Designation: C 1580 – 09

Standard Test Method for

Water-Soluble Sulfate in Soil1
This standard is issued under the fixed designation C 1580; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 4. Apparatus
1.1 This test method is for the determination of water- 4.1 Photometer—One of the following, given in order of
soluble sulfate in soils. preference:
1.2 This test method was developed for concentrations of 4.1.1 Nephelometer or turbidimeter,
water-soluble sulfate in soils between 0.02 and 3.33 % sulfate 4.1.2 Spectrophotometer for use at 420 nm with light path of
by mass. 4 to 5 cm, and
1.3 This test method does not determine sulfur in any form 4.1.3 Filter photometer with a violet filter having a maxi-
except as sulfate. mum near 420 nm and a light path of 4 to 5 cm. Filter
1.4 Some governing bodies regulate the movement of soils photometers and photometric practices prescribed in this test
from one area to another. It is up to the sampler and laboratory method shall conform to Practice E 60; spectrophotometer
to comply with all regulations. practices shall conform to Practice E 275.
1.5 The values stated in SI units are to be regarded as 4.2 Stopwatch, readable to 0.1 minutes.
standard. No other units of measurement are included in this 4.3 Measuring Spoon, capacity 0.2 to 0.3 mL.
standard. 4.4 Drying oven, capable of continuously heating at 110 6
1.6 This standard does not purport to address all of the 5 ºC.
safety concerns, if any, associated with its use. It is the 4.5 Balance, shall be capable of reproducing results within
responsibility of the user of this standard to establish appro- 0.0002 g with an accuracy of 60.0002 g. Direct-reading
priate safety and health practices and to determine the balances shall have a sensitivity not exceeding 0.0001 g.
applicability of regulatory limitations prior to use. Conventional two-pan balances shall have a maximum sensi-
bility reciprocal of 0.0003 g. Any rapid weighing device that
2. Referenced Documents may be provided, such as a chain, damped motion, or heavy
2.1 ASTM Standards:2 riders, shall not increase the basic inaccuracy by more than
C 114 Test Methods for Chemical Analysis of Hydraulic 0.0001 g at any reading and with any load within the rated
Cement capacity of the balance.
D 1193 Specification for Reagent Water 4.6 Stirrer, magnetic variable speed, with a TFE-
E 60 Practice for Analysis of Metals, Ores, and Related fluorocarbon coated magnetic stirring rod or an overhead stirrer
Materials by Molecular Absorption Spectrometry with a propeller.
E 275 Practice for Describing and Measuring Performance
of Ultraviolet and Visible Spectrophotometers 5. Reagents and Materials
5.1 Purity of Reagents—All reagents shall conform to the
3. Significance and Use specifications of the Committee on Analytical Reagents of the
3.1 This test method can be used to determine if soils could American Chemical Society.3
have an adverse reaction with hydraulic cement concrete. 5.2 Purity of Water—Unless otherwise indicated, reference
to water shall be understood to mean reagent water conforming
to Specification D 1193, Type I. Other reagent water types (See
1
This test method is under the jurisdiction of ASTM Committee C09 on Note 1) may be used, provided it is first ascertained that the
Concrete and Concrete Aggregates and is the direct responsibility of Subcommittee
on C09.69 Miscellaneous Tests.
3
Current edition approved April 1, 2009. Published May 2009. Originally Reagent Chemicals, American Chemical Society Specifications, American
approved in 2005. Last previous edition approved in 2005 as C 1580 – 05. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
the ASTM website. MD.

*A Summary of Changes section appears at the end of this standard.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 C 1580 – 09
water is of sufficiently high purity to permit its use without clear. Check the pH of the filtrate using pH paper and, if
adversely affecting the precision and bias of the test method. needed, neutralize each filtrate to pH of 7 6 1 using either 0.1N
HCl or 0.1N NaOH.
NOTE 1—Type II water was specified at the time of round robin testing
of this test method. 8.2 Adjust the temperature of the solution in the volumetric
flasks to between 20 and 25 °C [68 to 77 °F].
5.3 Barium Chloride—Crystals of barium chloride 8.3 Use an aliquot of 10 mL for specimen A1, 20 mL for
(BaCl2·2H2O) screened to 850 to 600 µm. To prepare in the specimen A2, 10 mL for specimen B1, and 20 mL for specimen
laboratory, spread crystals over a large watch glass, desiccate B2. Dilute to a volume of 100 mL in a volumetric flask and
for 24 h, screen to remove any crystals that are not 850 to 600 follow the procedure below or Test Methods C 114. Pour the
µm, and store in a clean, dry jar. 100 mL into a 250 mL beaker. Add 5.0 mL of conditioning
5.4 Conditioning Reagent—Place 30 mL of concentrated reagent. Mix by stirring with a stir bar and magnetic stirrer.
hydrochloric acid (HCl, sp gr 1.19), 300 mL reagent water, 100 Add 0.3 g of the prepared BaCl2 crystals using a measuring
mL 95 % ethanol or isopropanol and 75 g sodium chloride spoon and start the timer.
(NaCl) in a container. Add 50 mL glycerol and mix. 8.4 Stir exactly 1.0 min, at the same constant speed for all
5.5 Sulfate Solution, Standard (1 mL = 0.100 mg SO4)— determinations.
Dissolve 0.1479 g of anhydrous sodium sulfate (Na2SO4) in 8.5 Remove the beaker from the stirrer, pour solution into
water, and dilute with water to 1 L in a volumetric flask. the cell, and put the cell into the photometer. Record the
5.6 pH paper, readable to at least 0.5 pH units. turbidity at 4.0 min after pouring the solution into the cell.
5.7 Sodium Hydroxide, (0.1N)—Dissolve 4 g of sodium 8.6 Determine the mg of SO4 from the calibration curve.
hydroxide (NaOH) in water and dilute with water to 1L
5.8 Hydrochloric Acid (0.1N)—Dilute 8.6 mL of concen- 9. Calculation or Interpretation of Results
trated hydrochloric acid (HCl sp gr 1.19) to 1L with water 9.1 Calculate the sulfate content (% by mass) for each
specimen as follows:
6. Permissible Variations ·
6.1 Both the referee method and qualified methods as 2.5*M
P 5 A*W (1)
described in Test Methods C 114 are permissible as alternatives
to the turbidimetric procedure.
Where:
P = % SO4 in dried soil
7. Calibration and Standardization
M = mg/L of SO4 calculated from calibration curve
7.1 Prepare standards by diluting 0.0, 2.0, 5.0, 10.0, 15.0, W = mass of soil placed into 400 mL beaker, in g
20.0, 30.0, and 40.0 mL of standard sulfate solution with water A = volume of aliquot specimen, in mL
to 100-mL volumes in volumetric flasks. These solutions will 9.2 Limits of values for results to be valid. (See Note 3)
have sulfate ion concentrations of 0.0, 2.0, 5.0, 10.0, 15.0, 20.0, Specimen Lower Limit Upper Limit
30.0, and 40.0 mg/L, respectively. Follow the procedure given A1 0.04% 0.33%
A2 0.02% 0.17%
in Section 8 using appropriate amounts of the standard sulfate B1 0.41% 3.33%
solution prepared in accordance with 5.5 and prepare a B2 0.21% 1.67%
calibration curve showing sulfate ion content in mg/L plotted
1. Determine which results fall within the above limits
against the corresponding photometer readings.
2. Discard those that do not
7.2 A separate calibration curve must be prepared for each
3. Average all results that comply
photometer and a new curve must be prepared if it is necessary
to change the cell, lamp, or filter, or if any other alterations of NOTE 3—These values were derived from the limits on the sulfate test
instrument or reagents are made. Check the curve with each of 5 to 40 mg/L, and a solubility of sulfate of 1.6 g/L at pH 7 when calcium
series of tests by running two or more solutions of known sulfate is present. The method is not applicable for soils outside this range.
For those samples, see the Annex.
sulfate concentrations in the range of 5 to 40 mg SO4/L.
NOTE 2—The slope of the curve may not be linear below 5 or above 40 10. Report
mg SO4/L for this method. 10.1 Report the average obtained as % sulfate by mass of
sample. If milligrams sulfate in kilograms of soil (mg SO4/kg
8. Procedure soil) is desired, multiply % sulfate by 10 000. Report results to
8.1 Collect at least 100 g of representative soil for analysis. nearest 0.01 % or 100 mg/kg.
Dry the sample for 18 to 24 h at 110 °C. Crush to pass a 600
µm sieve. In a 400 mL beaker labeled Sample A, put a sample 11. Precision and Bias
consisting of approximately 30 g. In a second 400 mL beaker 11.1 Precision—The standard deviation was found to vary
labeled Sample B, place a sample of approximately 3 g. Record with concentration, so therefore, a coefficient of variation was
the mass of each sample to the nearest 0.001 g. Add 250 mL of used for the precision statement. The single operator coefficient
deionized water to each beaker, and stir on a magnetic stirrer of variation was found to be 4.4 %. Therefore, results of two
for at least 1.0 h but no more than 1.2 h. Filter the extraction properly conducted tests by the same operator on the same
through two dry medium texture filter papers under suction. Do material should not differ by more than 12.4 % of their
not wash the residue. Repeat the filtration if solution is not average. The multilaboratory coefficient of variation was found

2
 C 1580 – 09
to be 21.2 %. Therefore, results of two different laboratories on 12. Keywords
identical samples of a material should not differ from each
12.1 hydraulic cement; soil; Sulfate; turbidimeter
other by more than 60 % of their average.
11.2 Bias—Since there is no accepted reference material
suitable for determining bias, bias can not be determined.

ANNEX

(Mandatory Information)

A1. REDUCING THE NUMBER OF SUB-SAMPLES AND SAMPLES OUT OF COMPLIANCE

A1.1 This procedure was written to accommodate labora- sample masses and/or dilutions can be used. If this procedure
tories that are not familiar with the soil under test. If prior is followed, then the mg SO4 from the turbidimeter reading
knowledge is available, a lesser number of sub-samples, and/or shall be maintained within 5 to 40 mg/L. If another procedure
dilutions may be used. is used, then validation shall be provided showing that the
A1.2 If a sample falls above 3.33 % sulfate, then different results are within the linear range of the calibration.

SUMMARY OF CHANGES

Committee C09 has identified the location of selected changes to this test method since the last issue,
C 1580 – 05, that may impact the use of this test method. (Approved April 1, 2009)

(1) Revised 8.1.

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