacity to supply N. Application Organic Matter and Organic Carbon: Soil organic matter has been defined as the organic fraction of the soil exclusive of undecayed plant and animal residues and has been used synonymously with "humus" (Soil Science Society of America. References Bain. The organic matter content influences many soil properties. and soil aeration (Nelson and Sommers. and coal (Nelson and Sommers.E. In M. FeSO4 titration.J. p. This factor is based on the assumption that organic matter contains 58% organic C. The chemical analysis of rocks. Madison. In J.. Publ..L. 49-82. with the one selected wavelength for reporting purposes. In the past. 1996)..L. and B. <2 mm (4H2a1-3a1) 1. Data are reported to the nearest mg kg-1. and environmental samples. for laboratory analyses. D. method obsolete. 300-332. Washington. As organic C is the major component of soil organic matter. Walkley-Black modified aciddichromate digestion. A new method for decomposition and comprehensive analysis of silicates by atomic absorption spectrometry.g.8 and usually range from 1. NY. John Wiley and Sons. e. 40:1682-1686. Studies have indicated that subsoils have a higher factor than surface soils (Broadbent. 4th ed. However. graphite. plant and animal residues at various stages of decomposition. NY. Bernas. Sawhney. 1994. Inc. Soil Sci.g. 1968. SSSA. p. Organic C is a major component of soil organic matter. 1930. 10. and nearly inert and highly carbonized compounds.

Most of the organic C is associated with the organic matter fraction. Total S typically ranges from 0. with the organic fraction accounting for >95% of the total S in most soils from humid and semi-humid (Tabatabai. The C:N ratio generally ranges between 10 to 12. 2. wet or dry combustion. i. combustion) procedure (Bremmer. and 0. Two methods of analysis of total N have gained acceptance for the determination of total N in soils. The proportion of organic and inorganic S in a soil sample varies widely according to soil type and depth of sampling (Tabatabai. 1982. Reagents that have been used for measuring SO42-S include water. In well-drained. e. In marine tidal flats. 1996). The typical use of total S is an index of the total reserves of this element. 1996). organic C is also used at lower taxonomic levels. after which the loss in weight of the soil is taken as a measure of the organic matter content (5A). ustollic and fluventic subgroups (Soil Survey Staff.. Soils with large amounts of illites or vermiculties can “fix” significant amounts of N compared to those soils dominated by smectites or kaolinites (Young and Aldag. 1982). In total C determinations.05%. The SSL uses the combustion technique for analysis of total S (4H2a3). potassium phosphate 348 . Mineralization of organic S and its conversion to sulfate by chemical and biological activity may serve as a source of plant-available S. most of the inorganic S normally occurs as sulfate. The total N content of the soil may range from <0. there are usually large amounts of reduced S compounds that oxidize to sulfuric acid upon exposure to the air. The organic C in mineral soils generally ranges from 0 to 12% (Nelson and Sommers. and the N distribution in the soil profile. and the inorganic C is generally found with carbonate minerals. total S may be >0. Total Sulfur: Organic and inorganic S forms are found in soils. ammonium chloride and other chlorides. sodium carbonate and other carbonates.e.. Variations in the C:N ratio may serve as an indicator of the amount of soil inorganic N. The difference between total and inorganic C is an estimate of the organic C. ammonium acetate. other anaerobic marine sediments. The SSL uses dry combustion (4H2a1). 1996). In soil taxonomy.01 to 0. The SSL uses the combustion technique for analysis of total N (4H2a2). which may be converted to plant-available S. hot water. Nommik and Vahtras. The total N data may be used to determine the soil C:N ratio. the soil potential to supply N for plant growth. Extractable sulfate S (SO42-S) is an index of readily plant-available S. Since the organic C of may soils diminishes with depth while the level of “fixed” N remains constant or increases. 1996). 1999).5% in surface layers of many cultivated soil (Bremmer and Mulvaney.06 to 0. In arid regions. Organic C defines mineral and organic soils.The SSL also uses a direct determination of soil organic matter. The organic matter is destroyed. the C:N ratio narrows (Young and Aldag. Total C can be used to estimate the organic C content of a soil. These include the Kjeldahl (1883) method. The potential to “fix” N has important fertility implications as the “fixed” N is slowly available for plant growth. well-aerated soils.g.05% in most mineral soils.e. and mine spoils. Total C is quantified by two basic methods. which is essentially a wet oxidation procedure and the Dumas (1831) method. Uncultivated soils usually have higher C:N ratios than do cultivated soils.5% in peats. Total Nitrogen: Total N includes organic and inorganic forms. The percent organic matter lost on ignition (400°C) can be used in place of organic matter estimates by the Walkley-Black organic C method. In the SSL procedure 4E1a1a1. 1982). all forms of C in a soil are converted to CO2 followed by a quantification of the evolved CO2. significant amounts of inorganic S are found as sulfates such as gypsum and barite (Tabatabai. The inorganic C should be approximately equivalent to carbonate values measured by CO2 evolution with strong acid (Nelson and Sommers.. 1996). The amount of carbonate is then calculated as a CaCO3 equivalent basis. which is fundamentally a dry oxidation (i. In organic soils. the amount of carbonate in a soil is determined by treating a sample with HCl followed by manometrically measuring the evolved CO2. 1982). Total Carbon: Total C is the sum of organic and inorganic C.02% in subsoils. 1996).

and S are reported by methods 4H2a1-3a1. with helium as the flushing and carrier gas. 5. especially for total S and SO42-S. (1968).. Elementar varioEL and Elementar varioEL III. Burnt sample substance that remains in ash finger falsifies the results of subsequent samples.2 Quartz bridge 5.and other phosphate. and ammonium fluoride (Bray-1). Inc. 3. For detailed discussion of the application of total C. NJ. There are other methods available for determination of S. N. 4. MI) as follows: 5. Stevensville. refer to Soil Survey Staff (1995).1. The desired measuring components (N2.9 Tin boats (4 x 4 x 11 mm) 5. The combustion gases are freed from foreign gases. and combustibles (Elementar Americas. Extraction reagents for organic S include hydrogen peroxide. Substance loss after weighing should be avoided by exact folding of the sample into the tin foil. N. N.3 Combustion tube 5. Percent total C. Air in the sample material should be minimized (falsifying the N value) by compressing the sample packing.1 Elemental analyzer with on-line electronic balance (0. respectively.6 Support tube (65 mm) 5.4 Reduction tube 5. Summary of Method An air-dry (80 mesh. Extractable SO42-S does not include the labile fraction of soil organic S that is mineralized during the growing season (Tabatabai.5 Gas purification (U-tube.1.1± mg sensitivity) and automatic sample feeder. Equipment 5.1..1. The investigator may refer to the review by Beaton et al.. 1996). with varioEL software. Aggressive combustible products should not be analyzed.1. weighed. Alpha Resources Inc. the instrument must be cooled down and cooled off. avoid non-volatile sulfates).1 Quartz ash finger.1. sodium hydroxide. and printer 349 . and S by an elemental analyzer (procedures 4H2a1-3. Interferences Contamination through body grease or perspiration must be avoided in sample packing. decreasing their effectiveness and durability.8 O2 lance (150 mm rapid N) 5. sodium oxalate.1. HanauGermany. sodium bicarbonate. sodium peroxide. and sodium pyrophosphate.1. GL 18) 5.1.1. Insufficient O2 dosing reduces the catalysts. Laurel. and S. respectively). Elementar Analysensysteme GmbH. and SO2) are separated from each other with the help of specific adsorption columns and determined in succession with a thermal conductivity detector. quartz 5.10 Tin foil cups 5.7 Protective tube 5. Hanau-Germany. WO3 is used as sample additive and combustion filling to aid combustion or bind interfering substances (alkaline or earth-alkaline elements. 2. Before working on electrical connections (adsorption columns) or before changing reaction tubes. Safety Exhaust gas pipes should lead into a ventilated fume hood.2 Computer. CO2. <180 µm) sample is packed in a tin foil. Gloves and safety glasses should be worn at all times during operation and maintenance of instrument. The elemental analyzer works according to the principle of catalytic tube combustion in an oxygenated CO2 atmosphere and high temperature. Mt. Elementar Analysensysteme GmbH. and analyzed for total C.

carrier gas. Laurel. and 18.6% C. Elementar Americas. 3 – 5 mm 6. combustion tube filling 6.7% O.1% H.5% S 6. sample additive 6. 8. 1 – 2 mm 6.1 Refer to the manufacturer's manual for operation and maintenance of the elemental analyzer.9 Phosphorus pentoxide.6 Tungsten trioxide granulate. Reagents 6. combustion gas. NJ 6.8 Silver wool 6.1 Sulfanilic acid. Procedure Elemental Analyzer Set-up and Operation 7. Standby Timing Flush Oxygen Delay Auto Zero Delay Integrator Reset Delay Peak Anticipation N Peak Anticipation C Peak Anticipation S 1140° C 850 ° C 0°C 85 ° C 210 ° C 140 ° C 5s 10 s 30 s 50 s 70 s 125 s 70 s 60 s 3 mV 3 mV 3 mV 150 s 1s 90 s 120 s 180 s Integrated Reset Delay for S Thresholds N Peak C Peak S Peak O2 Dosing Index 1 Index 2 Index 3 Index 4 Index 5 350 .3 Corundum balls.7 Quartz wool 6.4 Cerium dioxide.. calibration standard.5 Tungsten oxide powder.1 % N. high purity.6. The following are only very general guidelines for instrument parameters for the various analytes in the CNS mode. 99. alumina spheres. Inc. Mt. 41.996% purity 6. Temperature Furnace 1 Furnace 2 Furnace 3 CO2 Column SO2 Column SO2 Col.11 Oxygen.995% purity 7. 4. 99.2 Copper sticks 6. Sicapent.10 Helium. 27. Conditioning of the elemental analyzer and determination of factor and blank value limit are part of the daily measuring routine.

100 g of tungsten oxide in tin foil and tare. or mixed). homogeneity.1 or if components that influence the results (e. Bremmer. Bull.g. oven-dry basis = N (%) instrument = Air-dry/oven-dry ratio (procedure 3D1) S (%) = Si x AD/OD where: S (%) Si AD/OD = S (%) on oven-dry basis = S (%) instrument = Air-dry/oven-dry ratio (procedure 3D1) 9. Nitrogen – Total. Report Report total C and S percentage to the nearest 0. Miller.3 Add 0. 8. ASA and SSSA. related to element content.) Methods of soil analysis. Sparks (ed. Re-calibration is recommended when the daily factor is outside the range of 0. References Beaton. Mulvaney. Keeney (eds.R. Determination of sulphur in soils and plant material. . 5. and D. 1968. and J. and combustion behavior of the sample.. 1982. WI.2 A calibration that covers the desired working range of each element is performed. Agron. Changing the desorption temperature of adsorption columns can also require a re-calibration. detector or adsorption column) have been exchanged. Nitrogen .9 to 1. ASA and SSSA. 595-624. polynomial.001%. The sample weight is entered in the PC from an on-line electronic balance via an interface. Tech. Monogr. 11. WI.. In D.M. The Sulfur Inst. Washington. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. The test substances sulfanilic acid with each given element content and different weights is analyzed.05 g). 7. 1085 – 1121. The PC program automatically computes the calibration function (linear. 9. Part 3. air-dry soil sample is then packed in this tin foil. G.L. Calibration will typically remain stable for at least 6 months. DC. Page. Madison. J. 10. Chemical methods. oven-dry basis = C (%) instrument = Air-dry/oven-dry ratio (procedure 3D1) N (%) = Ni x AD/OD where: N (%) Ni AD/OD = N (%). James D. A quality control (QC) sample is performed at a minimum of every 35 to 40 samples. Chemical and microbiological properties. and placed into the carousel of the automatic sample feeder of elemental analyzer.Total.L. 351 . Burns.R. No. 14. 2nd ed.S. 1996. In A.H.100 to 0.) Methods of soil analysis. weighed (0. Sample weight is based on visual observation of the sample. Platou. Part 2. Bremmer. No. p. J.Elemental Analyzer Calibration and Analysis 7. An homogenized fine-grind. p. Madison. and C. R.M... Calculations C (%) = Ci x AD/OD where: C (%) Ci AD/OD = C (%).01% and total N to the nearest 0.

S. Application The pH of a water sample is a commonly performed determination and one of the most indicative measurements of water chemical properties. Soil Sci. WI. Soil taxonomy: A basic system of soil classification for making and interpreting soil surveys. Retention and fixation of ammonium and ammonia in soils.1 Syringe filters.S. Stevenson (ed.E. Govt. and K. D. 1987. Total carbon. p. J.) Nitrogen in agricultural soils.E.0. Washington. WI. 436.Broadbent.45-µm diameter. The soil organic fraction. J. ASA and SSSA. 1953.L. neutrality.W. Fisher Scientific 352 . 1883. J. In F.J. ASA and SSSA.. Office..) Methods of soil analysis. WI. Nommik. U. Anal. 5. 3. 2nd ed. WI. Young. 5. Madison. 961-1010. 1996. Agronomy 22. standard glass body combination. Tabatabai. Ground and Surface Water Analysis (4I) Reaction (4I1) Electrode (4I1a) Standard Glass Body Combination (4I1a1) Digital pH/Ion Meter (4I1a1a) pH (4I1a1a1) 1. Print. with caps 5. Stevenson (ed. 1982.. Govt. 1999. Soil survey laboratory methods manual. Sparks (ed. Fisher Scientific 5.3 Digital pH/ion meter. Rev. P.B. and organic matter.W. Agronomy 22. 3. Washington. Neue Methode zur Bestimmung des Stickstoffs in organischen Korpern. 22:366-382. DC. Glossary of soil science terms. ed. Sparks (ed. Phys. 0. 247:198-213. Chemical methods. or basicity is a key factor in the evaluation of water quality.L. No. ASA and SSSA. p. Follow standard laboratory safety practices. 1831. M. Version No.A. Accumet Model AR 15. Madison. In D. H. NJ 5. Am. Z.) Methods of soil analysis. F. 5. 50-mL. Print. Adv. In F.L. 123-171. 1996). Handb. 2. Chemical methods. 5:153-183. Ann. Summary of Method The pH of the water sample is measured with a calibrated combination electrode/digital pH meter (procedure 4I1a1a1). 921-960. p. Vahtras.A. Cliffton. Equipment 5. Dumas. Aldag. The acidity. No. 43-66. Part 3. In D. Inorganic forms of nitrogen in soil. Office. Nelson. USDA-NRCS Agric. 42. Chem. Chim. 1982. organic carbon. Soil Survey Staff. Procedes de l’analyse organique. 4. U. Agron.. Safety No significant hazards are associated with the procedure.4 Electrode. 1996. Madison. Accu-flow. Soil Science Society of America.2 Tubes. Part 3. Sommers. Whatman. Madison. ASA and SSSA. WI. and R. Soil Survey Staff. DC. Soil Survey Investigations Report No. Sulfur. 1996.J. Soc. Madison. and L. Interfernces Water pH needs to be measured immediately upon arrival at the laboratory in order to maintain optimal preservation of sample (Velthorst.) Nitrogen in agricultural soils. Kjeldahl. USDANRCS.

Record pH to the nearest 0.1 pH unit. Procedure 7. 2. 8. 1993).) Manual for soil and water analysis. Ground and Surface Water Analyses (4I) Electrical Conductivity and Salts (4I2) Conductivity Bridge and Cup (4I2a) Electrical Conductivity (4I2a1) 1. gently wash the electrode with RO water. pH 7.J.00. Analyze samples within 72 h. Summary of Method The electrical conductivity of the water sample is measured using an electronic bridge (4I2a1). and pH 9. A primary source of salts is chemical weathering of the minerals present in soils and rocks. Dry the electrode. but it is not in soils because salinity is significantly affected by the prevailing moisture content. Report Report the pH of the water sample to the nearest 0. with the most important including dissolution. 353 . 7. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 10.1 Reverse osmosis (RO) water. CA. Buurman. and 9. 9. 7. van Lagen. pH 4. 1996.6 Gently raise the pH electrode from the paste and wash the electrode with a stream of RO water.00. 7. Backhuys Publ. E.J.3 After equipment calibration. Fullerton. 11.00. Velthorst (eds.4 Gently lower the electrode in the water sample until the KCl junction of the electrode is beneath the water surface.18.00. References Velthorst. and oxidation-reduction (National Research Council.6. Calculations No calculations are required for this procedure. ASTM Type III grade of reagent water 6. 7. B. Do not wipe the electrode with a tissue as this may cause a static charge on the electrode. If extracts are not to be determined immediately after collection. and E.5 Allow the pH meter to stabilize before recording the pH. p. Water analysis. Beckman.2 Calibrate the pH meter with pH 4. hydrolysis. acidification.1 Water sample is filtered into a 50-mL tube. then store samples at 4° C. Reagents 6. for electrode calibration.2 Borax pH buffers. Leiden. Application Measuring electrical conductivity (EC) and total dissolved salts (TDS) is straightforward.18 buffer solutions. In P.01 unit. 7. 121-242. carbonation. 7. All of these reactions contribute to an increase in the dissolved mineral load in the soil solution and in waters. 7.

Equipment 5. Dissolve 0.4 Record conductance to 0. with automatic temperature adjustment. EC (mmhos cm-1) x 10 = Cation or Anion (meq L-1) 9. Analyze samples within 72 h. Calculations 8.7456 g of KCl in RODI water and bring to 1-L volume. Precision and Accuracy Precision and accuracy data are available from the SSL upon request.1 Syringe filters. then store samples at 4° C.3.1 Water sample is filtered into a 50-mL tube and capped. 7.1°C. Amber Science. NJ 5. Dry KCl overnight in oven (110°C). Procedure 7. 50-mL. ASTM Type III grade of reagent water 6. If extracts are not to be determined immediately after collection.412 mmhos cm-1.3 Read conductance of water sample directly from the bridge. 8. 4. Eugene. 0. Follow standard laboratory safety practices. 0.1 Reverse osmosis (RO) water. 25 ± 0. Cliffton. The extract temperature is assumed to be 25°C.1 No calculations are required for this procedure. Provide airtight storage of KCl solution and samples to prevent soil release of alkaliearth cations.2 Standardize the conductivity bridge using RO water (blank) and 0.2 Potassium chloride (KCl). 7. OR 6. Conductivity at 25°C is 1. If the temperature deviates significantly. Exposure to air can cause gains and losses of water and dissolved gases significantly affecting EC readings.2 Use the following relationship to estimate the total soluble cation or anion concentration (meq L-1) in the water. 7. Reagents 6. 354 .01 mmhos cm-1. 5. a correction may be required.45-µm diameter. 8. Whatman. 7.41 mmhos cm-1).010 N.01 mmhos cm-1 10. with caps 5. Markson Model 1056. Interferences Reverse osmosis water is used to zero and flush the conductivity cell.3 Conductivity bridge and conductivity cell.010 N KCl (1.2 Tubes. Report Report prediction conductance to the nearest 0. Safety No significant hazards are associated with this procedure.

11. References National Research Council. 1993. Soil and water quality. An agenda for agriculture. Natl. Acad. Press, Washington, DC.

Ground and Surface Water Analyses (4I) Electrical Conductivity and Salts (4I2) Atomic Absorption Spectrophotometer (4I2b) Calcium, Magnesium, Potassium, and Sodium (4I2b1-4)
1. Application Nutrients (nitrogen and phosphorus), sediments, pesticides, salts, or trace elements in ground and surface water affect soil and water quality (National Research Council, 1993). This procedure is developed for the analysis of ground or surface water. 2. Summary of Method The water sample is filtered and diluted with an ionization suppressant (La2O3). The analytes are measured by an atomic absorption spectrophotometer (AAS). The data are automatically recorded by a computer and printer. The saturation extracted cations, Ca2+, Mg2+, K+, and Na+ are reported in meq L-1 (mmol (+) L-1) in procedures 4I2b1-4, respectively. 3. Interferences There are four types of interferences (matrix, spectral, chemical, and ionization) in the analysis of these cations. These interferences vary in importance, depending upon the particular analyte selected. Do not use borosilicate tubes because of potential leaching of analytes. 4. Safety Wear protective clothing and eye protection. When preparing reagents, exercise special care. Restrict the use of concentrated HCl to a fume hood. Many metal salts are extremely toxic and may be fatal if ingested. Thoroughly wash hands after handling these metal salts. Follow standard laboratory procedures when handling compressed gases. Gas cylinders should be chained or bolted in an upright position. Acetylene is highly flammable. Avoid open flames and sparks. Standard laboratory equipment includes fire blankets and extinguishers for use when necessary. Follow the manufacturer's safety precautions when using the AAS. 5. Equipment 5.1 Electronic balance, ±1.0-mg sensitivity 5.2 Syringe filters, 0.45-µm diameter, Whatman , Cliffton, NJ 5.3 Tubes, 50-mL, with caps 5.4 Atomic absorption spectrophotometer (AAS), double-beam, AAnalyst 300, Perkin-Elmer Corp., Norwalk, CT 5.5 Autosampler, AS-90, Perkin-Elmer Corp., Norwalk, CT 5.6 Computer, with AA WinLab software, Perkin-Elmer Corp., Norwalk, CT, and printer 5.7 Single-stage regulator, acetylene 5.8 Digital diluter/dispenser, with syringes 10000 and 1000 µL, gas tight, MicroLab 500, Hamilton Co., Reno, NV 5.9 Plastic test tubes, 15-mL, 16 mm x 100, for sample dilution and sample changer 5.10 Containers, polyethylene 5.11 Peristaltic pump 6. Reagents 6.1 Reverse osmosis deionized (RODI) water, ASTM Type I grade of reagent water 6.2 Hydrochloric acid (HCl), concentrated 12 N

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6.3 6.4

6.5 6.6 6.7

6.8

HCl, 1:1 HCl:RODI, 6 N. Carefully mix 1 part of concentrated HCl to 1 part RODI water. Stock lanthanum ionization suppressant solution (SLISS), 65,000 mg L-1. Wet 152.4 g of lanthanum oxide (La2O3) with 100 mL RODI water. Slowly and cautiously add 500 mL of 6 N HCl to dissolve the La2O3. Cooling the solution is necessary. Dilute to 2 L with RODI water. Filter solution. Store in polyethylene container. Working lanthanum ionization suppressant solution (WLISS), 2000 mg L-1. Dilute 61.5 mL of SLISS with 1800 mL of RODI water (1:10). Make to 2-L volume with RODI water. Invert to mix thoroughly. Store in polyethylene container. Primary stock standards solution (PSSS), high purity, 1000 mg L-1: Ca, Mg, K, and Na. Working stock mixed standards solution (WSMSS) for Ca, Mg, and K. In a 500-mL volumetric flask, add 250 mL Ca PSSS, 25 mL Mg PSSS, and 100 mL K PSSS = 500 mg L-1 Ca, 50 mg L-1 Mg, and 200 mg L-1 K. Dilute to volume with RODI water. Invert to thoroughly mix. Store in polyethylene containers. Prepare fresh weekly. Store in the refrigerator. Mixed calibration standards solution (MCSS), High, Medium, Low, Very Low, and Blank as follows:

6.8.1 MCSS High Standard (1:100): Dilute WSMSS 1:100 with WLISS. Invert to mix thoroughly mix. Store in polyethylene containers. Prepare fresh weekly. Store in a refrigerator. Allow to equilibrate to room temperature before use. Final concentration = 5 mg L-1 Ca, 0.5 mg L-1 Mg, and 2 mg L-1 K. 6.8.2 MCSS Medium Standard (1:200): To a 100-mL volumetric flask, add 50 mL of WSMSS and bring to volume with RODI water. Dilute 1:100 with WLISS. Invert to thoroughly mix. Store in polyethylene containers. Prepare fresh weekly. Store in a refrigerator. Allow to equilibrate to room temperature before use. Final concentration =2.5 mg L-1 Ca, 0.25 mg L-1 Mg, and 1 mg L-1 K. 6.8.3 MCSS Low Standard (1:400): To a 100-mL volumetric flask, add 25 mL of WSMSS and bring to volume with RODI water. Dilute 1:100 with WLISS. Invert to mix thoroughly. Store in polyethylene containers. Prepare fresh weekly. Store in a refrigerator. Allow to equilibrate to room temperature before use. Final concentration = 1.25 mg L-1 Ca, 0.125 mg L-1 Mg, and 0.5 mg L-1 K. 6.8.4 MCSS Very Low Standard (1:600): To a 100-mL volumetric flask, add 16.65 mL of WSMSS and bring to volume with RODI water. Dilute 1:100 with WLISS. Invert to mix thoroughly. Store in polyethylene containers. Prepare fresh weekly. Store in a refrigerator. Allow to equilibrate to room temperature before use. Final concentration = 0.83 mg L-1 Ca, 0.08 mg L-1 Mg, and 0.33 mg L-1 K. 6.8.5 MCSS Blank = 0 mL of Ca, Mg, and K. Dilute RODI water 1:100 with WLISS. 6.9 Na Calibration Standards Solution (NaCSS), High, Medium, Low, and Very Low as follows:

6.9.1 NaCSS High Standard (1:100): Dilute Na PSMSS (1000 mg L-1) 1:100 with WLISS. Invert to thoroughly mix. Store in polyethylene containers. Prepare fresh weekly. Store in a refrigerator. Allow to equilibrate to room temperature before use. Final concentration = 10 mg L-1 Na. 6.9.2 NaCSS Medium Standard (1:200): In a 50-mL volumetric, add 25 mL of Na PSMSS and bring to volume with RODI water. Dilute 1:100 with WLISS. Invert to mix thoroughly.

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Store in polyethylene containers. Prepare fresh weekly. Store in a refrigerator. Allow to equilibrate to room temperature before use. Final concentration = 5 mg L-1 Na. 6.9.3 NaCSS Low Standard (1:400): In a 50-mL volumetric flask, add 12.5 mL of PSMSS and bring to volume with RODI water. Dilute 1:100 with WLISS. Invert to thoroughly mix. Store in polyethylene containers. Prepare fresh weekly. Store in a refrigerator. Allow to equilibrate to room temperature before use. Final concentration = 2.5 mg L-1 Na. 6.9.4 NaCSS Very Low Standard (1:600) In a 50-mL volumetric flask, add 8.35 mL of PSMSS Na (1000 ppm) and bring to volume with RODI water. Dilute 1:100 with WLISS. Invert to thoroughly mix. Store in polyethylene containers. Prepare fresh weekly. Store in a refrigerator. Allow to equilibrate before use. Final concentration = 1.67 mg L-1 Na. 6.9.5 NaCSS Blank = 0 mL Na PSMSS. Dilute RODI water 1:100 with WLISS. 6.10 Compressed air with water and oil traps. 6.11 Acetylene gas, purity 99.6%. 7. Procedure 7.1 Water sample is filtered into a 50-mL tube and capped. If extracts are not to be determined immediately after collection, then store samples at 4° C. Analyze samples within 72 h. Dilution of Calibration Standards and Sample Extracts 7.2 The 10-mL syringe is for diluent (WLISS). The 1-mL syringe is for the MCSS and water sample. Set the digital diluter at a 1:100 dilution. See Sections 6.8 and 6.9 for preparation of the MCSS and NaCSS. Dilute the saturation extract sample with 100 parts of WLISS (1:100). 7.3 Dispense the diluted sample solutions into test tubes which have been placed in the sample holders of the sample changer. AAS Set-up and Operation 7.4 Refer to the manufacturer's manual for operation of the AAS. The following are only very general guidelines for instrument conditions for the various analytes. Conc. Burner Wavelength Slit Fuel/Oxidant & angle (nm) (mm) (C2H2/Air) (mg L-1) ⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯⎯ Ca 5.0 10 cm @ 0° 422.7 0.7 1.5/0.0 Mg 0.5 10 cm @ 0° 285.2 0.7 1.5/10.0 K 2.0 10 cm @ 0° 766.5 0.7 1.5/10.0 Na 10.0 10 cm @ 30° 589.0 0.2 1.5/10.0 7.5 Use the computer and printer to set instrument parameters and to collect and record instrument readings. AAS Calibration and Analysis 7.6 Calibrate the instrument by using the MCSS and NaCSS. The data system will then associate the concentrations with the instrument responses fore each MCSS and NaCSS. Rejection criteria for MCSS and NaCSS, if R2 <0.99. 7.7 If sample exceeds calibration standard, the sample is diluted 1:5, 1:20, 1:100, etc., with RODI water followed by 1:100 dilution with WLISS.
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Analyte

7.8 Perform one quality control (QC) (Low Standard) for every 12 samples. If reading is not within 10%, the instrument is re-calibrated and QC re-analyzed. 7.9 Record analyte readings to 0.01 mg L-1. 8. Calculations The instrument readings for analyte concentration are in mg L-1. These analyte concentrations are converted to meq L-1 as follows: Analyte Concentration in Soil (meq L-1) = (A x B)/C where: A = Analyte (Ca, Mg, K, Na) concentration in extract (mg L-1) B = Dilution ratio, if needed C = Equivalent weight where: Ca+2 = 20.04 mg meq-1 Mg+2 = 12.15 mg meq-1 K+1 = 39.10 mg meq-1 Na+1 = 22.99 mg meq-1 9. Report Report the saturation extraction cations of Ca2+, Mg2+, K+, and Na+ to the nearest 0.1 -1 meq L (mmol (+) L-1). 10. Precision and Accuracy Precision and accuracy data are available from the SSL upon request. 11. References National Research Council. 1993. Soil and water quality. An agenda for agriculture. Natl. Acad. Press, Washington, DC.

Ground and Surface Water Analyses (4I) Electrical Conductivity and Salts (4I2) Ion Chromatograph (4I2c) Conductivity Detector (4I2c1) Self-Regeneration Suppressor (4I2c1a) Bromide, Acetate, Chloride, Fluoride, Nitrate, Nitrite, Phosphate, and Sulfate (4I2c1a1-8)
1. Application Nutrients (nitrogen and phosphorus), sediments, pesticides, salts, or trace elements in ground and surface water affect soil and water quality (National Research Council, 1993). This procedure is developed for the analysis of ground or surface water. 2. Summary of Method The water sample is filtered and is diluted according to its electrical conductivity (ECs). The diluted sample is injected into the ion chromatograph, and the anions are separated. A conductivity detector is used to measure the anion species and content. Standard anion concentrations are used to calibrate the system. A calibration curve is determined, and the anion concentrations are calculated. A computer program automates these actions. The water
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anions, Br-, CH3COO-, Cl-, F-, NO3-, NO2-, PO43-, SO42- are reported in meq L-1 (mmol (-) L-1) by procedure 4I2c1a1-8, respectively. 3. Interferences Some water samples contain suspended solids and require filtering. Low molecular weight organic anions will co-elute with inorganic anions from the column. 4. Safety Wear protective clothing and safety glasses. When preparing reagents, exercise special care. Many metal salts are extremely toxic and may be fatal if ingested. Thoroughly wash hands after handling these metal salts. Follow the manufacturer's safety precautions when using the chromatograph. 5. Equipment 5.1 Syringe filters, 0.45-µm diameter, Whatman, Cliffton, NJ 5.2 Tubes, 50-mL, with caps 5.3 Guard column, IonPac AG14, 4 x 50 mm, Dionex Corp., Sunnyvale, CA 5.4 Analytical column, IonPac AS14, 4 x 250 mm, Dionex Corp., Sunnyvale, CA 5.5 Self-regeneration suppressor, ASRS – ULTRA, 4 mm, Dionex Corp., Sunnyvale, CA 5.6 Autosampler, AS40, Dionex Corp., Sunnyvale, CA 5.7 Computer with PeakNet software and printer 5.8 Digital diluter/dispenser, with syringes 10000 and 1000 µL, gas tight, MicroLab 500, Hamilton Co., Reno, NV 5.9 Poly-vials with caps, 5 mL, Dionex Corp., Sunnyvale, CA 6. Reagents 6.1 Reverse osmosis deionized filtered (RODI), ASTM Type I grade of reagent water 6.2 Helium gas 6.3 Eluent solution. Solution A: Mix 5.30 g of Na2CO3 with RODI water in a 500-mL volumetric and make to volume with RODI water. Solution B: Mix 4.20 g of NaHCO3 with RODI water in a 500-mL volumetric and make to volume with RODI water. Add 35 mL of Solution A and 10 mL of Solution B in a 1-L volumetric and make to volume with RODI water for a final concentration is 0.024 M Na2CO3 and 0.025 M NaHCO3. Make 2 L of eluent solution if chromatograph is to run overnight. Place eluent in eluent tank and degas with helium 15 min L-1 eluent (30 min total). Make fresh daily. 6.4 Primary stock standards solutions, (PSSS1000), high purity, 1000 mg L-1: Cl-, SO42-, F-, NO3-, NO2-, Br-, CH3COO-, and PO43-. 6.5 Primary stock standards solutions (PSSS100), 100 mg L-1: F-, NO3-, NO2-, Br-, and PO43-. Prepare fresh weekly. In five 250-mL volumetric flasks add as follows: 6.5.1 6.5.2 6.5.3 6.5.4 6.5.5 F- PSSS100 = 25 mL F- PSSS1000 Br- PSSS100 = 25 mL Br- PSSS1000 NO2- PSSS100 = 25 mL NO2- PSSS1000 NO3- PSSS100 = 25 mL NO3- PSSS1000 PO43- PSSS100 = 25 mL PO43- PSSS1000

Dilute each PSSS100 to volume with RODI water and invert to thoroughly mix. Store in the refrigerator. 6.6 Mixed calibration standards solutions (MCSS), A, B, C, D, E, and Blank as follows: 6.6.1 MCSSA = In a 250-mL volumetric flask, add as follows

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12.5 mL Cl- PSSS1000 = 50 mg L-1 25 mL SO42 PSSS1000 = 100 mg L-1 12.5 mL F- PSSS100 = 5 mg L-1 20 mL NO3- PSSS100 = 8 mg L-1 20 mL NO2- PSSS100 = 8 mg L-1 22 mL Br- PSSS100 = 8.8 mg L-1 20 mL CH3COO- PSSS1000 = 80 mg L-1 24 mL PO43- PSSS100 = 9.6 mg L-1 Dilute to volume with RODI water and invert to thoroughly mix. Store in glass containers. Store in the refrigerator. Prepare fresh weekly. 6.6.2 MCSSB = In a 100-mL volumetric flask, add 40 mL MCSSA and dilute to volume with RODI water. Final concentration = 20, 40, 2, 3.2, 3.2, 3.52, 30.4, and 3.52 mg L-1 Cl-, SO42-, F-, NO3-, NO2-, Br-, CH3COO-, and PO43-, respectively. Invert to thoroughly mix. Store in glass containers. Prepare fresh weekly. Store in the refrigerator. 6.6.3 MCSSC = In a 100-mL volumetric flask, add 20 mL MCSSA and dilute to volume with RODI water. Final concentration = 10, 20, 1, 1.6, 1.6, 1.76, 15.2, and 1.76 mg L-1 Cl-, SO42-, F-, NO3-, NO2-, Br-, CH3COO-, and PO43-, respectively. Invert to thoroughly mix. Store in glass containers. Prepare fresh weekly. Store in the refrigerator. 6.6.4 MCSSD = In a 250-mL volumetric flask, add 25 mL MCSSA and dilute to volume with RODI water. Invert to thoroughly mix. Final concentration = 5, 10, 0.5, 0.8, 0.8, 0.88, 7.6, and 0.88 mg L-1 Cl-, SO42-, F- , NO3-, NO2-, Br-, CH3COO-, and PO43-, respectively. Store in glass containers. Prepare fresh weekly. Store in the refrigerator. 6.6.5 MCSSE = In a 250-mL volumetric flask, add