310 KALRA: JOURNAL OF AOAC INTERNATIONAL VOL. 78, No.

2, 1995

AGRICULTURAL MATERIALS

Determination of pH of Soils by Different Methods:

Collaborative Study

YASH P. KALRA
Canadian Forest Service, 5320-122 St, Edmonton, AB, T6H 3S5, Canada

Collaborators: H.P. Agrawal; E. Allen; J. Ashworth; P. Audesse; v.w. Case; D. Collins; S.M. Combs; C. Dawson; J. Denning;
SJ. Donohue; B. Douglas; B.G. Drought; M.A. Flock; J.B. Friedericks; GJ. Gascho; Z. Gerstl; L. Hodgins; B. Hopkins; D.
Horneck; R.A. Isaac; P.M. Kelly; J. Konwicki; J. Kovar; G. Kowalenko; G. Lutwick; R.O. Miller; R. Munter; I. Murchison; A.
Neary; R. Neumann; M. Neville; c.B. Nolan; R. Olive; W. Pask; L. Pastorek; T.R. Peck; T. Peel; J. Ramakers; W.S. Reid; V.
Rodd; R. Schultz; R. Simard; R.S. Singh; J. Sorrels; M. Sullivan; S. Tran; D. Trenholm; J. Trush; M.R. Tucker; E. Turcotte; A.
Van Niekerk; P.N. Vijan; J. Villanueva; C. Wang; D.D. Warncke; M.E. Watson; L. Wikoff; P. Yeung

Fifty-three laboratories (including author's) from
Canada,India,Israel,and the United States partici
pated in a collaborative study for the measurement
of pH of different types of soils. A method with 2 al
ternative procedures was used for pH measure
ments of mineral soils (alternative I for soils
containing less than 17x organic carbon and alter
native II for soils with variable salt content),a sec
ond method was used for saline-sodic soils,and a
third method was used for organic soils (soils con
taining at least 17x organic carbon). The pH was
measured potentiometrically. The methods were se
lected by the Soil Science Society of America,S889
Committee on Coordination of Official Methods of
Soil Analysis. Each laboratory used all 4 proce
dures to analyze 10 blind duplicate samples per
procedure. The repeatability relative standard de
viation values (RSDr) were 1.45-7.80% for mineral
soils tested by the alternative I,0.95-6.91% for min
erai soils tested by the alternative II,0.74-7.09% for
saline-sodic soils,and 0.73-4.66% for organic
soils. The corresponding reproducibility relative
standard deviation (RSDR) values were 2.67-
10.75%,2.03-7.54%,2.45-9.93%,and 2.15-6.32%.
Repeatability and reproducibility data indicated that
the resuHs are within acceptable levels. The 3 meth
ods for pH measurements of mineral,saline-sodic,
and organic soils were adopted first action by
AOAC INTERNATIONAL.
Submitted for publication July 12, 1994.
The recommendation was approved by the Committee on Feeds,
Fertilizers and Agricultural Related Topics, and was adopted by the Official
Methods Board of the Association. See "Official Methods Board Actions"
(1994) J. AOAC Int. 77, 203A, and "Official Methods Board Actions"
(1994) The Referee 18, October issue.
efore 1990, none of the methods used for soils analyses
B had been validated by AOAC INTERNATIONAL. In
1990, the Soil Science Society of America (SSSA) and
AOAC INTERNATIONAL decided to conduct collaborative
studies of soils methods. The first methods chosen for valida
tion were for pH measurements, since pH is one of the most
important properties of soils.
The pH of mineral soils is normally determined in a 1:1
soil-to-water mixture (1). Schofield and Taylor (2) suggested
the use of CaCl2 solution for mineral soils to minimize interfer
ences from suspension effects (due to particles suspended in
the soil-solution mixture) and variable salt content. The recom
mendations for management of saline-sodic soils are related to
pH values obtained with the saturated paste method (3, 4). The
results by the saturated paste methods were obtained during
over 30 years' work by the U.S. Department of Agriculture Sa
linity Laboratory and other research laboratories. For organic
soils, a 1:4 soil-to-water mixture is recommended (5).
Collaborative Study
Fifty-three laboratories from Canada, India, Israel, and the
United States participated in this collaborative study. To make
the methods as widely applicable as possible, a broad range of
soils differing in pH, texture, organic matter, and other proper
ties, was selected. Descriptions of soils used in the study are
presented in the Appendix.
Copies of the protocol including methods and data sheets
were sent to the participants in September 1992. Eighty heat
sealed plastic bags containing the appropriate amounts of well
mixed representative soil samples (20 g for the method used for
mineral soils [lOg for each alternative], 50 g for the method for
saline-sodic soils, and 5 g for the method used for organic soils)
were mailed to each of the participants by Fred Kaisaki from
the National Soil Survey Laboratory, U.S. Department of Ag
riculture, Lincoln, NE, on October 1, 1992.
 KALRA: JOURNAL OF AOAC INTERNATIONAL VOL. 78, No.2, 1995 311

Table 1. Soils used in the collaborative study for pH measurementsB

Sample No. Soil Sample No. Soil Sample No. Soil Sample No. Soil

1-1 Malbis HI Laurentides 1-111 Houston 21-IV Peck 90-9

2-1 Peck 90-9 2-11 Peck 90-11 2-111 Houston 22-IV Peck 90-10
3-1 Peck 90-12 3-11 Houston 3-111 Peck 90-12 23-IV Peck 90-11
4-1 Saline soil 4-11 Peck 90-12 4-111 Halii 24-IV Peck 90-9
5-1 Peck 90-11 5-11 Peck 90-11 5-111 Peck 90-11 25-IV Houghton Oa3
6-1 Halii 6-11 Peck 90-12 6-111 Peck 90-10 26-IV Houghton Oa4
7-1 Peck 90-10 7-11 Myakka 7-111 Myakka 27-IV Peck 90-12
8-1 . Myakka 8-11 Malbis 8-111 Peck 90-12 28-IV Houghton Oa3
9-1 Halii 9-11 Peck 90-10 9-111 Peck 90-11 29-IV Houghton Oa5
10-1 Laurentides 10-11 Halii 10-111 Peck 90-9 30-IV Houghton Oa2
11-1 Peck 90-10 1HI Peck 90-10 11-111 Saline Soil 31-IV Peck 90-12
12-1 Saline Soil 12-11 Myakka 12-111 Peck 90-10 32-IV Houghton Oa5
13-1 Peck 90-11 13-11 Halii 13-111 Saline soil 33-IV Laurentides LFH
14-1 Peck 90-9 14-11 Peck 90-9 14-111 Laurentides 34-IV Peck 90-11
15-1 Myakka 15-11 Malbis 15-111 Peck 90-9 35-IV Houghton Oa1
16-1 Houston 16-11 Peck 90-9 16-111 Laurentides 36-IV Laurentides LFH
17-1 Malbis 17-11 Saline Soil 17-111 Myakka 37-IV Houghton Oa4
18-1 Laurentides 18-11 Houston 18-111 Halii 38-IV Houghton Oa2
19-1 Peck 90-12 19-11 Laurentides 19-111 Malbis 39-IV Peck 90-10
20-1 Houston 20-11 Saline Soil 20-111 Malbis 40-IV Houghton Oal

a Roman numbers indicate the method used for the analysis: I = method 994.16-Altemative I; II = method 994.16-Altemative II; III = method
994.17; and IV method 994.18.
=

The soil samples conformed to all known regulations of the B. Apparatus

United States concerning biological pest abatement. The soil
samples did not require special handling or disposal measures,
nor did the participating laboratory need to be licensed or in
spected to receive, handle, or dispose of these samples. The
"blind duplicate" design was used. A number was assigned to
each soil sample as follows: duplicate 1 x 2 in. cards containing
numbers from 1 to 20 were placed in a large kraft paper bag
and mixed for 1 min by vigorous shaking. The cards were then
removed (blind selection) one at a time and samples received
the numbers in the order they were removed from the bag. This
procedure was repeated for every set of samples prepared for
each procedure. Numbers assigned to all samples are presented
in Table 1.
994.16 pH Measurement of Mineral Soils
First Action 1994
Alternative I
(Applicable to pH measurement of mineral soils [soils con
taining <17% organic carbon].)
Method Performance:
See Table 994.16A for method performance data.
A. Principle
Air-dried soil sample is mixed with H20 (1 + 1). pH is
measured potentiometrically.
(a) pH meter.-Equipped with glass electrodes (indicating
and reference), or combination electrode.
(b) Automatic pipet.-Capable of accurately delivering
10 mL.
(c) Stirrer.--Glass rod or portable mechanical stirrer, capa
ble of stirring at 1550 rpm. Small stirrer motor mounted on
handle with short, slightly bent plastic or glass rod agitator is
acceptable.
(d) Glassware.-Paper cups holding 28 g; or glass beak-
ers, 50 mL.
C. Reagents
(a) H20.-Distilled or deionized.
(b) Standard buffers.-pH 4.00, 7.00, and 10.00. Use
pH 4.00 and 7.00 for acid soils, and pH 7.00 and 10.00 for al
kaline soils.
D. Calibration
Calibrate pH meter to appropriate setting using 2 standard
buffers, C(b), depending on type of test sample. If reading of
second standard buffer is not within 0.05 pH unit after adjust
ing to first standard buffer, follow manufacturer's instructions.
E. Preparation of Standard Soils
Use 3 different standard soils (air-dried) ofknown pH, cov
ering pH range of test samples. Weigh 10 g air-dried soil into
paper cup. (Note: Calibrated volume measurement of soil may
be substituted for weighing.) Add 10 mL H20, C(a), to soil
with automatic pipet. (Note: For fine-textured soils containing
312 KALRA: JOURNAL OF AOAC INTERNATIONAL VOL. 78, No.2, 1995

Table 994.16A. Method performance for pH measurements of mineral soils using alternative I

Repeatability Reproducibility
Overall mean of Repeatability Reproducibility relative standard relative standard
laboratorY values standard standard Reproducibility deviation (RSD,), deviation
Soil (x) deviation (s,) Repeatability (r) deviation (SR) (R) 0/0 (RSDR),%

Malbis 5.62 0.30 0.86 0.40 1.14 5.28 7.20

Peck 90-9 6.13 0.19 0.54 0.23 0.66 3.04 3.69
Peck 90-12 4.88 0.18 0.51 0.28 0.80 3.60 5.73
Saline soil 9.74 0.16 0.46 0.26 0.74 1.67 2.67
Peck 90-11 7.86 0.39 1.11 0.44 1.25 4.92 5.54
Halii 4.55 0.18 0.51 0.29 0.83 3.94 6.35
Peck 90-10 5.87 0.18 0.51 0.24 0.68 3.14 4.00
Myakka 5.94 0.29 0.83 0.34 0.97 4.80 5.80
Laurentides 4.28 0.33 0.94 0.46 1.31 7.80 10.75
Houston 7.73 0.11 0.31 0.22 0.63 1.45 2.81

high level of organic matter it may be necessary to add addi G. Determination

tional 1O mL H20 to make suspension.) Mix thoroughly 5 sec
with glass rod or mechanical stirrer. Let soil-H20 suspension
stand for 30 min. Measure pH of each standard as in G. pH
values are acceptable within 0.1 pH unit of known values. If
pH values fall outside this range, recalibrate instrument with
standard buffers and check pH of standard soils again. Follow
manufacturer's instructions for recalibration. Replace elec
trodes if they cannot be calibrated within acceptable limits.
If pH values of all standard soils are >0.1 pH unit lower or
higher than known pH of soil, recheck reference electrode.
Repeat pH measurements of standard soils just before
analysis of test sample.
Perform pH measurement at 20-25C. Before analysis stir
test sample from F with glass rod or mechanical stirrer. Insert
electrode(s) of calibrated pH meter from D into container and
swirl soil-H20 suspension slightly. (Note: Position of reference
electrode with respect to glass electrode and flow rate from
reference electrode may affect pH determination; follow
manufacturer's instructions for electrode[s].) Read pH imme
diately (after 30-60 s) to the nearest 0.1 pH unit. After remov
ing electrode(s) from soil-H20 suspension rinse them with
H20; blot off excess H20 with filter paper.
Follow manufacturer's instructions for storing and main
taining pH electrodes.

F. Preparation of Test Sample

Alternative II
Air dry soil at 20-4QC for 1-4 days depending on the rela
tive humidity and soil properties. Grind air-dried soil to pass (Applicable to pH measurement of mineral soils with vari
2 mm sieve and mix well. Prepare soil sample-H20 suspension able salt content.)
as in E, beginning "Weigh 10 g air-dried soil into paper Method Performance:
cup ... .
" See Table 994.16B for method performance data.

Table 994.168. Method performance for pH measurements of mineral soils using alternative II

Repeatability Reproducibility
Overall mean of Repeatability Reproducibility relative standard relative standard
laboratorY values standard standard Reproducibility deviation (RSD,), deviation
Soil (x) deviation (s,) Repeatability (r) deviation (SR) (R) % (RSDR), %

Malbis 5.09 0.07 0.20 0.13 0.37 1.40 2.47

Peck 90-9 5.53 0.12 0.34 0.17 0.48 2.21 3.13
Peck 90-12 4.39 0.14 0.40 0.20 0.57 3.09 4.51
Saline soil 9.25 0.09 0.26 0.19 0.54 0.95 2.03
Peck 90-11 7.36 0.18 0.51 0.33 0.94 2.41 4.47
Halii 4.34 0.08 0.23 0.18 0.51 1.75 4.16
Peck 90-10 5.40 0.06 0.17 0.13 0.37 1.13 2.41
Myakka 4.31 0.04 0.11 0.12 0.34 0.99 2.86
Laurentides 3.69 0.25 0.71 0.28 0.80 6.91 7.54
Houston 7.48 0.15 0.43 0.16 0.46 2.02 2.17
 KALRA: JOURNAL OF AOAC INTERNATIONAL VOL. 78, No.2, 1995 313

H. Principle M. Preparation of Test Sample

Salt content in soil influences ionic activity, which affects Air dry soil at 20-40C for 1-4 days, depending on relative
pH value of soil-water suspension. W anions are displaced by humidity and soil properties. Grind air-dried soil to pass 2 mm
cations. Exchangeable AI is displaced, which increases con sieve and mix well. Prepare soil sample-CaCl2 suspension as
centration of H+ in solution. pH is decreased by ca 0.5 pH unit in L, beginning "Weigh 10 g air-dried soil into paper cup .... "

if CaCh is used instead of H20.

N. Determination
I. Apparatus Proceed as in G.
Ref.: J. AOAC Int. 78, 310 (1995).
Same as in B.

J. Reagents 994.17 pH Measurement of Saline-Sodie Soils

See C(a)-(b).
First Action 1994
(c) CaCl2 solution.-O.01M. Dissolve 14.7 g CaCl2 2H20
in 10 L H20. pH of solution should be 5.0--6.5. If required,
(Applicable to pH measurement of saline-sodic soils [i.e.,
adjust pH with Ca(OHh or HCl. Specific conductivity should containing large amounts of soluble salts and sufficient ex
be 2.32 0.08 mS/cm at 25C.
changeable sodium to interfere with growth of most crop
K. Calibration plants].)
Method Performance:
Perform as in D. See Table 994.17 for method performance data.

L. Preparation of Standard Soils A. Principle

Use 3 different standard soils (air-dried) of known pH, cov
ering pH range of test samples. Weigh 10 g air-dried soil into
paper cup. (Note: Calibrated volume measurement of soil may
be substituted for weighing.) Add 10 mLO.01M CaCI2> J(c), to
soil with automatic pipet. (Note: For fine-textured soils con
taining high level of organic matter it may be necessary to add
additional 10 mLO.01M CaCl2 to make suspension.) Mix thor
oughly 5 s with glass rod or mechanical stirrer. Let soil-CaCl2
suspension stand for 30 min. Measure pH of each standard as
in G. pH values are acceptable within 0.1 pH unit of known
values. If pH values fall outside this range, recalibrate instru
ment and check pH of standard soils again. Follow manufac
turer's instructions for recalibration. Replace electrodes if they
cannot be calibrated within acceptable limits.
If pH values of all standard soils are 0.1 pH unit lower or
higher than known pH of soil, recheck reference electrode.
Repeat pH measurements just before analysis of test sample.
H20 is added to air-dried soil until saturated paste is ob
tained and then pH is measured. For determination of sodium
adsorption ratio, salt analysis is performed on saturation extract
from paste.
B. Apparatus
(a) pH meter.-Equipped with glass electrodes (indicating
and reference), or combination electrode.
(b) Glassware.-Paper cups holding 25-250 g; or glass
beakers, 50-400 mL.
(c) Spatula.
C. Reagents
(a) H20.-Distilled or deionized.
(b) Standard buffers.-pH 4.00, 7.00, and 10.00. Use pH
4.00 and 7.00 for acid soils, and pH 7.00 and 10.00 for alkaline
soils.

Table 994.17. Method performance for pH measurements in soil paste

Repeatability Reproducibility
Overall mean of Repeatability Reproducibility relative standard relative standard
laboratorY values standard standard Reproducibility deviation (RSD,), deviation
Soil type (x) deviation (s,) Repeatability (r) deviation (SR) (R) % (RSDR), %

Malbis 5.47 0.05 0.14 0.18 0.51 1.00 3.27

Peck 90-9 5.99 0.22 0.63 0.25 0.71 3.59 4.14
Peck 90-12 4.82 0.21 0.60 0.28 0.80 4.43 5.78
Saline soil 9.48 0.07 0.20 0.26 0.74 0.74 2.76
Peck 90-11 7.64 0.12 0.34 0.22 0.63 1.58 2.94
Halii 4.35 0.09 0.26 0.17 0.48 2.02 3.95
Peck 90-10 5.83 0.17 0.48 0.22 0.63 2.84 3.82
Myakka 5.42 0.10 0.29 0.17 0.48 1.80 3.22
Laurentides 4.18 0.30 0.86 0.42 1.20 7.09 9.93
Houston 7.51 0.11 0.31 0.18 0.51 1.46 2.45
314 KALRA: JOURNAL OF AOAC INTERNATIONAL VOL. 78, NO.2, 1995

D. Calibration Repeat pH measurements of standard soils just before

analysis of test sample.
Calibrate pH meter to appropriate setting using 2 standard
buffers,C(b), depending on type of test sample. If reading of F. Preparation of Test Sample
second standard buffer is not within 0.05 pH unit after adjust Air dry soil at 20 -40C for 1-4 days, depending on relative
ing to fIrst standard buffer, follow manufacturer's instructions humidity and soil properties. Grind air-dried soil to pass2 mm
for recalibration. sieve and mix well. Prepare soil paste as in E, beginning
"Weigh 50-250 air-dried soil. ...
"

E. Preparation of Standard Soils

G. Determination
Use 3 different standard soils (air-dried) of known pH, cov
Perform pH measurement at 20-25C. Insert electrode(s)
ering pH range of test samples. Weigh 50-250 g air-dried soil
of standardized pH meter from D almost to the bottom of con
into paper cup or glass beaker. (Note: Use smaller amounts of
tainer containing soil paste. Gently rotate container to remove
soil for pH measurement only; use larger amounts to obtain
air bubbles and provide good contact between electrode(s) and
sufficient volume of saturation extract for other measure
soil paste. Remove hands from container while measuring pH
ments.) Wet soil with H20, C(a), while stirring with spatula.
of soil paste.
(Note: Calibrated volume of soils may be substituted for
Read pH immediately (after 30-60 s) to the nearest 0.1 pH
weighing. Alternatively, add sufficient amount of soil to known
unit. After removing electrode(s) from soil paste, rinse them
volume of H20 to obtain saturated paste. Moisture content in
with H20; blot off excess H20 with fIlter paper.
soil may vary [25-100%] depending on soil texture, clay min
Follow manufacturer's instructions for storing and main
eralogy, and content of organic matter.)
taining pH electrodes.
Tap container gently against workbench to settle soil paste.
Ref.: 1. AOAC Int. 78, 310 (1995).
At saturation, surface of paste should glisten but no supernatant
H20 should be present. (Note: Saturated soil paste also slides
freely and cleanly from spatula when blade is turned vertically.
994.18 pH Measurement of Organic Soils
At saturation, soil will slowly flow together after it has been
parted by spatula.) Add more H20 if needed to obtain saturated
First Action 1994
paste. If excess H20 is present, add small amount of soil, stir,
and tap container again. Add H20 or soil until proper moisture (Applicable to pH measurement of organic soils [soils con-

content is obtained. taining 17% organic carbon].)

Method Performance:
Cover container with watch glass and let stand for 1-4 h.
After 60 min some high clay soils may require addition of more
See Table 994.18 for method performance data.
H20, as interstitial spaces in some clays become saturated with
A. Principle
H20. After further saturation let soil paste stand longer.
Measure pH of each standard as in G. pH values are accept Dried soil sample is mixed with H20 (1 + 4). pH is meas
able within 0.1 pH unit of known values. If pH values fall ured potentiometrically.
outside this range, recalibrate instrument and check pH of
B. Apparatus
standard soils again. Follow manufacturer's instructions for re
calibration. Replace electrodes if they cannot be calibrated (a) pH meter.-Equipped with glass electrodes (indicating
within acceptable limits. and reference), or combination electrode.

Table 994.18. Method performance for pH measurements of organic soils

Repeatability Reproducibility
Overall mean of Repeatability Reproducibility relative standard relative standard
laboratoIY values standard standard Reproducibility deviation (RSDr), deviation
Soil (x) deviation (sr) Repeatability (r) deviation (SR) (R) % (RSDR), %

Houghton Oa3 7.43 0.05 0.14 0.06 0.17 0.73 3.16

Peck 90-9 6.24 0.22 0.63 0.30 0.86 3.57 4.74
Peck 90-12 5.08 0.24 0.68 0.32 0.91 4.66 6.32
Houghton Oa4 7.07 0.06 0.17 0.18 0.51 0.87 2.51
Peck 90-11 7.96 0.21 0.60 0.38 1.08 2.62 4.82
Houghton Oa5 6.85 0.17 0.48 0.23 0.66 2.50 3.43
Peck 90-10 6.07 0.18 0.51 0.27 0.77 2.94 4.49
Houghton Oa2 7.73 0.26 0.74 0.34 0.97 3.32 4.36
Laurentides LFH 6.62 0.10 0.29 0.15 0.43 1.55 2.33
Houghton Oa1 7.37 0.06 0.17 0.16 0.46 0.77 2.15
 KALRA: JOURNAL OF AOAC INTERNATIONAL VOL 78, No.2, 1995
(b) Automatic pipet.-Capable of accurately delivering
20 mL.
(c) Stirrer.-Glass rod or portable mechanical stirrer,capa
ble of stirring at 1550 rpm. Small stirrer motor mounted on
handle with short,slightly bent plastic or glass rod agitator is
acceptable.
(d) Glassware.-Paper cups holding 28 g; or glass beak-
ers,50mL.
C. Reagents
(a) H20.-Distilled or deionized.
(b) Standard buffers.-pH 4.00, 7.00, and 10.00. Use pH
4.00 and 7.00 for acid soils,and pH 7.00 and 10.00 for alkaline
soils.
D. Calibration
Calibrate pH meter to appropriate setting using 2 standard
buffers,C(b), depending on type of test sample. If reading of
second standard buffer is not within 0.05 pH unit after adjust
ing to fIrst standard buffer,follow manufacturer's instructions.
E. Preparation of Standard Soils
Use 3 different air-dried standard organic soils of known
pH,covering pH range of test samples. Weigh 5 g air-dried soil
into paper cup. (Note: Calibrated volume measurement of soil .
may be substituted for weighing.) Add 20 mL H20,C(a), to
soil with automatic pipet. Mix thoroughly 5 sec with glass rod
or mechanical stirrer. Let soil-H20 suspension stand for
30 min. Measure pH of each standard as in G. pH values are
acceptable within 0.1 pH unit of known values. If pH values
fall outside this range,recalibrate instrument and check pH of
standard soils again. Follow manufacturer's instructions for re
calibration. Replace electrod:!s if they cannot be calibrated
within acceptable limits.
If pH values of all standard soils are >0.1 pH unit lower or
higher than known pH of soil,recheck reference electrode.
Repeat pH measurements of standard soils just before
analysis of test sample.
F. Preparation of Test Sample
Pass dried soils (at 30C) through 2 mm sieve and mix well.
(Note: Many organic soils become hydrophobic when they are
dried and may require longer time to wet.) Weigh 5 g dried soil
sample into paper cup. (Note: Calibrated volume measurement
of soil may be substituted for weighing.) Add 20 mL H20,
C(a), to soil with automatic pipet. Mix thoroughly 5 sec with
portable mechanical stirrer. Let soil-H20 suspension stand for
30 min before pH measurements.
G. Determination
Perform pH measurement at 20-25C. Before analysis stir
test sample from F with glass rod or mechanical stirrer. Insert
electrode(s) of calibrated pH meter from D into container and
swirl soil-H20 suspension slightly. (Note: Position of reference
electrode with respect to glass electrode and flow rate from
reference electrode may affect pH determination; follow
manufacturer's instructions for placement of electrode[s].)
315
Read pH immediately (after 30--60 s) to the nearest 0.1 pH
unit. After removing electrode(s) from soil-H20 suspension
rinse them with H20; blot off excess H20 with ftlter paper.
Follow manufacturer's instructions for storing and main
taining pH electrodes.
Ref.: 1. AOAC Int. 78, 310 (1995).
Results and Discussion
The results of analyses were received from 53 collaborators
by February 5, 1993, and are presented in Tables 2-5. Results
were analyzed using statistics software and worksheets devel
oped by the Statistics Committee,AOAC INTERNATIONAL
(6--8). Results of statistical analyses are presented in Tables
994.16A-B, 994.17, and 994.18.
All 53 participants provided results obtained by the meth
ods for mineral and organic soils,while 51 laboratories pro
vided data from the method for saline-sodic soils. In general,
the more diluted the soil suspension,the higher pH of the soil.
The alternative I for mineral soils and the method for saline-so
dic soils use a mixture of soil and water. In alternative I for
mineral soils the amount of water is fIxed (100%). However,
for saline-sodic soils the amount of water needed to prepare a
saturated paste depends on soil properties such as texture and
organic matter. For soils that require 100% water for saturated
paste,the pH will be the same as when using alternative I for
mineral soils; it will be lower if less water is needed. Halii soil
uses less water to make a paste (method for saline-sodic soils)
than in the alternative I for mineral soils; therefore,the pH
would be lower by 0.2 unit. For Mykka soil,the pH differences
are large because this type of soil is a fIne sand and,therefore,
much less water is required to prepare a paste.
All valid data were included in the statistical analyses. The
tests used for determination of outliers were: (I) Cochran test
for removal of laboratories showing signifIcantly greater
within-laboratory variability than the other laboratories,and
(2) Grubbs (Single and Double Grubbs) test for removal of
laboratories with extreme values. The repeatability relative
standard deviation (RSDr) values were 1.45-7.80% by the al
ternative I of the method for mineral soils,0.95.91% by the
alternative II of the method for mineral soils,0.74-7.09% from
the method for saline-sodic soils,and 0.73-4.66% from the
method for organic soils. The corresponding reproducibility
relative standard deviation (RSD0 values were 2.67-10.75%,
2.03-7.54%, 2.45-9.93%, and 2.15.32%. There were out
liers indicated but repeatability and reproducibility standard
deviations show that these values are well within acceptable
limits for pH measurement in soil (9). Therefore,no laborato
ries were deleted from statistical analysis. It is interesting to
note that one sample (Laurentides) gave the highest RSDr and
RSDR values by the methods for mineral and saline-sodic soils;
this sample was not analyzed by the method for organic soils.
Collaborators' Comments
The participants were asked to indicate any questions,prob
lems,and suggestions regarding their work with these methods.
316 KALRA: JOURNAL OF AOAC INTERNATIONAL VOL. 78, No.2, 1995

Table 2. Collaborative study results for pH measurements of mineral soils using alternative I

Sample

Lab. 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20

1 5.90 6.35 5.13 9.61 8.04 4.50 6.12 6.08 4.51 4.37 6.13 9.62 8.08 6.49 6.10 7.83 5.95 4.38 5.15 7.83
2 5.48 6.01 4.82 9.77 7.98 4.43 6.14 5.90 4.48 4.25 5.84 9.77 7.88 6.11 5.91 7.71 5.69 4.28 4.85 7.65
3 5.50 6.10 4.80 9.65 7.80 4.20 5.90 5.80 4.20 4.05 5.80 9.60 7.85 6.00 5.80 7.80 5.50 4.05 4.80 7.70
4 5.45 6.04 4.84 9.97 7.93 4.38 5.90 5.91 4.33 4.26 5.85 9.99 7.87 6.04 5.85 7.91 5.52 4.30 4.87 8.04
5 5.37 6.19 5.13 9.33 7.52 4.76 5.92 5.67 4.44 4.20 5.89 9.44 7.73 6.19 5.70 7.68 5.59 4.24 4.87 7.42
6 5.18 5.80 4.59 9.67 7.85 4.38 5.74 5.75 4.30 4.03 5.70 9.65 7.89 6.10 5.75 7.65 5.57 4.06 4.68 7.58
7 5.46 6.13 4.88 9.70 7.95 4.38 5.95 5.86 4.38 4.16 5.93 9.65 7.97 6.14 5.85 7.82 5.53 4.17 4.91 7.82
8 5.64 6.21 4.98 9.89 8.06 4.62 6.08 6.07 4.52 4.22 5.85 9.80 8.08 6.47 6.19 7.86 5.84 4.28 4.95 7.91
9 5.30 5.70 4.50 9.90 7.80 4.20 5.70 5.50 4.30 4.60 5.80 10.00 8.40 6.00 5.60 7.70 5.20 3.90 4.50 7.60
10 5.86 6.12 4.91 9.54 7.91 4.98 5.93 5.93 4.58 4.24 5.85 9.50 7.87 6.12 5.82 7.65 6.14 4.42 5.03 7.57
11 4.92 5.65 4.42 9.67 7.78 4.66 5.57 5.77 4.05 3.82 5.32 9.65 7.51 6.73 6.75 7.25 5.46 3.93 4.36 6.97
12 5.40 5.89 4.80 9.89 7.94 4.22 5.83 5.70 4.34 4.04 5.92 9.84 8.00 6.12 5.79 8.06 5.49 4.17 4.89 7.80
13 6.29 6.51 5.48 9.36 7.80 5.48 6.54 6.27 4.86 4.49 5.99 9.05 7.95 6.29 5.02 7.60 6.54 4.78 5.06 7.63
14 5.65 6.24 5.04 9.79 8.05 4.54 6.04 6.05 4.49 4.39 5.99 9.77 8.03 6.31 6.07 7.82 5.73 4.42 5.01 7.76
15 5.45 6.05 6.05 10.15 8.15 4.55 5.85 6.25 4.65 5.09 6.14 11.69 9.31 6.35 7.03 7.96 7.10 4.61 5.61 7.67
16 5.55 6.05 4.84 9.76 7.70 4.44 5.82 5.98 4.40 4.25 5.81 9.86 7.90 6.12 6.09 7.77 5.82 4.39 4.88 7.76
17 5.42 6.81 4.78 9.73 7.76 5.14 6.11 5.83 4.23 6.10 5.81 9.90 7.85 5.92 7.27 7.30 5.33 4.15 4.91 7.51
18 5.46 6.10 4.73 9.47 7.85 4.32 5.90 5.78 4.30 4.11 5.91 9.56 7.76 6.13 5.81 7.58 5.57 4.16 4.80 7.51
19 4.95 5.68 4.37 9.85 4.13 4.12 5.54 5.33 3.78 3.75 5.66 9.95 7.70 5.75 5.66 7.56 5.18 3.81 4.55 7.21
20 5.51 6.12 4.84 9.67 8.07 4.45 6.16 6.07 4.54 4.40 6.11 9.75 8.10 6.42 6.20 8.04 5.89 4.60 5.28 8.09
21 5.40 6.01 4.70 10.23 7.84 4.75 5.75 5.78 4.25 4.06 5.74 9.95 7.75 6.60 6.90 7.69 7.45 4.27 4.68 7.14
22 5.40 6.00 4.80 9.74 7.82 4.40 5.80 5.70 4.40 4.06 5.83 9.76 7.86 6.06 5.70 7.91 5.40 4.06 4.78 8.01
23 5.78 6.30 5.03 9.88 8.18 4.46 6.10 6.05 4.48 4.30 6.00 9.89 8.00 6.23 6.33 8.05 5.70 4.33 4.94 7.75
24 5.11 5.74 4.32 9.57 7.52 4.21 5.39 5.08 4.24 3.65 5.44 9.63 7.60 5.86 5.45 7.57 5.58 3.79 4.50 7.53
25 5.47 5.97 4.73 9.72 7.84 4.31 5.83 5.76 4.32 4.15 5.88 9.65 7.85 6.02 5.78 7.85 5.51 4.18 4.77 7.88
26 5.59 5.96 5.03 9.62 7.95 4.55 5.74 6.25 4.47 4.19 5.65 9.53 8.00 5.92 5.62 7.99 5.46 4.10 4.79 7.90
27 5.46 6.11 4.91 9.66 7.84 4.57 5.95 5.88 4.39 4.21 5.96 9.76 7.90 6.13 5.96 7.67 5.51 4.24 4.88 7.70
28 6.25 6.45 5.20 C).55 7.90 4.65 6.15 6.20 4.65 4.60 6.10 9.65 7.95 6.45 6.15 7.85 5.80 4.50 5.50 7.85
29 5.25 5.85 4.66 9.91 7.78 4.44 5.75 5.62 4.37 4.02 5.67 9.89 7.82 5.85 5.80 7.86 5.30 4.01 4.65 7.86
30 5.45 6.05 4.81 9.79 7.97 4.82 5.91 5.94 4.79 4.16 5.90 9.78 7.98 6.07 5.92 7.82 5.48 4.16 4.84 7.89
31 5.46 5.98 4.81 9.69 7.88 4.63 5.95 6.00 4.41 4.24 5.88 9.66 7.87 6.17 6.08 7.69 6.00 4.29 4.84 7.60
32 5.42 6.02 4.78 9.71 7.95 4.74 5.84 5.81 4.72 4.10 5.86 9.68 7.95 6.06 5.81 7.77 5.40 4.06 4.79 7.74
33 5.45 5.96 4.69 9.52 7.75 4.36 4.33 5.77 4.27 4.12 5.75 9.54 7.80 6.00 5.80 7.68 5.50 4.15 4.61 7.65
34 5.44 6.02 4.78 9.60 7.99 5.25 5.82 6.54 4.69 4.32 5.73 9.57 7.83 6.17 6.57 7.62 5.63 4.55 4.94 7.91
35 5.52 6.07 4.90 9.69 8.05 4.42 5.93 5.90 4.41 4.21 5.88 9.67 8.03 6.12 5.91 7.91 5.52 4.22 4.86 7.91
36 5.54 6.02 6.25 9.92 7.99 5.05 5.99 6.00 4.90 4.12 4.87 9.91 7.94 6.28 6.06 7.80 5.70 4.15 4.80 7.61
37 5.42 6.11 4.82 9.65 7.97 4.69 6.10 5.78 4.62 4.06 5.97 9.75 7.94 6.13 5.81 7.74 5.51 4.09 4.90 7.77
38 5.50 6.10 4.90 9.70 7.90 4.80 5.90 5.90 4.80 4.20 5.90 9.70 7.90 6.10 5.90 7.90 5.50 4.20 4.90 7.90
39 5.63 6.14 4.94 9.76 8.02 4.39 5.91 6.01 4.40 4.22 5.94 9.69 7.93 6.05 5.97 7.83 5.56 4.22 4.84 7.90
40 5.40 6.06 4.83 9.60 7.89 4.51 5.90 5.71 4.36 4.06 5.87 9.68 7.95 5.98 5.69 7.84 5.46 4.06 4.78 7.88
41 5.16 5.96 4.73 9.68 7.88 4.73 5.79 5.55 4.69 3.91 5.78 9.66 7.86 5.97 5.50 7.73 5.19 3.95 4.75 7.72
42 5.58 6.07 4.82 9.93 8.01 4.42 5.84 5.97 4.33 4.17 5.77 9.78 7.96 6.20 5.97 7.76 5.78 4.28 4.80 7.78
43 5.50 6.10 4.90 10.00 8.00 4.70 5.90 5.80 4.70 4.10 5.90 10.00 8.00 6.00 5.80 8.00 5.50 4.10 4.80 8.00
44 5.45 5.96 4.81 9.72 7.92 4.39 5.83 5.95 4.29 4.19 5.81 9.74 7.85 6.11 6.07 7.79 5.52 4.15 4.75 7.76
45 7.08 6.60 5.18 10.14 7.44 5.73 6.13 6.20 5.18 4.63 5.42 9.97 6.90 6.98 6.96 7.13 7.07 4.90 5.11 6.83
46 5.57 6.55 4.87 9.72 7.38 4.78 5.95 6.34 7.80 4.14 5.88 9.67 7.91 6.06 5.56 7.74 5.44 4.19 4.84 7.73
47 5.59 6.22 5.05 9.79 8.07 4.55 6.08 5.82 4.44 4.25 5.95 9.69 8.08 6.45 6.11 7.78 5.76 4.36 4.98 7.91
48 5.55 6.09 4.90 9.66 7.98 4.50 5.96 5.95 4.44 4.22 5.89 9.66 7.99 6.22 6.02 7.84 5.99 4.41 4.99 7.76
49 5.51 6.04 4.80 9.60 7.91 4.80 5.92 5.72 4.78 4.01 5.82 9.61 7.87 6.19 5.70 7.67 5.62 4.10 4.84 7.68
50 5.22 5.81 4.60 9.64 7.70 4.68 5.68 5.60 4.67 4.00 5.68 9.65 7.76 5.91 5.65 7.80 5.33 4.04 4.66 7.80
51 5.70 6.22 5.03 9.63 8.04 4.51 6.05 6.09 4.50 4.81 6.04 9.65 8.01 6.29 6.16 7.92 5.77 4.90 5.11 7.81
52 5.62 6.17 4.98 9.69 7.96 4.42 5.98 5.90 4.43 4.22 5.95 9.66 7.98 6.15 5.91 7.74 5.61 4.25 4.96 7.76
53 5.83 6.17 4.90 9.32 7.19 5.26 5.93 6.29 4.70 5.13 6.38 9.50 7.90 6.42 6.36 7.74 6.29 7.73 4.86 7.40
 KALRA: JOURNAL OF AOAC INTERNATIONAL VOL. 78, No.2, 1995 317

Table 3. Collaborative study results for pH measurements of mineral soils using alternative II

Sample

Lab. 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20

1 3.76 7.49 7.47 4.49 7.48 4.53 4.36 5.32 5.64 4.48 5.64 4.44 4.44 5.77 5.33 5.80 9.08 7.56 3.75 9.10
2 3.59 7.41 7.50 4.41 7.45 4.30 4.28 5.07 5.44 4.52 5.40 4.28 4.20 5.46 5.10 5.52 9.35 7.48 3.64 9.35
3 3.50 7.60 7.60 4.25 7.60 4.25 4.25 5.15 5.45 4.20 5.45 4.25 4.20 5.60 5.15 5.60 9.35 7.60 3.50 9.35
4 3.61 7.44 7.42 4.34 7.45 4.32 4.37 5.03 5.29 4.24 5.36 4.35 4.25 5.51 5.06 5.51 9.53 7.44 3.59 9.46
5 3.73 7.13 7.25 4.85 7.33 4.43 4.35 4.91 5.35 4.44 5.40 4.37 4.22 5.48 5.01 5.58 8.76 7.28 3.93 8.74
6 3.38 7.26 7.41 4.49 7.25 4.29 4.26 5.05 5.35 4.22 5.38 4.32 4.26 5.51 5.13 5.54 9.09 7.56 3.70 9.05
7 3.62 7.58 7.55 4.33 7.56 4.33 4.28 5.09 5.41 4.30 5.43 4.28 4.27 5.57 5.13 5.58 9.26 7.53 3.68 9.24
8 3.58 7.33 7.37 4.34 7.34 4.28 4.31 4.98 5.26 4.22 5.36 4.32 4.28 5.36 4.99 5.36 9.29 7.53 3.52 9.27
9 3.50 7.40 7.50 4.30 7.10 4.20 3.80 4.80 5.10 4.00 5.40 3.80 3.80 5.20 4.80 5.30 7.00 7.40 3.60 9.71
10 3.73 7.28 7.39 4.83 7.39 4.42 4.34 5.11 5.40 4.39 5.44 4.33 4.34 5.60 5.20 5.69 9.09 7.47 3.78 9.03
11 3.66 6.82 7.22 4.39 6.70 4.41 4.43 5.02 5.36 4.34 5.38 4.32 4.23 5.48 5.10 5.48 8.61 7.67 3.69 9.24
12 3.34 7.15 7.36 4.15 7.41 4.16 4.18 4.84 4.99 3.93 5.09 4.20 3.97 5.26 4.89 5.40 9.44 7.43 3.65 9.43
13 3.59 7.35 7.49 4.52 7.42 4.35 4.24 4.91 5.49 4.72 5.44 4.26 4.26 5.49 5.12 5.53 9.14 7.45 3.96 9.19
14 3.78 7.62 7.59 4.46 7.71 4.42 4.42 5.26 5.60 4.40 5.54 4.46 4.49 5.67 5.26 5.68 9.41 7.64 3.78 9.42
15 4.66 7.59 7.88 4.74 7.78 4.50 4.55 5.20 5.62 4.37 5.64 4.63 4.70 6.05 5.47 5.74 9.47 7.70 3.70 9.39
16 3.98 7.49 7.60 4.63 7.57 4.60 4.59 5.32 5.59 4.56 5.59 4.57 4.51 5.71 5.34 5.74 9.32 7.66 4.08 9.37
17 3.34 6.92 7.09 4.59 6.98 4.31 4.17 4.95 5.31 4.18 5.29 4.17 4.16 5.42 4.99 5.44 9.29 7.82 3.87 9.14
18 3.55 7.34 7.42 4.36 7.44 4.38 4.29 5.10 5.46 4.27 5.46 4.18 4.25 5.66 5.12 5.70 9.28 7.46 3.57 9.32
19 3.45 7.11 7.42 4.32 6.95 4.31 4.26 5.05 5.44 4.21 5.41 4.26 4.21 5.55 5.11 5.58 9.36 7.61 3.56 9.25
20 3.69 7.23 7.34 4.46 7.33 4.46 4.44 5.27 5.52 4.47 5.51 4.47 4.44 5.72 5.40 5.75 8.93 7.50 3.97 8.93
21 3.59 7.53 7.60 4.59 7.50 4.50 4.35 4.99 5.50 4.29 5.25 4.39 4.29 5.59 5.20 5.60 9.45 7.53 3.73 9.20
22 3.49 7.51 7.53 4.35 7.57 4.26 4.23 5.09 5.39 4.31 5.40 4.25 4.23 5.56 5.04 5.56 9.40 7.55 3.48 9.42
23 3.66 7.50 7.57 4.46 7.40 4.50 4.42 5.22 5.54 4.37 5.53 4.45 4.46 5.70 5.35 5.75 9.49 7.65 3.93 9.53
24 3.24 7.33 7.35 4.22 7.33 4.18 4.13 4.90 5.10 4.20 4.93 4.30 4.19 5.22 4.90 5.28 9.32 7.23 3.56 8.91
25 3.66 7.45 7.48 4.27 7.46 4.25 4.25 5.09 5.35 4.23 5.36 4.25 4.24 5.51 5.08 5.50 9.20 7.47 3.65 9.24
26 3.67 6.74 6.96 4.46 6.80 4.27 4.28 5.06 5.33 4.40 5.55 4.53 4.42 5.65 5.18 5.59 9.28 7.62 3.68 9.09
27 3.54 7.35 7.31 4.30 7.36 4.26 4.36 5.06 5.38 4.25 5.40 4.38 4.27 5.49 5.11 5.58 9.16 7.34 3.66 9.22
28 3.65 7.20 7.15 4.25 7.20 4.30 4.30 5.05 5.30 5.00 5.55 4.25 5.00 5.50 5.05 5.50 8.80 7.20 3.75 8.70
29 3.63 7.49 7.46 4.31 7.42 4.23 4.26 5.09 5.33 4.25 5.34 4.29 4.24 5.50 5.06 5.51 9.52 7.51 3.73 9.47
30 3.61 7.57 7.61 4.41 7.57 4.34 4.36 5.19 5.46 4.58 5.45 4.37 4.58 5.62 5.13 5.61 9.44 7.65 3.74 9.46
31 3.58 7.31 7.46 4.35 7.37 4.31 4.30 5.13 5.39 4.30 5.39 4.31 4.33 5.56 5.14 5.59 9.25 7.47 3.71 9.29
32 3.58 7.58 7.53 4.30 7.57 4.27 4.24 5.06 5.38 4.50 5.38 4.24 4.47 5.52 5.04 5.51 9.31 7.53 3.55 9.31
33 3.51 7.47 7.44 4.53 7.48 4.26 4.27 5.07 5.38 4.25 5.42 4.30 4.22 5.52 5.08 5.54 9.26 7.45 3.95 9.28
34 3.56 7.26 7.32 4.38 7.26 4.24 4.29 5.02 5.26 4.21 5.26 4.36 4.24 5.45 5.07 5.43 9.14 7.49 4.69 9.10
35 3.62 7.48 7.48 4.29 7.52 4.33 4.30 5.12 5.43 4.29 5.41 4.29 4.29 5.55 5.16 5.59 9.22 7.57 3.64 9.24
36 3.82 7.41 7.47 4.58 7.45 4.53 4.39 5.08 5.37 4.63 5.36 4.40 4.55 5.53 5.11 5.84 9.29 7.56 3.75 9.29
37 3.51 7.45 7.47 4.23 7.46 4.21 4.20 5.04 5.39 4.37 5.35 4.23 4.36 5.47 5.02 5.52 9.21 7.47 3.50 9.19
38 3.60 7.60 7.60 4.20 7.60 4.20 4.40 5.10 5.40 4.50 5.40 4.40 4.50 5.50 5.10 5.50 9.30 7.60 3.80 9.30
39 3.55 7.39 7.39 4.21 7.44 4.23 4.26 5.05 5.29 4.21 5.28 4.17 4.13 5.44 5.02 5.42 9.11 7.36 3.52 9.17
40 3.56 7.58 7.52 4.35 7.58 4.29 4.28 5.08 5.42 4.27 5.43 4.29 4.25 5.54 5.08 5.54 9.27 7.52 3.72 9.29
41 3.51 7.52 7.53 4.30 7.53 4.29 4.26 5.03 5.38 4.53 5.38 4.23 4.53 5.55 5.04 5.56 9.30 7.54 3.52 9.32
42 3.64 7.41 7.52 4.45 7.42 4.30 4.27 5.04 5.35 4.23 5.34 4.35 4.24 5.48 5.09 5.53 9.42 7.59 4.25 9.35
43 3.40 7.60 7.70 4.30 7.60 4.20 4.10 5.00 5.30 4.40 5.30 4.10 4.40 5.50 5.00 5.50 9.70 7.60 3.60 9.70
44 3.54 7.34 7.43 4.20 7.35 4.21 4.20 5.00 5.30 4.19 5.29 4.21 4.12 5.42 5.02 5.34 9.28 7.42 3.33 9.27
45 3.72 6.37 6.61 4.73 6.40 4.67 4.22 4.79 5.20 4.28 5.17 4.34 4.21 5.28 5.08 5.37 9.20 7.59 3.69 9.40
46 3.69 5.18 7.58 4.61 6.84 5.05 4.37 4.76 5.70 4.65 5.48 4.37 4.63 5.12 5.18 5.61 9.28 7.57 3.79 9.26
47 3.69 7.64 7.57 4.51 7.58 4.45 4.35 5.20 5.60 4.36 5.62 4.30 4.39 5.73 5.22 5.69 9.26 7.62 3.81 9.30
48 3.63 7.55 7.55 4.49 7.55 4.39 4.37 5.13 5.47 4.32 5.44 4.37 4.30 5.55 5.14 5.56 9.29 7.58 4.04 9.29
49 3.60 7.49 7.40 4.45 7.49 4.27 4.21 5.02 5.36 4.41 5.39 4.21 4.41 5.58 5.01 5.50 9.30 7.38 3.81 9.37
50 3.51 7.42 7.48 4.33 7.44 4.27 4.40 4.97 5.30 4.48 5.32 4.26 4.50 5.49 5.01 5.48 9.28 7.49 3.54 9.28
51 4.04 7.64 7.62 4.60 7.67 4.53 4.51 5.30 5.55 4.41 5.54 4.51 4.40 5.68 5.28 5.68 9.34 7.62 4.31 9.32
52 3.61 7.60 7.58 4.31 7.61 4.31 4.30 5.13 5.46 4.26 5.51 4.31 4.27 5.58 5.13 5.60 9.28 7.60 3.68 9.28
53 3.60 7.18 7.27 5.34 7.38 4.54 4.42 5.20 5.40 4.44 5.36 4.47 4.31 4.45 5.16 5.47 8.96 7.42 5.22 8.95
318 KALRA: JOURNAL OF AOAC INTERNATIONAL VOL. 78, No.2, 1995

a
Table 4. Collaborative study results for pH measurements of saline-sodie soils

Sample

Lab. 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20

1 7.47 7.59 4.98 4.35 7.67 5.95 5.50 4.90 7.76 6.17 9.36 5.94 9.47 4.28 6.10 4.12 5.48 4.34 5.60 5.64
2 7.66 7.46 4.81 4.26 7.80 5.75 5.44 4.78 7.68 5.89 9.75 5.79 9.71 4.41 5.92 3.96 5.40 4.23 5.40 5.42
3 7.45 7.40 4.60 4.15 7.60 5.70 5.15 4.60 7.60 5.80 9.25 5.65 9.15 3.70 5.80 3.70 5.20 4.10 5.35 5.35
4 7.52 7.63 4.87 4.11 7.76 5.80 5.64 4.70 7.79 6.02 9.76 5.66 9.80 4.23 5.89 4.12 5.49 4.07 5.46 5.36
5 7.56 7.57 5.16 4.46 7.76 5.76 5.54 4.70 7.79 5.96 9.27 5.74 9.20 4.04 5.90 3.93 5.40 4.23 5.37 5.38
6 7.33 7.40 4.54 4.11 7.45 5.55 5.16 4.51 7.47 5.76 9.47 5.64 9.48 3.89 5.75 3.91 5.23 4.17 5.27 5.23
7 7.54 7.57 4.84 4.31 7.78 5.80 5.39 4.81 7.79 6.00 9.46 5.82 9.46 4.21 6.00 4.05 5.37 4.31 5.56 5.56
8 7.42 7.61 5.02 4.16 7.58 5.98 5.70 4.88 7.64 6.20 9.47 5.99 9.52 4.32 5.94 4.05 5.52 4.31 5.21 5.19
9 7.65 7.67 4.84 4.20 7.63 5.82 5.42 5.05 7.79 6.08 9.65 5.90 9.78 5.30 6.17 4.09 5.13 4.20 5.20 5.30
10 7.31 7.47 4.87 4.33 7.48 5.81 5.38 4.79 7.56 6.01 9.21 7.07 9.36 4.31 5.78 4.04 5.26 4.31 5.48 5.51
11 7.14 7.48 4.52 4.27 7.31 5.61 5.16 4.41 7.17 6.45 9.34 5.51 9.26 4.16 5.67 3.90 5.24 4.15 5.01 5.12
12 7.47 7.70 4.66 4.25 7.62 5.65 5.41 4.67 7.68 5.87 9.62 5.64 9.61 3.99 5.87 3.97 5.39 4.27 5.45 5.49
13 7.49 7.58 4.90 4.34 7.65 5.79 5.44 4.82 7.90 6.00 9.49 5.79 9.39 4.06 6.16 4.03 5.47 4.37 5.60 5.60
14 7.54 7.57 4.95 4.44 7.70 5.81 5.53 4.85 7.75 5.99 9.52 5.87 9.59 4.68 6.61 4.17 5.58 4.44 5.68 5.65
15 7.66 7.59 4.90 4.43 7.62 5.88 5.36 4.75 7.43 5.90 9.16 5.80 9.20 4.06 5.86 3.92 5.32 4.29 5.45 5.53
16 7.56 7.65 4.95 4.49 7.66 5.91 5.65 4.90 7.82 6.14 9.64 6.11 9.63 4.24 6.00 4.20 5.55 4.50 5.62 5.65
17 7.35 7.49 5.22 4.53 7.82 5.92 5.72 5.02 7.79 6.27 9.44 6.48 9.32 6.27 6.50 5.54 5.60 4.61 5.68 5.75
18 7.38 7.43 4.85 4.28 7.58 5.87 5.45 4.85 7.61 6.11 9.52 6.10 9.64 4.14 6.11 4.02 5.45 4.30 5.56 5.55
19 7.62 7.68 4.61 4.21 7.33 5.64 5.13 4.39 7.45 5.75 9.98 5.59 9.82 4.22 5.68 3.67 5.08 4.17 4.97 4.99
20 7.33 7.37 4.69 4.31 7.47 5.73 5.33 4.74 7.51 5.92 9.12 5.92 9.21 4.43 5.95 4.03 5.49 4.40 5.54 5.52
21 7.38 7.35 5.92 4.55 7.28 5.95 5.42 5.35 4.59 7.59 9.48 5.98 9.57 5.14 5.91 4.08 5.38 4.24 5.39 5.35
22 7.78 7.59 4.62 4.29 7.72 5.78 5.42 4.75 7.77 5.99 9.67 5.78 9.63 4.00 5.95 3.95 5.43 4.26 5.50 5.52
23 7.85 7.51 5.04 4.42 7.56 5.92 5.44 4.89 7.59 6.18 9.53 5.92 9.50 4.38 5.86 4.13 5.43 4.34 5.58 5.60
24 7.45 7.52 4.35 4.16 7.48 5.66 5.60 4.31 7.54 5.98 9.69 5.76 9.71 4.33 5.84 3.88 5.13 4.14 5.25 5.28
26 6.70 6.71 4.31 4.22 6.77 5.32 5.12 4.23 6.77 5.36 9.09 5.23 9.10 3.53 5.34 3.75 5.27 4.06 4.95 4.87
27 7.48 7.50 4.67 4.23 7.74 5.80 5.44 4.65 7.70 5.94 9.26 5.70 9.22 3.92 5.95 3.90 5.36 4.20 5.47 5.14
28 7.30 7.00 4.70 4.10 7.05 5.50 5.20 4.70 7.30 5.70 8.20 6.00 8.65 4.30 5.70 4.00 5.25 4.25 5.45 5.50
29 7.60 7.60 4.70 4.02 7.74 5.61 5.45 4.72 7.77 5.92 9.73 5.81 9.70 4.45 5.90 4.01 5.45 4.36 5.48 5.47
30 7.60 7.60 4.78 4.54 7.78 5.78 5.55 4.76 7.77 5.92 9.55 5.81 9.57 4.15 5.91 4.03 5.49 4.55 5.50 5.49
31 7.30 7.52 4.79 4.26 7.41 5.63 5.43 4.61 7.39 5.95 9.43 5.69 9.41 4.35 5.78 4.03 5.39 4.19 5.38 5.40
32 7.53 7.55 4.80 4.62 7.82 5.78 5.50 4.78 7.74 6.03 9.56 5.76 9.51 4.40 5.99 4.04 5.42 4.53 5.55 5.52
33 7.33 7.35 5.54 4.40 7.60 5.63 5.25 4.60 7.54 5.92 9.31 5.80 9.29 5.23 5.92 4.05 5.32 4.25 5.45 5.41
34 7.38 7.50 5.93 4.59 7.50 6.16 5.14 4.67 7.48 6.56 9.03 6.48 9.08 3.99 6.08 4.20 5.35 4.19 5.67 5.42
35 7.65 7.61 5.05 4.33 7.90 5.86 5.40 4.78 7.89 6.07 9.51 6.02 9.54 4.53 6.07 4.05 5.58 4.35 5.72 5.74
36 7.63 7.66 5.03 4.68 7.60 5.81 5.65 4.82 7.61 6.02 9.65 5.95 9.69 4.24 6.07 4.23 5.51 4.63 5.47 5.51
37 7.54 7.53 4.57 4.61 7.75 5.80 5.34 4.78 7.66 5.96 9.45 5.81 9.42 3.88 5.97 3.88 5.34 4.66 5.46 5.42
38 7.50 7.50 4.70 4.50 7.70 5.80 5.40 4.70 7.80 6.00 9.50 5.80 9.50 3.90 6.00 3.90 5.30 4.50 5.50 5.50
39 7.64 7.60 4.74 4.24 7.73 5.71 5.41 4.79 7.76 5.97 9.60 5.69 9.64 4.04 5.94 4.00 5.45 4.29 5.54 5.55
40 7.51 7.51 4.75 4.32 7.70 5.85 5.41 4.86 7.70 6.08 9.49 5.85 9.49 4.12 6.08 3.95 5.40 4.39 5.57 5.59
41 7.61 7.61 4.76 4.63 7.77 5.83 5.39 4.76 7.80 6.00 9.60 5.82 9.65 3.97 6.04 3.96 5.33 4.63 5.46 5.50
42 7.62 7.66 4.89 4.36 7.76 5.87 5.58 4.78 7.79 6.04 9.60 5.91 9.63 4.09 6.01 4.05 5.46 4.31 5.57 5.60
43 7.70 7.70 4.70 4.50 7.80 5.70 5.30 4.70 7.90 6.00 9.90 5.70 10.00 4.10 5.90 3.90 5.30 4.60 5.50 5.50
44 7.45 7.42 4.58 4.16 7.59 5.61 5.29 4.56 7.58 5.78 9.29 5.64 9.39 3.92 5.85 3.88 5.31 4.17 5.36 5.40
45 6.98 7.67 5.09 4.41 6.94 5.93 5.86 4.91 7.90 6.13 9.89 5.98 10.02 4.35 5.72 4.16 5.38 4.29 5.67 5.53
46 7.31 7.56 4.92 4.74 7.79 5.87 5.43 4.82 8.15 6.03 9.64 5.89 9.75 4.07 5.95 4.07 5.42 4.73 5.60 5.63
47 7.55 7.65 4.97 4.41 7.85 6.07 5.69 5.06 7.87 6.30 9.43 6.09 9.46 5.04 6.11 4.26 5.63 4.45 5.72 5.68
48 7.47 7.50 4.83 4.30 7.60 5.73 5.43 4.77 7.59 5.88 9.31 5.78 9.38 4.45 5.78 3.78 5.16 4.05 5.35 5.33
49 7.59 7.59 4.78 4.63 7.72 5.79 5.39 4.74 7.72 6.00 9.52 5.80 9.52 4.02 5.99 3.98 5.40 4.61 5.46 5.49
51 7.72 7.67 5.25 4.49 7.85 5.92 5.51 4.79 7.83 6.04 9.61 6.23 9.44 4.81 6.15 4.11 5.49 4.24 5.57 5.54
52 7.68 7.74 4.88 4.30 7.90 5.84 5.46 4.85 7.90 6.10 9.71 5.93 9.64 4.04 6.10 4.01 5.46 4.30 5.60 5.57
53 7.64 7.58 5.84 4.50 7.61 6.12 6.16 4.91 7.54 5.98 9.10 5.83 9.24 5.43 5.91 4.83 6.02 4.59 5.82 5.64

Results not provided by Laboratories 25 and 50.

 KALRA: JOURNAL OF AOAC INTERNATIONAL VOL. 78, No.2, 1995 319

Table 5. Collaborative study results for pH measurements of organic soils

Sample

Lab. 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40

6.51 6.34 8.13 6.80 7.66 7.27 5.54 7.61 7.02 7.87 5.49 7.05 6.66 8.09 7.55 6.81 7.23 7.88 6.40 7.57
2 6.03 6.00 8.10 6.60 7.50 7.11 5.12 7.56 6.91 7.84 5.18 6.93 6.64 8.19 7.41 6.67 7.13 7.83 6.16 7.40
3 6.20 6.05 8.00 6.15 7.50 7.10 4.85 7.50 6.90 7.75 4.90 6.85 6.60 8.05 7.40 6.55 7.05 7.80 6.05 7.40
4 5.91 5.97 7.97 6.06 7.41 6.97 4.90 7.43 6.83 7.74 4.91 6.81 6.54 7.99 7.34 6.58 6.99 7.72 5.89 7.29
5 6.18 6.22 7.94 6.37 7.43 6.99 5.18 7.41 6.82 7.76 5.18 6.75 6.53 7.99 7.35 6.47 7.01 7.75 6.24 7.36
6 5.78 5.69 7.30 6.62 7.14 7.07 4.80 7.06 6.95 7.48 4.91 6.57 6.52 7.52 7.39 6.92 6.99 7.54 6.13 7.27
7 6.30 6.17 8.21 6.32 7.56 7.18 5.12 7.54 6.89 7.81 5.02 6.90 6.58 8.12 7.41 6.59 7.13 7.80 6.01 7.38
8 6.13 5.96 8.06 6.47 7.48 7.28 5.19 7.50 7.11 7.91 5.16 6.72 6.63 8.08 7.49 6.97 7.26 7.83 6.31 7.42
9 5.60 5.50 7.60 5.80 7.30 6.50 4.30 7.10 6.60 7.60 4.80 6.30 6.30 7.90 7.20 6.40 6.60 7.40 6.00 7.10
10 6.23 6.14 7.97 6.45 7.23 7.22 5.16 7.44 6.92 7.72 5.26 6.69 6.57 7.85 7.38 6.68 7.12 7.59 6.49 7.36
11 5.24 5.25 7.10 6.60 6.37 6.75 4.63 6.55 6.76 6.93 4.43 5.64 6.60 6.54 6.88 6.66 6.50 6.64 5.22 6.67
12 6.26 6.19 8.18 6.35 7.54 7.19 5.18 7.56 6.99 7.72 5.16 6.97 6.63 8.39 7.43 6.58 7.08 7.81 6.12 7.39
13 5.82 5.59 7.57 5.79 7.32 6.85 4.54 7.30 6.67 7.52 4.54 6.63 6.45 7.63 7.28 6.49 6.81 7.53 5.62 7.25
14 6.45 6.25 8.34 6.33 7.68 7.32 5.25 7.63 7.07 7.88 5.28 7.03 6.76 8.25 7.56 6.74 7.16 7.88 6.31 7.54
15 6.38 6.23 8.20 6.40 7.61 7.25 5.25 7.60 6.97 7.95 5.29 6.80 6.70 8.18 7.48 6.62 7.16 7.96 6.64 7.50
16 6.39 6.17 8.11 6.37 7.64 7.28 5.18 7.58 7.08 7.90 5.17 6.95 6.76 8.10 7.54 6.84 7.24 7.91 6.20 7.56
17 6.54 6.26 7.93 6.44 7.56 7.06 5.17 7.36 6.99 7.76 5.46 6.96 6.68 7.95 7.49 6.77 7.07 7.64 6.30 7.46
18 6.37 6.14 7.87 6.29 7.51 7.08 5.09 7.54 6.86 7.73 5.06 6.99 6.67 8.06 7.41 6.61 7.08 7.73 6.16 7.39
19 5.48 5.44 7.41 6.35 7.33 7.00 5.51 7.28 6.82 7.61 4.49 6.52 6.41 7.55 7.34 6.74 6.86 7.67 5.81 7.28
20 6.14 6.07 8.05 6.28 7.49 7.10 4.96 7.49 6.88 7.77 4.96 6.85 6.56 8.06 7.39 6.63 7.06 7.76 6.02 7.38
21 5.70 5.87 5.97 6.12 7.27 7.14 5.30 7.02 6.78 7.59 5.43 6.35 6.41 7.30 7.32 6.89 7.07 7.44 7.12 7.25
22 6.32 6.14 8.35 6.42 7.59 7.21 5.14 7.52 7.01 7.92 5.12 6.96 6.63 8.36 7.38 6.63 7.10 7.79 6.14 7.38
23 5.99 6.02 7.44 6.55 7.33 7.18 5.32 7.34 6.94 7.82 5.32 6.78 6.67 7.99 7.48 6.87 7.24 7.88 6.35 7.39
24 5.69 5.61 7.60 5.76 7.22 6.86 4.52 7.22 6.67 7.52 4.55 6.58 6.39 7.69 7.11 6.44 6.86 7.54 5.85 7.17
25 6.15 6.00 8.08 6.20 7.54 7.17 4.98 7.53 6.89 7.74 4.96 6.88 6.59 8.04 7.41 6.59 7.06 7.77 6.04 7.38
26 5.18 5.08 6.96 5.70 6.66 6.33 4.84 6.77 6.35 7.12 4.09 5.86 5.75 7.12 6.81 6.23 6.52 6.95 5.64 6.70
27 6.30 6.06 8.06 6.23 7.45 7.07 5.10 7.52 6.85 7.75 5.08 6.84 6.57 8.03 7.38 6.54 7.02 7.74 6.02 7.33
28 6.20 6.05 7.60 6.15 7.15 6.90 5.15 7.15 6.70 7.40 5.10 6.70 6.40 7.70 7.10 6.45 6.80 7.40 6.10 7.10
29 5.78 6.56 7.80 5.85 7.40 6.89 4.60 7.44 6.72 7.77 4.60 6.70 6.46 7.98 7.34 6.42 6.86 7.69 5.75 7.34
30 6.29 6.12 8.18 6.35 7.53 7.16 5.09 7.51 6.95 7.94 5.12 6.90 6.61 8.20 7.42 6.62 7.15 7.97 6.14 7.40
31 6.02 5.85 7.88 6.08 7.38 7.00 5.06 7.49 6.86 7.71 5.05 6.81 6.63 7.94 7.42 6.71 7.05 7.70 6.08 7.35
32 6.21 6.04 8.09 6.31 7.52 7.09 5.00 7.51 6.89 7.90 5.05 6.88 6.60 8.12 7.40 6.62 7.11 7.85 6.09 7.41
33 6.02 6.00 7.99 6.22 7.46 7.12 4.87 7.46 6.96 7.76 4.93 6.87 6.64 8.05 7.42 6.72 7.11 7.76 6.06 7.40
34 6.15 5.99 8.01 6.30 7.46 7.07 5.10 7.49 7.77 5.15 7.03 7.04 6.76 8.07 7.36 6.84 7.09 7.74 6.18 7.35
35 6.23 6.09 8.20 6.30 7.56 7.19 5.08 7.58 6.97 7.91 5.12 6.88 6.65 8.22 7.45 6.69 7.16 7.85 6.18 7.44
36 6.10 6.01 8.10 6.31 7.53 7.77 4.98 7.50 7.00 7.94 5.14 6.88 6.63 8.16 7.43 6.72 7.16 7.95 6.18 7.41
37 6.28 6.17 8.13 6.33 7.47 7.02 5.02 7.45 6.85 7.79 5.01 6.83 6.62 8.11 7.40 6.57 7.05 7.84 6.10 7.34
38 6.30 6.20 8.20 6.30 7.60 7.20 5.10 7.60 7.00 8.00 5.10 7.00 6.70 8.20 7.40 6.70 7.20 8.00 6.20 7.40
39 6.84 6.31 8.28 6.74 7.60 7.31 5.23 7.56 7.05 7.86 5.23 6.93 6.67 8.20 7.44 6.68 7.14 7.84 6.17 7.43
40 6.29 6.10 8.15 6.27 7.57 7.13 5.01 7.57 6.96 7.81 5.04 6.94 6.64 8.15 7.46 6.62 7.05 7.83 6.10 7.44
41 6.11 5.94 8.06 6.16 7.50 7.06 4.95 7.51 6.83 7.89 4.95 6.85 6.58 8.08 7.40 6.57 7.06 7.89 5.97 7.42
42 6.35 6.08 8.10 6.32 7.67 7.25 4.99 7.64 7.02 7.89 5.05 6.95 6.69 8.09 7.51 6.73 7.20 7.90 6.19 7.49
43 6.20 6.00 8.10 6.20 7.60 7.10 5.10 7.60 6.90 8.10 5.10 6.90 6.50 8.40 7.40 6.50 7.10 8.10 6.00 7.50
44 6.35 6.06 8.14 6.52 7.42 7.17 5.28 7.38 6.91 7.78 5.14 6.70 6.56 8.12 7.37 6.65 7.08 7.79 6.22 7.31
45 6.63 6.38 6.92 6.83 6.93 6.78 5.45 6.84 6.86 7.75 5.24 6.59 6.43 8.23 7.42 6.57 6.90 7.80 6.29 7.41
46 6.25 6.04 8.11 6.51 7.62 7.36 5.08 7.59 6.96 7.95 5.17 6.77 6.61 8.14 7.48 6.65 7.11 7.91 6.07 7.40
47 6.43 6.28 8.22 6.50 7.64 7.21 5.26 7.68 7.09 7.94 5.25 7.06 6.75 8.30 7.56 6.74 7.22 7.93 6.29 7.49
48 6.34 6.20 8.19 6.42 7.56 7.23 5.22 7.53 7.00 7.86 5.24 6.94 6.66 8.20 7.43 6.69 7.11 7.84 6.26 7.41
49 6.38 6.10 8.00 6.38 7.48 7.04 5.10 7.41 6.88 7.82 5.18 6.83 6.52 7.98 7.41 6.59 7.01 7.82 6.10 7.40
50 6.12 6.04 8.17 6.23 7.52 7.09 5.02 7.51 6.91 7.93 5.02 6.87 6.58 8.13 7.38 6.61 7.06 7.93 6.08 7.38
51 6.53 6.36 8.22 6.57 7.66 7.23 5.50 7.64 7.03 7.88 5.53 7.00 6.72 8.24 7.52 6.74 7.20 7.88 6.37 7.49
52 6.40 6.20 8.30 6.37 7.60 7.22 5.19 7.61 6.97 7.88 5.19 6.90 6.62 8.27 7.51 6.74 7.15 7.80 6.26 7.46
53 6.27 6.23 7.92 6.60 7.46 7.14 5.41 7.39 7.02 7.64 5.15 6.88 6.75 7.88 7.45 6.95 7.03 7.64 6.06 7.00
320 KALRA: JOURNAL OF AOAC INTERNATIONAL VOL. 78, NO.2, 1995
All laboratories infonned us that all 80 bags containing test
samples were received intact. All 53laboratories were familiar
with soil-to-liquid suspension methods. Five laboratories indi
cated that they did not have any experience with the saturated
paste method.
Most of the participants used a combination electrode, while
some used a glass electrode and a calomel reference electrode.
Two laboratories reported that it was difficult to obtain a stable
reading when using the method for mineral soils (due to lack
of a significant amount of supernatant liquid), while the
method for saline-sodic soils gave stable readings. Ten labora
tories found it necessary to tilt beakers when measuring pH by
the method for mineral soils in order to cover the junction of
the combination electrode by the supernatant liquid. Increasing
the amount of soil to 20 g and the volume of water or CaCl2
solution to 20 mL would have eliminated that problem.
One laboratory reported that readings from the method for
organic soils were less stable than from the methods for mineral
and saline-sodic soils. When using the saline-sodic soils
method, most of the collaborators took readings 1 h after pre
paring the saturated paste. One laboratory reported that there
was no difference in the readings taken at 1 , 1 . 5, or 2 h after the
preparation of saturated paste.
There are no potential hazards in handling reagents, sam
ples, or buffer solutions. None of the participating laboratories
provided any comments regarding the safety aspects of the col
laboratively studied methods.
Recommendation
On the basis of the results of this study it is recommended
that the methods for measurement of pH of mineral, saline-so
dic, and organic soils be adopted ftrst action.
Acknowledgments
The Associate Referee is grateful to the Soil Science Society
of America (SSSA) and the AOAC INTERNATIONAL for the
opportunity to coordinate this study. Thanks are also due to the
Canadian Forest Service for its cooperation. I thank the follow
ing individuals for their assistance at different stages of the
study, whose help and cooperation have been of vital impor
tance to this collaborative study: AOAC Methods and Safety
Committees; Nat B. Dellavalle; Editors of Agronomy News and
The Referee; Thomas L. Jensen and Charles L. Focht (Succeed
ing General Referees for Nutrients in Soils); 1. Benton Jones,
Jr; Fred Kaisaki; John 1. Mortvedt (Chainnan) and other mem
bers of the SSSA S889 Committee: Joan K. Bartz (also SSSA
liaison to AOAC INTERNATIONAL), Boyd G. Ellis, Ellis G.
Knox, Ted R. Peck, and Dean E. Wesley; Daniel H. Mowrey
(Committee Statistician); Julie Nonnan and Lucyna Kurtyka
(Succeeding Methods Program Coordinators); D.G. Maynard;
John Shuya; Sheldon Radford; Joe Crumbaugh; SSSA Re
viewers: SJ. Donohue, Mark A. Flock, Gordon V. Johnson,
John L. Kovar, and Dean E. Wesley; Harold C. Thompson, Jr
(Chainnan of the Methods Committee on Feeds, Fertilizers and
Agricultural Related Materials); and the following collabora
tors:
Donna Collins, W.M. Ward Technical Services Laboratory,
Manitoba Environment, Winnipeg, MB, Canada
Clive Dawson, B.c. Ministry of Forests, Research Labora
tory, Victoria, BC, Canada
Brian Douglas, P.E.I. Soil and Feed Testing Laboratory,
Charlottetown, PEl, Canada
Brian G. Drought, Soil Science & Agricultural Engineering,
Agriculture Canada, Research Station, Summerland, BC, Can
ada
Lloyd Hodgins, Saskatchewan Soil Testing Laboratory,
University of Saskatchewan, Saskatoon, SK, Canada
P.M. Kelly, Chemical and Geological Laboratories, Cal
gary, AB, Canada
John Konwicki, Department of Soil Science, Faculty of Ag
riculture and Forestry, University of Alberta, Edmonton, AB,
Canada
Grant Kowalenko, Agriculture Canada, Research Station,
Agassiz, BC, Canada
Ian Murchison, Agriculture Canada, Research Station,
Brandon, MB, Canada
Anne Neary, Ministry of Environment, Dorset, ON, Canada
Randy Neumann, and John Ashworth, Norwest Laborato
ries, Edmonton, AB, Canada
Rosalind Olive, Soil and Plant Testing Laboratory, Univer
sity of New Brunswick, Hugh John Flemming Forestry Centre,
Fredericton, NB, Canada
Liz Pastorek, and Jane Trush, Laboratory Services Branch,
Ministry of Environment, Rexdale, ON, Canada
Terry Peel, Econotech Services Ltd., New Westminster, BC,
Canada
Jo Ramakers, Great Lakes Forestry Centre, Canadian Forest
Service, Sault Ste. Marie, ON, Canada
Vernon Rodd, Nappan Experimental Farm, Nappan, NS,
Canada
Rod Schultz, and Gerry Lutwick, Alberta Environment,
Lethbridge, AB, Canada
Regis Simard, Agriculture Canada, Research Station,
Sainte-Foy, PQ, Canada
Sen Tran, and Pierre Audesse, MAPAQ, Soils Service,
Sainte-Foy, PQ, Canada
Donald Trenholm, Newfoundland Forestry Centre, Cana
dian Forest Service, St. John's, NF, Canada
Evelyn Turcotte, Petawawa National Forestry Institute, Ca
nadian Forest Service, Chalk River, ON, Canada
Ann Van Niekerk, Paciftc Forestry Centre, Canadian Forest
Service, Victoria, BC, Canada
Joel Villanueva, and P.N. Vijan, Alpha Laboratories, Inc.,
Don Mills, ON, Canada
Chang Wang, Centre for Land and Biological Resources
Research, Central Experimental Farm, Ottawa, ON, Canada
Paul Yeung, Alberta Environmental Centre, Vegreville, AB,
Canada
H.P. Agrawal, Department of Soil Science and Agricultural
Chemistry, Banaras Hindu University, Varanasi, India
 KALRA: JOURNAL OF AOAC INTERNATIONAL VOL. 78, No. 2, 1995 321

R.S. Singh,Central Research Laboratory,Udai Pratap Col W. Shaw Reid,CU Nutrient Analysis Laboratory,Cornell
lege,Varanasi,India University,Department of Soil,Crops and Atmosperic Sci
Zev Gerstl,Agricultural Research Organization,The Vol ences,Ithaca,
cani Center,Institute of Soils & Water,Bet Dagan,Israel Janet Sorrels, Agrico Agronomic Services Laboratory,

Earl Allen,Department of Agronomy,Oklahoma State Uni Washington Court House,OH

versity,Stillwater,OK M. Ray Tucker,North Carolina Department of Agriculture,

Vernon W. Case,University of Kentucky,Soil Testing Raleigh,NC

Laboratory,Lexington,KY Darryl D. Warncke,MSU Soil Testing Laboratory,Michi

gan State University,East Lansing,MI
Sherry M. Combs,University of Wisconsin,Department of
Maurice E. Watson,Research Extension Analytical Labora
Soil Science,Madison,WI
tory,Ohio State University,Wooster,OH
Joe Denning,University of Nebraska,Lincoln,NE
Larry Wikoff, Minn. Valley Testing Laboratory,Grand
SJ. Donohue, Soil Testing Laboratory, VIrginia Tech,
Forks,ND
Blacksburg,VA
Mark A. Flock,Brookside Farms Laboratory Association,
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Reprinted from the Journal of AOAC International

Vol. 78, No. 2, 1995
322 K-\LRA: jOl!RNAL OF AOAC I:--'IERNATIONAL VOL. 78. No. 2. 1 995
Appendix: Descriptions of Soils Used in the Collaborative Study
for pH Measurementsa
Halii Series
Clnssification: Clayey, fefitic, isothennic Typic Gibbsihumox.
Location: Island of Kauai, Hawaii, University of Hawaii
Wailua Experiment Station, Wailua, Kauai, edge of experimen
tal maize field. approximately 270 m northwest of Station of
fice and approximately 35 m east of dirt road along western
portion of ridge: latitude 2204' 1 7''N, longitude 1 5924'03"W.
Vegetation: Grassy area adjacent to experimental maize
field; Kaimi clover (Desmodium canum), Hilograss (Paspalum
conjugatum), Dallisgrass (Paspalum dilatatum), and rattail
grass (Sporobolus africanus).
Climate: Mean annual rainfall, 2500 mm, mean annual tem-
perature. 20e.
Parent material: Residuum from melilite nepheline basalt
Physiography: Gently sloping upland ridge.
Relief Convex side slope of ridge.
Slope: 3%.
Permeability: Moderately rapid.
Drainage: Well drained.
Moisture: Moist.
Descnbed by: H. Ikawa.
Collected by: H. Ikawa, lR. Gordines, and K. Kagihara.
Date sampled: March 19, 1 9 8 1 .
Remarks: Colors are for moist soil. Textures are "apparent
field textures."
Ap---3
-O- 5 cm; dark brown (7.5YR 3/2) gravelly silty clay
loam; moderage very fine and fme subangular blocky struc
ture; friable, sticky, plastic, many very fme roots; many very
fine pores; lower portion of horizon has many iron concretions,
mostly ranging in size 1-2 mm., some as large as I cm; few
rock fragments, mostly 2-3 cm. occasionally 5-10 cm; very
strongly acid (pH 5.0); abrupt smooth boundary.
Houghton Series
The Houghton series is a member of the euic, mesic family
of Typic Medisaprists. The soil formes chiefly in herbaceous
organic deposits more than 5 1 in. thick. The surface 0-12 in.
layer is dominated by black highly decomposed organic mate
rial, subsurface 1 2-35 in. layer is dark reddish brown and black
highly decomposed organic material and the bottom layer is
dark reddish brown highly decomposed organic material. The
soil is about neutral throughout.
Type location: Clinton County, Ml; 1 00 ft west of farm lane
at comer where lane turns north; SEV4, SWV4, SWV4, Sec. 1 1 ,
Bath Township; on Michigan State University muck farm.
Typifying pedon: Houghton muck-<:ultivated. (Colors are
for moist soils unless otherwise stated.)
Oal-D-9"-Black (7.5YR 210) broken face and rubbed
sapric material; about 5% fiber, a trace rubbed; weak coarse
subangular blocky structure : neutral (pH 7.0 in KC1); abrupt
smooth boundary.
0a2-9- 1 3"-Black (7.5YR 2/0) broken face very dark
brown (7.5YR 212) rubbed sapric material; about 5 % fiber, a
trace rubbed; weak medium granular structure; neutral (pH 7.0
in KC1); abrupt smooth boundary.
0a3-1 3-24"-Dark reddish brown (5YR 3/2) broken face
dark reddish brown (5YR 212) rubbed sapric material; about
1 5% fiber, less than 5% rubbed; massive, breaking to thick
platy fragments; neutral (pH 7.0 in KCl); abrupt smooth
boundary.
Oa4-24-32"-Black (5YR 21 1 ) broken face and rubbed
sapric material; about 10% fiber. a trace rubbed; massive; few
woody fragments; neutral (pH 7.0 in KC1); clear wavy bound
ary.
OaS-32-48"-Dark reddish brown (5YR 212) broken face
black (5YR 211) rubbed sapric material about 20% fiber, less
than 10% rubbed; massive, breaking to thick platy fragments;
neutral (pH 7.0 in KC1); abrupt smooth boundary.
Houston
Soil type: Houston Black clay, 1-3% slopes.
Classification: Udic Pellusterts, fine montmorillonitic, thennic.
Location: Bell County, TX; ca 2 miles south of Temple, in
native pasture in south part of the Blackland Research Center.
In microbasin.
Date sampled: June 3, 1977, sampled in core hole 30 in. in
diameter. Sampled by Robert N. Ramsey.
Physiography: Gently sloping upland. The soil formed in
Taylor Marl of the Upper Cretaceous period.
Sample numbers: National Soil Survey Laboratory (NSSL)
Tex-77-U27-2- 1 -2-3-4.
Pedon description: All 0-36 cm, very dark gray ( 1OYR 3/1)
clay, black ( l OYR 211 ) moist; moderate fme subangular and
angular blocky structure; extremely hard, very firm; common
fine roots; few fragments of snail shells; calcareous, moder
ately alkaline; clear wavy. NSSL-Tex-77-027-2- 1 boundary.
Laurentides
Location: Laurentides Provincial Park, latitude 4716'00"
N, longitude 7 1 9'20" W.
Altitude: 700 m M.S.L.
Landform: Rolling morainal.
Slope: Upper slope, 5%.
Drainage: Well drained.
Vegetation: Abies balsamea L., Betula papyri/era Marsh,
Picea glauca Voss, Picea mariana BSP, Dryopteris spinulosa,
and Oxalis Montana.
Climate: Precipitation, 1 39 cm (47 cm from snowfall).
 KALRA: JOU'1AL OF AOAC I:'oITERNATIONAL VOL. 78. NO. 2. 1 995
Parent material: Glacial till. loamy sand.
Classification : Orthic ferro-humic podzol (Canadian). Hu
mic cryothod (American ).
Laurentides: Ae (A2)' 0-5 cm Gray (7 .5YR 5/0 m). light
gray ( 7 .5YR 7/0 d) loamy sand: single grain to weak fine
subangular: firm in place. friable when removed: few fine and
medium roots: abrupt, wavy to irregular boundary: 3- 1 3 cm
thick: pH 3.9.
Laurentides LFH: 8-0 cm Black ( I 0YR 211 m), very dark
grayish-brown ( lOYR 3/1 d), semi-decomposed to well-de
composed organic matter: fibrous to fine granular: abundant
fine and medium roots; abrupt, smooth boundary, 5-15 cm
thick; pH 3.6.
Malbis Series
Sample number. S76AL-003-1-( l -4).
Representative profile: Malbis fine sandy loam.
Classification: Plinthic Paleudults: tine-loamy, siliceous,
thermic.
Location: Gulf Coast Substation, Baldwin County, AL.
Use of vegetation: Presently used as winter pasture.
Parent rock or regolith: Medium textured Coastal Plain
sediments.
Geomorphology, region: Lower Coastal Plain, MLRA- 133.
Position: Upland.
Elevation: About 150 ft.
Drainage and penneability: Well drained and moderately
permeable to ca 55 in. Moderately slowly permeable below.
Water table and duration: Water table at 55 in. when de-
scribed.
Slope: Less than 1 %.
Effective rooting depth: About 50 in.
Sampled by: B.E llajek, R.L. Guthrie, D.E. Lewis. and L.E
Ratliff.
Date sampled: December 17, 1 976.
Described by: R.L. Guthrie and D.E. Lewis.
B21t-7-27 in.; yellowish brown ( 1 OYR 5/6) loam; weak
medium subangular blocky structure; friable; few fine roots; thin
patchy clay films on faces ofpeds; 5% medium ironstone concre
tions; strongly acid; clear wavy boundary. (S76AL-003-1 -2).
Myaaka
Taxonomic class: Sandy, siliceous, hyperthermic Aeric
Haplaquods.
Location: Pardee County, FL; on a Range Cattle Experi
ment Station, on an ARC pasture 74, 1400 ft north of drainage
canal and 100 west of Hwy 663, NEV4, NWV4, Sec. 33, T. 35;
R 24 E.
Vegetation and use: Slash pine and saw palmetto. Used as
pasture.
Drainage and penneability: Poorly drained. Permeability is
rapid in the surface layer and substratum and moderate or mod
erately rapid in the subsoil.
Parent material: Marine deposits of sandy materials.
313
Samples collected and profile described by: John M. Rob
bins, Jr, Richard D. Ford. SCS. and Tom Hallmark, IFAS. April
6, 1978.
Horizon : A I .
Depth : 0--8 c m (0--3 in.).
Description : Very dark gray ( l OYR 311 crushed) fine sand;
uncrushed colors have a salt and pepper appearance; weak fine
crumbs structure: very friable: matted with many fine and me
dium roots: strongly acid: clear smooth boundary.
Peck 90-9: Flanagan SiCL that is classified as a fine, mont
morillonitic, mesic Aquic Argiudoll that has a water pH of 6 . 1
was circulated as soil No. 90-9 in the Fall 1 990 Split Soil Sam
ple Study, as soil No. 9 1 -4 in the Spring 199 1 , and as soil No.
9 1 -7 in the Fall 199 1 study. This soil came from a field that was
never limed and had not been fertilized with phosphorus or
potassium for 4 years but was fertilized with nitrogen as the
field has grown corn since 1982.
Peck 90-10: Drummer SiCL that is classified as a fine silty,
mixed, mesic, Typic Haplaquoll that has a water pH of 5.9 was
circulated as soil No. 90- 10 in the Fall 1 990 Split Soil Sample
Study, as soil No. 9 1 -5 in the Spring 1 99 1 , and as soil No. 9 1 - 1 0
in the Fall 199 1 study. This soil came from a research plot grass
border area that has not been fertilized or limed for at least
10 years.
Peck 90-11: Harpster SiCL that is classified as a fine silty,
mixed, mesic, Typic Calciaquoll that has a water pH of 7.8 was
circulated as soil No. 90- 1 1 in the Fall 1 990 Split Soil Sample
Study, as soil No. 9 1 - 1 in the Spring 199 1 , and as soil No. 9 1-8
in the Fall 199 1 study. This soil came from the same field as the
Flanagan SiCL previously described.
Peck 90-12: Cisne SiL that is classified as a fine, montrnoril
lonitic, mesil Typic Albaqualf that has a water pH of 4.9 was
circulated as soil No. 90- 1 2 in the Fall 1 990 Split Soil Sample
Study, as soil No. 9 1 -3 in the Spring 199 1 , and as soil No. 9 1 - 1 1
in the Fall 199 1 study.
Saline soil (EC = 4.50 mS/cm)
U.S. Department of Agriculture-Soil Conservation Serv-
ice
NSSL identification No. : 89PO 1 10.
Soil survey No.: S88-ID-029-012-A.
Location: 227- 15; 280'E and 1 200' S of NW corner of sec-
tion 15.
Classification: Fine silty, mixed, frigid Typic Natrixeralf.
Physiography: Flood plain.
Slope Characteristics: 00 1 % south west facing undulating.
Elevation: 1502 m MSL.
Hydraulic conductivity: Moderately low.
Drainage class: Well drained.
Erosion: Slight.
Parent material: Alluvium material.
Described by: Michael Cook.
Date sampled: August 1 988.
324 K>.LRA: JOURNAL OF AOAC b'TERNATlONAL VOL. 78. NO. 2. 1 995

Notes: Vegetation-greasewood.
A I-4-5 cm: dark brown ( l OYR 3/3) loam; pale brown
( l OYR 6/3) dry; strong very tine platy structure: soft. very fri
able. slightly sticky, slightly plastic: common very fine roots:
common very fine vesicular pores: 89094 1 ; slightly efferves
cent: abrupt smooth boundary.

" Provided by F. Kaisaki. except for Peck 90-9. 90- 10. 90- 1 1 . and
90- 1 2 samples.
/) Details received from TR. Peck.