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West Conshohocken. United States 1 . and Hydrated Lime to Terminology E456.2 The values stated in SI units are to be regarded as the standard. in the case of revision. 1. A number in parentheses indicates the year of last reapproval. or whether the perfor- 2 For referenced ASTM] @ 2015-04-01 Designation: C1271 − 99 (Reapproved 2012) Standard Test Method for X-ray Spectrometric Analysis of Lime and Limestone1 This standard is issued under the fixed designation on Chemical Tests. ANSI-NIST Handbook 114 NIST Standards Catalog 1.astm. No further reproduction or distribution permitted.2 lime—unless otherwise specified.1 This test method covers the X-ray emission spectromet.1 A briquetted powder specimen or a fused-glass disk by the Industry) specimen is irradiated by a high-energy X-ray beam. C50 Practice for Sampling. E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method 5. http://www. It provides rapid. Ores. Gaithersburg. MD 20899-1070. Terminology 1. for definitions of terms used in this test method pertaining to lime. PA 19428-2959. multi-element determinations with sufficient accuracy to 1 This test method is under the jurisdiction of ASTM Committee C07 on Lime ensure product quality and minimize production delays. Packaging. 3 4 The last approved version of this historical standard is referenced on Available from National Institute of Standards and Technology (NIST). the year of last revision. contact ASTM Customer Service at service@astm.1 This procedure is suitable for manufacturing control and cal Methods of Analysis (Withdrawn 1997)3 verifying that the product meets specifications. associated with its use. Bureau Dr. 1. 2. and and the intensities are measured by suitable detectors at Related Materials selected Stop 1070. Reagents. Originally approved in 1994. www.3 This standard does not purport to address all of the 3. Specific precau- tionary statements are given in Section 10. 3.1. refer Quicklime. responsibility of the user of this standard to establish appro- for definitions of terms used in this test method pertaining to priate safety and health practices and determine the applica- emission spectroscopy. For Annual Book of ASTM Standards volume information. bility of regulatory limitations prior to use. analytical performance data included may be used as a bench- Current edition approved Dec. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval. 2. Published December 2012.1. and Related Materials fixed time. PO Box C700.1 Definitions: safety concerns.. secondary X rays produced are dispersed by means of crystals. Summary of Test Method C51 Terminology Relating to Lime and Limestone (as used 4. 100 Barr Harbor Drive.2 NIST Documents:4 draulic lime using wavelength dispersive instruments. or integration of voltage for a fixed time. Referenced Documents Terminology C51. hydrated lime.1520/C1271-99R12. or mance of a particular X-ray spectrometer has changed. Significance and Use E1060 Practice for Interlaboratory Testing of Spectrochemi- 5. and Marking of Lime and Limestone Products 4. visit the ASTM and Safety Consid. 2012. 100 www.3 statistical—unless otherwise specified. of terms used in this test method pertaining to statistics.1 ASTM Standards:2 3. quicklime. refer to Terminology E135.1. Ores. Sample Preparation. The and is the direct responsibility of Subcommittee C07. refer to 2. vide equivalent precision and accuracy. X-Ray Spectrometric Analysis ric analysis of limestone. if any. refer to the standard’s Document Summary page on the ASTM website.nist. Printed / viewed by: [ for definitions C25 Test Methods for Chemical Analysis of Limestone. and hy.brochero@sgs. It is the 3. Data are collected based on the time E135 Terminology Relating to Analytical Chemistry for required to reach a fixed number of counts. Copyrighted material licensed to SGS SA. 3. erations for Chemical Analysis of Metals. Last previous edition approved in 2006 as C1271 – 99 (2006).1 emission spectroscopy—unless otherwise specified. mark to determine whether similar X-ray spectrometers pro- DOI: 10. Copyright © ASTM International. The E50 Practices for Apparatus. Concen- E305 Practice for Establishing and Controlling Atomic trations of the elements are determined by relating the mea- Emission Spectrochemical Analytical Curves sured radiation of unknown specimens to analytical curves E456 Terminology Relating to Quality and Statistics prepared from reference materials of known composition. Scope E1361 Guide for Correction of Interelement Effects in 1. the number immediately following the designation indicates the year of original adoption or. total count for a Metals.

Copyrighted material licensed to SGS SA. ger counters. The 6. may be required to provide more accurate measurements for some measurements. or integrated voltages may be 7. below 20). As a general rule.4 Excitation Source: 9. 7.1 Interelement effects or matrix effects may exist for some generator may be equipped with a line voltage regulator and of the elements listed.4 Spectral interferences from the X-ray tube may also pump.1 Analyzing Crystals—Flat or curved crystals with op- lyzed by this test method. The counts. with a flat bottom 30 to 35 reproducible fashion in the melt.3.4.3 Contamination from the grinding apparatus is an ever. elements. usually 13 Pa or less. 95 % platinum/5 % dispersing the analyzed elements in an homogeneous and gold alloy. The press shall be equipped with a mold assembly that provides a briquet compatible with the 8.2 Fusion Crucibles: be present in the analytical sample as in the reference materials 7. equipped for vacuum operation.3 Polishing Wheel.1. the sample to binder ratio must 7. consisting of a mixture of 90 % to obtain a uniform surface for irradiation.4 Vacuum System. Pulse height analyzers grinding containers and timer control for final grinding. with targets of various high-purity designated concentration ranges.6 Measuring System.3). equipped with specimen holders and a specimen chamber. 7. gage. The flux must be capable of dissolving or 7. or integrated voltages can also be rotating disk for further grinding.1 Certified reference materials are available from the tial or rectified power of sufficient energy to produce secondary National Institute for Standards and Technology (NIST) and 2 . 7. capable of providing pressures up 8.1 Furnace or Gas Burners. for limiting the characteristic X rays to a Orders of all wavelengths may cause interference. 7. and electrical controls to provide automatic occur.4 Detector Gas (P-10). 95 % platinum/5 % gold alloy. scintillation counters or equivalent. count rate. Apparatus pable of counting or integrating pulses received from the 7.2 Collimator. determined.3. recorders. The analyst must be aware of all timized capability for diffraction of the wavelengths of interest. possible interferences and matrix effects of this element.3. digital counters. 20 to 30-mL capacity. 7. parallel bundle when flat crystals are used in the instrument. A the effect of CaKβ1 (2nd order) on PKα1.1 Purity and Concentration of Reagents—The purity and X-ray specimen holder.2 Plate Grinder or Pulverizer. proportional type. collimator is not necessary for curved crystal optics. for example.3 Detectors.2 Binders—Various binders have been used successfully heating the sample and flux to at least 1000 °C and homog. 6. may be used alterna.5. the binder should not contain an element that will be determined.1 X-Ray Tube Power Supply. Interferences radiation of the specimen for the elements specified.3. prepare fusion disks.5.5. 7.2 Calcium is the primary component of the matrix ana. The analyst should argon and 10 % methane for use with gas flow proportional be aware at all times of possible contamination from the counters only.4. The system shall consist of at least one vacuum 6.2 X-Ray Tubes. providing for the determination of be cognizant. No further reproduction or distribution permitted. 30 to 8. Reference Materials 7.3 Platinum/Gold Casting Dish. The prepared disks must then mm in diameter. suitable for polishing the fusion disk 8. sealed or gas flow. present source of interference of which the analyst must always 7. elements whose radiation is absorbed by air (atomic number chrome. providing that the analytical chamber may contain a specimen spinner. consisting of electronic circuits ca- 7. enizing the melt. 30 to 35-mL capacity. and nickel to the prepared sample. capable of 8. Mathematical corrections.1 Jaw Crusher. designed for X-ray emission analysis and or fundamental parameter calculations.2. derived from empirical relationships 7. The tively.3. concentration of chemical reagents shall conform to the re- quirements prescribed in Practices E50.2.1 Briquetting Press. For example. pressure. for initial crushing of lumps. with a flat bottom 30 to 35 mm in diameter. Reagents and Materials to 550 MPa (80 000 psi).3. In addition. with a timer. or] @ 2015-04-01 C1271 − 99 (2012) 6. and that will excite the elements to be reference materials used to prepare the calibration curve. providing constant poten.1 Vitreous Carbon or Graphite.3 Fusion Equipment: 7. stainless steel will impart iron.5. One way to compensate for these effects current stabilizer.1 Specimen Preparation Equipment: detectors. with hardened conversion to percent concentration. capable of continuous operation at required poten- men being analyzed must match closely the composition of the tials and currents.5 Spectrometer. with one static and one The counts. polishing media used for surfacing the disk (6.3 Fluxes—Various fluxes have been used successfully to 35-mL capacity. displayed on meters. to prepare briquettes suitable for presentation to the instrument.2. 7. presented to a computer or programmable calculator for 7. for example. 7. Printed / viewed by: [maribel. line overlap from CrKβ1 on MnKα1 pumpdown of the optical path and maintain a controlled caused by a chrome target tube. 7. The composition of the speci.1. be suitable for presentation to the instrument. Any of these are acceptable.2. 7. that were used to establish the calibration.1. Gei- 6.3 Rotary Disk Mill or Shatter Box.brochero@sgs.2 Platinum/Gold.2 Briquetting Equipment: 7. is to prepare a series of calibration curves to cover the 7. count rates. 9. and it must be accuracy required by this test method is achieved.

count rate is obtainable only after unacceptable long counting 10. 15. Alternate wavelengths without interference may be used. laps. Either fixed count survey record.4 Special precautions for operators and maintenance times for lime materials.1 Gross sample is to be taken in accordance with interferences. 10. Safety Precautions element in the reference materials. using the parameters 3 . with the exception of the major oxides personnel shall be posted at the equipment site. Titanium 2. RAP. RAP.3 Special preparation may be required to grind the Sodium 11. 10. LiF 220 with the manufacturer’s instructions. Select a sufficient number of reference materials to cover the concentration ranges of the elements sought. PET.91 TLAP.2 Reference materials with matrixes similar to that of the 14. Printed / viewed by: [maribel. PET Specimens Sulfur 5. EDdT.775 LiF 200. Drift is indicated by tenance personnel follow the guidelines of safe operating a change in counts that exceeds the normal variation of counts procedures given in current handbooks and publications from for that element. TLAP. the radiation survey record. Element Wavelength. verify that acceptable analyses are obtained after the adjust- ments are made. Refer to Test Meth.126 PET.359 LiF 200. parameters closely to ensure repeatable analyses. Once established. and estab- be used to create standards for which appropriate reference lish a calibration curve for each element in accordance with materials are not available for an element desired to be Practice E305.8766 LiF 200. Preparation of Apparatus Strontium 0. 15. using care not to contaminate the surface to be Periodic radiation surveys of the equipment for leaks and excited.2 Standardization (Analytical Curve Adjustment)— radiation shall be observed at all X-ray emission spectrometer Verify that the calibration curve for each element has not installations. and Mg). Establish the curve by a least squares or analyzed.] @ 2015-04-01 C1271 − 99 (2012) other international certification agencies. PET same way throughout the procedure.750 LiF 200. The personal film badge counting rate measurement for each element. 15.2 Sample preparation is to be performed in accordance TABLE 1 Analytical Lines and Crystals with Methods C50 and Test Methods C25. EDdT.3 Standard additions method or spiked samples may also intensity measurements of each reference material. Copyrighted material licensed to SGS SA.338 PET. Fe.6 Fail-Safe “X-ray on” warning lights shall be used on will not resolve radiation completely from several line over- the equipment.937 LiF 200.175 LiF 200. Ge 12. RAP Silicon 7.1 Treat reference materials and specimens exactly the Potassium 3.1 Calibration (Preparation of Analytical Curves)— analyzed in accordance with ASTM standard test methods. A change of 1 % or greater usually signifies the original equipment manufacturer. chamber. and federal radiation standards.155 Ge. Otherwise. and an equipment or fixed time modes may be used.S.103 LiF 200.brochero@sgs. 11. A minimum counting time of 60 s is 10.373 Ge. LiF 220 Manganese 2.3 Monitoring Devices—Either film badges or dosimeters 15. LiF 220 13. Re-measure the reference materials to NIST Standards Catalog and ANSI-NIST Handbook 114. Government that the calibration curve for that element has drifted and Printing Office. (Si. person using an ionization chamber detector to meet local.2 Personnel—X-ray equipment shall be used only under the guidance and supervision of a responsible. Preparation of Reference Materials and Test Phosphorus 6. drifted using a control reference material. LiF 220 Iron 1.889 ADP.742 LiF 200. versus the corresponding weight percent concentrations of the 10. InSb 12.2 Radiation Measurements—Obtain and record the state. Al.3 Spectral Interferences—Some X-ray spectrometers 10.1 Occupational health and safety standards for ionizing 14. NIST. See should thus be adjusted. Procedure 10. given in Table 1. 9.729 PET. A Crystals 11. or similar handbooks on radiation safety. No further reproduction or distribution permitted.2. LiF 220 Barium 2. multilayer analytical sample finer than is required in 11. control all instrument ods C25 for a current listing. LiF 220 13. Average duplicate 9. Either briquetted powder Calcium 3.1 Excitation—Introduce the specimen into the specimen shall be worn by all operating and maintenance personnel. multilayer Aluminum 8. The matrix material must match that of the test multiple regression fit of the X-ray intensity measurements specimen. Care must therefore be exercised in these cases. Produce the secondary fluorescence using the equip- excessive scattered radiation shall be made by a qualified ment used in 7. Calibration and Standardization test specimen and containing varying amounts of the elements to be determined may be used provided that they have been 14. 11. Methods C50. Magnesium 9. Sampling mathematical calculations must be used to correct for the 11. It is also recommended that operating and main.5 Radiation caution signs shall be posted near the X-ray acceptable. Ca.1 Prepare and operate the spectrometer in accordance Lead 1. qualified person. PET or fused disk specimens may be used. NaCl Chlorine 4. A predetermined minimum maintenance record shall be available upon request. equipment and at all entrances to the radiation area.

683 0. 17.156 0. analyzing more than one specimen.0021 0.032 0.401 0. 17. calculated results are usually printed without operator X-ray spectrometer is not improved significantly by making involvement.356 1. Refer to the 18.2 If mathematical corrections must be made to correct with Practice E1060 are included in the annex.359 0.0359 0.133 S-1142 0.015 0.2 Precision—The relative precision of this test S-1143 55.0244 0. Printed / viewed by: [maribel.599 0.0050 0.0111 0.1.028 0. S-1145 0.150 0.0064 0.3.010 0.048 0. 15. Confi- tested this test method in accordance with Practice E1060.0259 0.138 0.1 chemical analysis.0436 A1.875 0.2 Reproducibility (R2)—Calculations for between- 16. was conducted in 1997. No further reproduction or distribution permitted.071 0.1 Repeatability (R1)—Calculations for within- 16.0062 0.4404 0.0036 0.009 0. HIGH CALCIUM LIMESTONE BY THE BRIQUETTE METHOD A1.0102 0.2 Iron as % Ferric Oxide (% Fe2O3): 4 .637 0.1159 0.054 0.1917 0.406 0.216 0.1 Round Robin—An interlaboratory study.067 Material Average Sr SR r R S-1142 0.0168 0.298 S-1145 0.284 0.3 Aluminum as % Aluminum Oxide (% A12O3): Material Average Sr SR r R A1.1142 0. Periodic checks to to Guide E1361 for a guide to interelement corrections.428 0.794 method.0899 A1.1 Summary of Test Method: Material Average Sr SR r R S-1143 0. S-1141 53.0924 S-1142 0.0173 S-1142 0.5 Magnesium as % Magnesium Oxide (% MgO): ibility (SR and R) has been determined for the materials and Material Average Sr SR r R elements to be: S-1143 0.0015 0.0058 0.3 Precision and Bias: S-1141 0.0067 0.0083 0.106 0.2. consistent A1.2. Calculation of Results laboratory precision are listed in the annex.371 0.0924 S-1144 0. however.0042 0. hydraulic lime.4 Replicate Measurements—Make a minimum of two NOTE 2—With computer-controlled X-ray spectrometers that convert output signals automatically to percent concentrations and make interele- measurements on each test specimen.049 0. characterized by repeatability (Sr and r) and reproduc.0188 limestone is prepared and irradiated as directed in Test Method S-1141 0.2.091 0. X-ray spectrometric ANNEX (Mandatory Information) A1.8792 0.0736 S-1141 1. Computers are normally interfaced to the X-ray spec. for those elements not having sufficient 17.brochero@sgs.143 0.1.085 0. any one of a number of correction procedures may be used.021 0.012 0.0156 0.0018 0.1 Determine the concentration of the various elements laboratory precision are listed in the annex.039 A1. S-1144 0.0321 0. Copyrighted material licensed to SGS SA.238 A1.006 0.1244 A1. multiple measurements on the same surface of the same specimen.446 1.0330 0.017 0. Keywords equipment manufacturer’s manual for the instrument being 18.176 0.006 S-1145 55. the statistics near the 17. Material Average Sr SR r R Five high calcium limestone materials were analyzed by eight S-1144 53.4 Calcium as % Calcium Oxide (% CaO): with the guidelines of Practice E691.2.421 0.237 S-1144 0.127 0.627 0. lime- used. hydrated lime. dence in the accuracy of analysis will also improve by Precision data are provided in the annex.1087 A1. verify the setting are advisable.866 0. stone.110 0.034 0. wavelength dispersive.084 0. the setting for the 2 θ peak must be trometers in laboratories using such correction] @ 2015-04-01 C1271 − 99 (2012) NOTE 1—If a goniometer is used.295 0.026 0.3.347 0.011 0.039 0.174 0.026 0.2. A1.070 0.0330 0.0013 0.0040 0.3.1 Silicon as % Silicon Dioxide (% SiO2): S-1145 0.234 S-1144 1.0457 0.1 Precision—An acceptable number of laboratories detection limit will improve with multiple exposures.826 laboratories performing replicate measurements on four bri.2.254 A1.0444 0.2 Bias (Accuracy)—Bias data calculated in accordance 16.1357 0.837 0.0388 0.304 0.062 0.0463 0.0038 0.1 There are no special provisions in the test method S-1143 0.0724 that are not referred to in Test Method C1271.307 1.197 S-1141 0.0030 0.024 0.0023 0.0383 0.159 0.2 Provisions : A1.0469 C1271.919 0. the concentrations for interelement effects.0137 0. Precision and Bias counts in the predetermined time. 17.3.007 0. Refer determined experimentally within each laboratory. S-1142 54. quicklime.042 0.109 S-1143 0. using the radiation measurements for the test specimen and the appropriate analytical curves.1.085 0.199 quettes. The performance of an ment corrections.022 0.3.0163 0.1 A briquetted powder specimen of high calcium S-1145 0.

0248 0.0411 x where: x is the average of test results.973 Magnesium as % Magnesium Oxide (% MgO) 0.0009 0.0128 using samples taken at random from a single sample prepared S-1141 0.0027 method.3. ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard.0015 + 0. carried out in different laboratories S-1142 0.0016 0.0751 x calibration of this test method.588 x Silicon as % Silicon Dioxide (% SiO2) 0.0036 0.0003 0.0024 0. 5 .astm.0004 0. at the address shown below.95 Aluminum as % Aluminum Oxide (% Al2O3) 0. Printed / viewed by: [maribel. in the same Silicon as % Silicon Dioxide (% SiO2) 0.5 Bias—Certified reference materials are used for the Magnesium as % Magnesium Oxide (% MgO) 0. may Iron as % Ferric Oxide (% Fe2O3)] @ 2015-04-01 C1271 − 99 (2012) A1.95 (95 % confidence level).0101 0.0059 S-1144 0. This standard is copyrighted by ASTM International. The repeatability limit for this test Calcium as % Calcium Oxide (% CaO) 0. Your comments will receive careful consideration at a meeting of the responsible technical committee. No bias is expected for the Manganese as % Manganese (% Mn) 0. or through the ASTM website (www.0015 0. The reproducibility limit for this tween test results of the averages of two briquettes of the same test method is the following: sample. which you may attend.astm.1781 + 0.3 Repeatability—The difference in absolute value be- 0. 100 Barr Harbor Drive. Copyrighted material licensed to SGS SA.0046 0.0011 0.081 x Iron as % Ferric Oxide (% Fe2O3) 0.0007 0. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM International Headquarters. PA 19428-2959.brochero@sgs.0009 0. may be expected to occur with a probability of approximately A1.1038 x Calcium as % Calcium Oxide (% CaO) 0.0900 0.0021 0. West Conshohocken.0003 0.6 Manganese as % Manganese (% Mn): where: x is the average of test results from two briquettes.0227 + 0.386 A1.0170 0.0768 + 0. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised. Permission rights to photocopy the standard may also be secured from the ASTM website (www.4 Reproducibility—The difference in absolute value of S-1143 0. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above address or at 610-832-9585 (phone).0035 0.109 + 0. and the risk of infringement of such rights.0003 0. carried out separately and consecutively. either reapproved or withdrawn.0174 x method is the following: Manganese as % Manganese (% Mn) 0.3. or service@astm. Aluminum as % Aluminum Oxide (% Al2O3) 0. PO Box COPYRIGHT/).0963 x be expected to occur with a probability of approximately 0. United States.093 x laboratory by the same operator using the same apparatus.0044 A1.2.3. No further reproduction or distribution permitted.009 + 0. Users of this standard are expressly advised that determination of the validity of any such patent rights. 610-832-9555 (fax).1104 x (95 % confidence level). Material Average Sr SR r R S-1145 If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards.0550 from the same bulk sample after the last stage of reduction.0196 0.0041 replicate (e-mail). are entirely their own responsibility.

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