ASTM D4542-22

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4542 − 15 D4542 − 22
Standard Test Methods for
Pore Water Extraction and Determination of the Soluble Salt
Content of Soils by Refractometer
This standard is issued under the fixed designation D4542; 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*
1.1 These test methods cover a rapid procedure for squeezing pore water from finegrainedfine-grained soils for the purpose of
determining the amount of soluble salts present in the extracted pore water.
1.2 These test methods were developed for soils having a water content equal to or greater than approximately 14 %, for example,
marine soils. An extensive summary of procedures for extracting pore water from soils has been presented by Kriukov and
Manheim (1).
1.3 These test methods are not generally applicable for determining the soluble salt content of the pore water extracted from
coarse-grained soils, such as clean sands and gravels.
1.4 Test Method A provides a procedure using a refractometer with a refraction index scale; Test Method B provides a procedure
using a refractometer with a parts per thousand (ppt) scale.
1.5 Units—The values stated in SI units are to be regarded as the standard.
1.6 All observed and calculated values shall conform to the guidelines for significant digits and rounding established in Practice
D6026 unless superseded by these test methods.
1.6.1 The procedures used to specify how data are collected/recorded and calculated in the standard are regarded as the industry
standard. In addition, they are representative of the significant digits that generally should be retained. The procedures used do not
consider material variation, purpose for obtaining the data, special purpose studies, or any considerations for the user’s objectives;
and it is common practice to increase or reduce significant digits of reported data to be commensurate with these considerations.
It is beyond the scope of these test methods to consider significant digits used in analysis methods for engineering data.
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.8 All observed and calculated values shall conform to the guidelines for significant digits and rounding established in Practice
D6026.
This test method is under the jurisdiction of ASTM Committee D18 on Soil and Rock and is the direct responsibility of Subcommittee D18.06 on Physical-Chemical
Interactions of Soil and Rock.
Current edition approved Nov. 1, 2015Aug. 1, 2022. Published December 2015August 2022. Originally approved in 1985. Last previous edition approved in 20072015
as D4542 – 07.D4542 – 15. DOI: 10.1520/D4542-15.10.1520/D4542-22.
The boldface numbers in parentheses refer to the list of references appended to this standard.
*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
D4542 − 22
1.8 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D653 Terminology Relating to Soil, Rock, and Contained Fluids
D3740 Practice for Minimum Requirements for Agencies Engaged in Testing and/or Inspection of Soil and Rock as Used in
Engineering Design and Construction
D4753 Guide for Evaluating, Selecting, and Specifying Balances and Standard Masses for Use in Soil, Rock, and Construction
Materials Testing
D6026 Practice for Using Significant Digits and Data Records in Geotechnical Data
E832 Specification for Laboratory Filter Papers
2.2 Federal Document:
GG-S-945a Specification for Syringe and Needle, Disposable, Hypodermic, Sterile, Single Injection
3. Terminology
3.1 Definitions:
3.1.1 For definitions of common technical terms used in this standard, refer to Terminology D653.
3.2 Acronyms:
3.2.1 ppt, n—parts per thousand
4. Significance and Use
4.1 The soluble salt content may be used to correct the index properties of soils such as water content, void ratio, specific gravity,
degree of saturation, and dry density).density.
4.2 Minimize the time period between sampling and testing to reduce chemical changes, which may occur within the soil sample.
NOTE 1—The quality of the result produced by this standard is dependent on the competence of the personnel performing it, and the suitability of the
equipment and facilities used. Agencies that meet the criteria of Practice D3740 are generally considered capable of competent and objective
testing/sampling/inspection/etc. Users of this standard are cautioned that compliance with Practice D3740 does not in itself ensure reliable results.
Reliable results depend on many factors; Practice D3740 provides a means of evaluating some of those factors.
NOTE 2—Hulbert and Brindle (2) and Torrance (3) have shown that prolonged storage should be avoided as unpredictable and non-reproducible chemical
changes may occur.
NOTE 1—The quality of the result produced by this standard is dependent on the competence of the personnel performing it, and the suitability of the
equipment and facilities used. Agencies that meet the criteria of Practice D3740 are generally considered capable of competent and objective
testing/sampling/inspection/etc. Users of this standard are cautioned that compliance with Practice D3740 does not in itself assure reliable results. Reliable
results depend on many factors; Practice D3740 provides a means of evaluating some of those factors.
5. Apparatus
5.1 Refractometer—A temperature compensated refractometer scaled to either index of refraction (Method A) or ppt (parts per
thousand). (Method B). A typical hand held refractometer is shown in Fig. 1.
5.2 Soil Press—The apparatus shall conform to the example shown in Fig. 2. It and should be constructed from material
appropriate for the application and chemically compatible with the material being tested. Use flexible TFE-fluorocarbon gaskets
on each side to prevent soil/mud from circumventing the stainless steel wire screen.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from Naval Publications and Forms Center, 5801 Tabor Ave., Philadelphia, PA, 19120.
D4542 − 22
FIG. 1 Typical Hand-Held Refractometer
5.3 Syringe—A 25-cm25 cm disposable syringe without needle, in accordance with Fed. Std. GG-S-945a.
5.4 Balance—A balance capable of determining massconforming to the requirements of Guide D4753 with and having a
readability without estimation of 60.010.01 g.
5.5 Filter Paper:
5.5.1 A general purpose quantitative filter paper in accordance with Specification E832, Type II, Class F, for medium crystalline
precipitates in the size range from 5 to 10 μm, with an ash content of 0.13 mg/12.5-cm circle. Cut filter paper to a diameter of 55
mm.
5.5.2 A general purpose quantitative filter paper in accordance with Specification E832, Type II, Class G, for fine crystalline
precipitates in the size range from 0.45 μm, with an ash content of 0.13 mg/12.5-cm circle. Cut filter paper to a diameter of 25
mm.
5.6 Refrigerator—Cooling unit capable of maintaining a uniform temperature between 1 and 5°C.
5.7 Micro-Syringe Filter Holder—A device made of stainless steel to filter a liquid directly from a syringe.
5.8 100-mL Polyethylene or Glass Bottle and Cap. Bottle—A clean 100 mL polyethylene or glass bottle with cap.
5.8.1 A clean bottle is one that is washed with detergent and rinsed with tap water. Then rinsed once with diluted HCl (1:10), twice
with distilled water, and then drained thoroughly.
5.9 Miscellaneous Supplies—Distilled water, alcohol, diluted HCl (1:10), detergent, and optional sterile bags for sample storage
(seeItems such as steel wool, soap/detergent, compressed air, and sterile plastic bags may be useful, necessary, 8.6).or both.
6. Reagents
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytic Reagents of the American Chemical Society, where such
specifications are available.
6.1.1 Hydrochloric Acid diluted 1:10
An apparatus such as the stainless steel Millipore Micro-Syringe Filter Holder XX30-025-00 is satisfactory for this purpose.
Reagent Chemicals, American Chemical Society Specifications,” American Chemical Society, Washington, DC. For suggestions on the testing of reagents lot listed by
the America Chemical Society, see “Reagent Chemicals and Standards,” by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States Pharmacopeia.”
D4542 − 22
FIG. 2 Example of Heavy Duty Soil Press
6.1.2 Alcohol
6.1.3 Chromic acid
6.1.4 Acetone
6.2 Distilled water
7. Preparation of Apparatus
7.1 Soil Press—Wash the parts of the soil press thoroughly. Rinse twice with distilled water and dry. Rust should not be Make sure
there is no rust present, especially inside or around the top of the cylinder. If rust is present, scrub gently with steel wool and soap
or chromic acid. Rinse well with tap water and then twice with distilled water and dry.
7.1.1 If the soil press parts have been coated with rust preventer, wash them with alcohol and rinse once with tap water and twice
with distilled water.
7.1.2 Dry by a method that will not contaminate the press. Clean compressed air, oven or air drying, or rinsing with acetone
followed by air drying are acceptable.
7.1.3 Assemble the soil press.
7.2 If the press parts have been coated with rust preventer, wash them with alcohol and rinse once with tap water and twice with
distilled water.
7.3 Dry by a method that will not contaminate the press. Clean compressed air, oven or air drying, or rinsing with acetone followed
by air drying are acceptable.
7.2 Refractometer—Assemble the press.Thoroughly wash with distilled water and dry the refractometer.
NOTE 3—To prevent mud from circumventing the stainless steel wire screen, use flexible TFE-fluorocarbon gaskets on each side.
D4542 − 22
8. Sampling and Test Specimen SqueezingPreparation
8.1 To reduce the potential for undesirable chemical changes that may occur within the soil, keep the time period between
sampling and testing to a minimum (Note 2).
8.2 Select a representative soil sample of approximately at least 50 g and place into the cylinder on top of a single sheet of 5 to
10-μm (55-mm) filter paper.Class F filter paper cut to a diameter of 55 mm.
8.3 Apply pressure slowly until the first drops of water are expelled, then insert a clean, disposable, syringe (25 mL) in the effluent
passage shown in Fig. 2. This process reduces the amount of air in the syringe and therefore, the amount of evaporation.
8.4 Apply pressure gradually to a maximum of 80 MPa, and hold until no more water is expelled or until the syringe is full (see
Note 43 and Note 54).
8.5 Withdraw the syringe when the pressure is at a maximum and immediately expel the fluid from the syringe through a stainless
steel micro-syringe holder, fitted with fresh 0.45-μm (25-mm) filter paper, Class G filter paper cut to a diameter of 25 mm, into
a clean 100-mL bottle (see bottle. Note 6). Cap the bottle. Expose the collected water to the atmosphere as little as possible.
8.6 Repeat 8.18.2 – 8.48.5, using the same syringe and filter if additional water is needed for experimentation and can be collected.
needed. Usually about 25 mL of pore water maycan be collected from 50 g of soil (see (Note 75 and Note 86). Store the water
at a temperature between 1 and 5°C (see Note 97 and Sections 9 and 10).
8.7 Remove the soil from the press. If additional tests are anticipated, store soil in a sterile plastic bag at a temperature between
1 and 5°C (see Note 97).
NOTE 2—Hulbert and Brindle (2) and Torrance (3) have shown that prolonged storage should be avoided as unpredictable and nonreproducible chemical
changes may occur.
NOTE 3—Only a few drops (0.05 mL) of pore fluid are required to conduct the soluble salt determination by refractometer. It is recommended that 25
mL of pore water be collected, if possible, to allow for retesting or additional tests, or both.
NOTE 4—Kriukov and Komarova (4) have found that at a pr
...