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ASTM D7458-08

(Test Method)

Standard Test Method for Determination of Beryllium in Soil, Rock, Sediment, and Fly Ash Using Ammonium Bifluoride Extraction and Fluorescence Detection

Standard Test Method for Determination of Beryllium in Soil, Rock, Sediment, and Fly Ash Using Ammonium Bifluoride Extraction and Fluorescence Detection

SIGNIFICANCE AND USE
Exposure to beryllium can cause a potentially fatal disease, and occupational exposure limits for beryllium in air and on surfaces have been established to reduce exposure risks to potentially affected workers (2, 3). Measurement of beryllium in matrices such as soil, rock, sediment, and fly ash is important in environmental remediation projects involving beryllium contamination (4) and for establishment of background levels of beryllium at sites where anthropogenic beryllium may have been used (2). Sampling and analytical methods for beryllium are needed in order to meet the challenges relating to exposure assessment and risk reduction. Sampling and analysis methods, such as the procedure described in this test method, are desired in order to facilitate measurements of beryllium that can be used as a basis for management of remediation projects and protection of human health.
This test method can be used for purposes such as environmental remediation projects where beryllium is a contaminant of concern. It is also useful for characterization of levels of beryllium in soil at sites where beryllium is in mining or manufacturing applications, and for determination of background levels of beryllium in soil.
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 D 3740 are generally considered capable of competent and objective testing, sampling, inspection, etc. Users of this standard are cautioned that compliance with Practice D 3740 does not in itself assure reliable results. Reliable results depend on many factors; Practice D 3740 provides a means of evaluating some of those factors.
SCOPE
1.1 This test method is intended for use in the determination of beryllium in samples of soil, rock, sediment, and fly ash. This test method can be used for purposes such as environmental remediation projects where beryllium is a contaminant of concern. It is also useful for characterization of levels of beryllium in soil at sites where beryllium is in mining or manufacturing applications, and for determination of background levels of beryllium in soil.
1.2 This test method assumes that samples of soil, rock, sediment, or fly ash are collected using appropriate and applicable ASTM International standard practices.
1.3 This test method includes a procedure for on-site extraction (dissolution) of beryllium in dilute ammonium bifluoride, followed by analysis of aliquots of the extract solution using a beryllium-specific fluorescent dye.
1.4 No detailed operating instructions are provided because of differences among various makes and models of suitable fluorometric instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This test method does not address comparative accuracy of different devices or the precision between instruments of the same make and model.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 All observed and calculated values shall conform to the guidelines for significant digits and rounding established in Practice D 6026.
1.6.1 The procedures used to specify how data are collected/recorded, or calculated, in this 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 this standard to consider significant digits used in analytical methods for engineering design.
...

General Information

Status
Historical
Publication Date
30-Sep-2008
ICS
13.080.10 - Chemical characteristics of soils
Technical Committee
D18 - Soil and Rock
Drafting Committee
D18.01 - Surface and Subsurface Investigation
Current Stage
Ref Project

Relations

Referred By
ASTM D8299-19 - Standard Guide for Using Metal Ratios in Soils to Distinguish Between Anthropogenic and Natural Beryllium
Effective Date
01-Oct-2008
Referred By
ASTM D7202-22 - Standard Test Method for Determination of Beryllium in the Workplace by Extraction and Optical Fluorescence Detection
Effective Date
01-Oct-2008

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ASTM D7458-08 - Standard Test Method for Determination of Beryllium in Soil, Rock, Sediment, and Fly Ash Using Ammonium Bifluoride Extraction and Fluorescence DetectionASTM D7458-08 - Standard Test Method for Determination of Beryllium in Soil, Rock, Sediment, and Fly Ash Using Ammonium Bifluoride Extraction and Fluorescence Detection
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ASTM D7458-08 - Standard Test Method for Determination of Beryllium in Soil, Rock, Sediment, and Fly Ash Using Ammonium Bifluoride Extraction and Fluorescence Detection
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D7458 −08
StandardTest Method for
Determination of Beryllium in Soil, Rock, Sediment, and Fly
Ash Using Ammonium Bifluoride Extraction and
1
Fluorescence Detection
This standard is issued under the fixed designation D7458; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope dures used do not consider material variation, purpose for
obtaining the data, special purpose studies, or any consider-
1.1 Thistestmethodisintendedforuseinthedetermination
ations for the user’s objectives; and it is common practice to
of beryllium in samples of soil, rock, sediment, and fly ash.
increase or reduce significant digits of reported data to be
This test method can be used for purposes such as environ-
commensuratewiththeseconsiderations.Itisbeyondthescope
mental remediation projects where beryllium is a contaminant
of this standard to consider significant digits used in analytical
of concern. It is also useful for characterization of levels of
methods for engineering design.
beryllium in soil at sites where beryllium is in mining or
manufacturing applications, and for determination of back- 1.7 Thistestmethodcontainsnotesthatareexplanatoryand
ground levels of beryllium in soil. not part of mandatory requirements of the standard.
1.8 This standard does not purport to address all of the
1.2 This test method assumes that samples of soil, rock,
safety concerns, if any, associated with its use. It is the
sediment, or fly ash are collected using appropriate and
responsibility of the user of this standard to establish appro-
applicable ASTM International standard practices.
priate safety and health practices and determine the applica-
1.3 This test method includes a procedure for on-site ex-
bility of regulatory limitations prior to use. Specific hazards
traction (dissolution) of beryllium in dilute ammonium
associated with performance of this test method are described
bifluoride, followed by analysis of aliquots of the extract
in Section 9.
solution using a beryllium-specific fluorescent dye.
2. Referenced Documents
1.4 No detailed operating instructions are provided because
2
of differences among various makes and models of suitable
2.1 ASTM Standards:
fluorometric instruments. Instead, the analyst shall follow the
D653Terminology Relating to Soil, Rock, and Contained
instructions provided by the manufacturer of the particular
Fluids
instrument. This test method does not address comparative
D1193Specification for Reagent Water
accuracy of different devices or the precision between instru-
D3740Practice for Minimum Requirements for Agencies
ments of the same make and model.
Engaged in Testing and/or Inspection of Soil and Rock as
Used in Engineering Design and Construction
1.5 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this D4840Guide for Sample Chain-of-Custody Procedures
D5730Guide for Site Characterization for Environmental
standard.
Purposes With Emphasis on Soil, Rock, the Vadose Zone
1.6 All observed and calculated values shall conform to the
and Ground Water
guidelines for significant digits and rounding established in
D6026Practice for Using Significant Digits in Geotechnical
Practice D6026.
Data
1.6.1 Theproceduresusedtospecifyhowdataarecollected/
D7202Test Method for Determination of Beryllium in the
recorded, or calculated, in this standard are regarded as the
Workplace Using Field-Based Extraction and Optical
industry standard. In addition, they are representative of the
Fluorescence Detection
significant digits that generally should be retained. The proce-
E177Practice for Use of the Terms Precision and Bias in
ASTM Test Methods
1
ThistestmethodisunderthejurisdictionofASTMCommitteeD18onSoiland
2
Rock and is the direct responsibility of Subcommittee D18.01 on Surface and For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Subsurface Characterization. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved Oct. 1, 2008. Published October 2008. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D7458-08. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7458−08
E691Practice for Conducting an Interlaboratory Study to levelsofberylliuminsoilatsiteswhereberylliumisinmining
Determine the Precision of a Test Method or manufacturing applications, and for determination of back-
E882Guide for Accountability a
...

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5.1 Where sulfates are suspected, subgrade soils should be tested as an integral part of a geotechnical evaluation because the possibility that sulfate induced heave may occur if calcium containing stabilizers are used to improve the soils and sulfate reactions may also cause deterioration in concrete structures. When planning to treat a soil used in construction with lime, testing the soil for water soluble sulfates prior to treatment becomes very important (Note 2).  
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1.1 These methods determine the water soluble sulfate content of cohesive soils used in construction by using the colorimetric technique. Two methods are presented in this standard. Method A is for use in the field and Method B is for use in the laboratory. The colorimetric technique involves measuring the scattering of a light beam through a solution that contains suspended particulate matter. Measurements of sulfate concentrations in construction soils can be used to guide professionals in the selection of appropriate stabilization methods and to assist in assessment of potential deterioration in concrete structures.
Note 1: These test methods are partially based on the research conducted by Texas A & M University.  
1.2 The field method, Method A, is used as a screening test for the presence of sulfates and their concentration. The laboratory method, Method B, provides better resolution than the field method.  
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SIGNIFICANCE AND USE
5.1 The specific gravity value is used in many phase relation equations to determine relative volumes of particle, water, and gas mixtures.  
5.2 The term soil particle typically refers to a naturally occurring mineral grain that is not readily soluble in water. Therefore, the specific gravity of soils that contain extraneous matter (such as cement, lime, and the like) or water-soluble material (such as salt) must be corrected for the precipitate that forms on the test specimen after drying. If the precipitate has a specific gravity less than the parent soil grains, the uncorrected test result will be too low. If the precipitate has a higher specific gravity, then the uncorrected test value will be too high.  
5.3 Heating during drying may diagenetically alter the structure of some clay minerals.3 Therefore caution should be exercised if the mineral composition of a clay test specimen is going to be determined after drying. It is possible to dry the test specimen at a lower temperature. However, the effect on water content4 and hence specific gravity should be investigated. In addition, some materials other than clay may be affected by drying at 110°C, such as gypsum, soils containing organics, fly ash containing residual coal, island sands. Test Method D2216 includes recommendations for drying gypsum using a lower temperature, such as 60°C.
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1.1 This test method covers the determination of the specific gravity of soil solids by means of a gas pycnometer. Particle size is limited by the dimensions of the test specimen container of the particular pycnometer being used.  
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Standard Test Methods for Pore Water Extraction and Determination of the Soluble Salt Content of Soils by Refractometer

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.
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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.  
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SIGNIFICANCE AND USE
5.1 This test method is used to determine the presence and quantity of carbonate in a soil or soft rock specimen in terms of the calcite equivalent. The method is generally intended for use as an index of approximate carbonate content to assist with characterizing marine soils, but can be used for other soils and soft rock. Other test methods exist (such as Method C25 and Test Method D3042) to evaluate calcium carbonate equivalency for purposes of characterizing use of calcareous materials as soil modifiers or agricultural lining materials.  
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1.1 This test method covers the determination of carbonate content of soils and soft rock which can be readily broken down by mechanical effort. It is a gasometric method that uses a simple portable apparatus. Results should be clearly stated as the calcite equivalent in percent because different carbonate species cover a wide range of percent calcite equivalent as shown below for a number of carbonates:    
Species  
Cation  
Calcite
Equivalent, %  
Magnesite  
Mg  
117.0  
Dolomite  
Ca, Mg  
108.6  
Calcite  
Ca  
100.0  
Aragonite  
Ca  
100.0  
Rhodocrosite  
Mn  
87.1  
Siderite  
Fe  
86.4  
Smithsonite  
Zn  
79.8  
Witherite  
Ba  
50.7  
Cerrusite  
Pb  
37.5
For example, a 100 % dolomite would be expected to yield 108.6 % calcite equivalent while 100 % siderite would yield only 86.4 % calcite equivalent. Calcite and aragonite reactions will typically complete within about 10 minutes. This method does not distinguish between the carbonate species and such determination must be made using quantitative chemical analysis methods such as atomic absorption.  
1.2 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses are provided for information only and are not considered standard. Reporting of test results in units other than SI shall not be regarded as nonconformance with this standard  
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SIGNIFICANCE AND USE
5.1 Chronic Beryllium Disease (CBD) and Beryllium Sensitization (Be-S) caused by exposure to anthropogenic Beryllium (A-Be) are a continuing health concern in the nuclear and defense industries. The traditional worker protection strategy has been to compare total Be (T-Be) measurements taken in workplaces with appropriate limits or local background Be measurements. That strategy can be ineffective, however, where naturally occurring Be (N-Be) from local soils can be a non-negligible component of the measured T-Be. N-Be is not known to have adverse health effects. This MRM uses the ratio(s) of measurements of Be with measurements of one or more metals found in background materials, but not likely to be in facilities, to predict the amount of N-Be expected in individual samples based on the measurement(s) of the predictor metal(s) in those samples. The measured T-Be can be compared with the predictions to estimate the amount of A-Be present, if any.  
5.2 In order to use the MRM it is required to identify local sources of N-Be that can be credibly transported into facilities, along with a means of sampling those sources. It would be helpful also to have insight into the metal content of the soils at those sources, to facilitate the identification of candidate predictor metals. Regarding the latter, there are published databases describing the chemistry of surface soils in many regions; however, information found in those databases should be regarded as suggestive, due to the modified sample preparation and analysis methods currently expected to be used because of the need to digest high-fired BeO, one form of A-Be of concern.
SCOPE
1.1 This guide describes a general approach to planning investigations in which the goal is to obtain background measurements of naturally occurring Beryllium (N-Be) along with one or more predictor metals in local soils, to be used in predicting the amount of N-Be expected in samples taken for evaluation using the Metal Ratio Method (MRM). Generally, systematic random sampling is recommended, after which the results are interpreted using statistical methods described in this guide.  
1.2 The total Be (T-Be) measured in evaluation samples can then be compared with the predicted N-Be to estimate the amount of anthropogenic Be (A-Be) present, if any. Several scenarios are discussed in which samples taken and analyzed for T-Be for worker or public protection purposes might include both N-Be and A-Be (see 6.1). This method can allow the N-Be and A-Be components of T-Be measurements to be estimated.  
1.3 Values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This guide offers an organized collection of information or a series of options and does not recommend a specific course of action. This document cannot replace education or experience and should be used in conjunction with professional judgment. Not all aspects of this guide may be applicable in all circumstances. This ASTM standard guide is not intended to represent or replace the standard of care by which the adequacy of a given professional service must be judged, nor should this document be applied without consideration of a project’s many unique aspects. The word “Standard” in the title of this document means only that the document has been approved through the ASTM consensus process.  
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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ASTM D4972-19(Test Method)
Standard Test Methods for pH of Soils

SIGNIFICANCE AND USE
5.1 The pH of the soil is a useful variable in determining the solubility of soil minerals, the mobility of ions in the soil, and assessing the viability of the soil-plant environment.  
5.2 pH measurements are made in both test water and a calcium chloride solution because the calcium displaces some of the exchangeable aluminum. The low ionic strength counters the dilution effect on the exchange equilibrium by setting the salt concentration of the solution closer to that expected in the soil solution. The pH values obtained in the solution of calcium chloride are slightly lower than those measured in water due to the release of more aluminum ions which then hydrolyses. Therefore, both measurements are needed to fully define the character of the soil's pH.  
5.3 For the purpose of these test methods, the test specimens are sieved through a 2.00 mm (No. 10) sieve. Measurements on soils or soil fractions having particle sizes larger than 2.0 mm by these test methods may be invalid. If soil or soil fractions with particles larger than 2.0 mm are used, it must be stated in the report since the results may be significantly different.
Note 2: 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.
SCOPE
1.1 These test methods cover the measurement of the pH of soils that will pass the 2.00 mm (No. 10) sieve. Such measurements are used in the agricultural, environmental, geotechnical, and natural resources fields. This measurement determines the degree of acidity or alkalinity in soil materials suspended in water and a 0.01 M calcium chloride solution. Measurements in both liquids are necessary to fully define the soil's pH. This variable is useful in determining the solubility of soil minerals and the mobility of ions in the soil and assessing the viability of the soil-plant environment. A more detailed discussion of the usefulness of this parameter is given in Refs (1-6)2.  
1.2 Two methods for measuring the pH of soils are provided. The method to be used shall be specified by the requesting authority. When no method is specified, Method A shall be used. The pH is determined in test water and a calcium chloride solution for both methods.  
1.2.1 Method A—The pH is measured using a potentiometer having a pH sensitive electrode system. This method can be used for any application and must be used when the application warrants a higher level of resolution.  
1.2.2 Method B—The pH is measured using pH sensitive paper. This method can be used for any application, however, because paper typically has a lower resolution, it provides an approximate estimate of the pH of the soil and should not be used when the application requires a higher level of resolution (Note 1).
Note 1: For example, paper with a sensitivity to the nearest 1 pH unit placed into a buffer solution of 4 should indicate a pH of 4, however, it would not indicate if the pH is 4.449 or 3.449.  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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Standard Practice for Screening Fuels in Soils

SIGNIFICANCE AND USE
5.1 This practice is a screening procedure for determining the presence of fuels containing aromatic compounds in soils. If a sample of the contaminant fuel is available for use in calibration, the approximate concentration of the fuel in the soil can be calculated. If the fuel type is known but a sample of the contaminant fuel is not available for calibration, an estimate of the contaminant fuel concentration can be calculated using average response factors based on composition of the fuel in the soil. If the composition of the contaminant fuel is unknown, a contaminant concentration cannot be calculated, and this practice can only be used only to indicate the presence or absence of fuel contamination.  
5.2 Fuels containing aromatic compounds, such as diesel fuel and gasoline, as well as other aromatic-containing hydrocarbon materials, such as crude oil, coal oil, and motor oil, can be determined by this practice. The quantitation limit for diesel fuel is about 75 mg/kg. Approximate quantitation limits for other aromatic-containing hydrocarbon materials that can be determined by this screening practice are given in Table 1. Quantitation limits for highly aliphatic materials, such as aviation gasoline and synthetic motor oil, are much higher than those for more aromatic materials, such as coal oil and diesel fuel.  
Note 1: The quantitation limits listed in Table 1 are estimated values because in this practice, the quantitation limit can be influenced by the particular fuel type and soil background. For information on how the values given in Table 1 were determined, see Appendix X1. Data generated during the development of this screening practice and other information pertaining to this practice can be found in the referenced research reports (1, 2).3  
5.3 When applying this practice to sites contaminated by diesel fuel, care should be taken in selecting the appropriate response factor from the list given in Table 2, with consideration given to whether or not t...
SCOPE
1.1 This practice is a screening procedure for assessing the presence of fuels containing aromatic compounds in soils. If a sample of the contaminant fuel is available, the concentration of the fuel in the soil can be determined. If the contaminant fuel type is known but a sample of the contaminant fuel is not available, an estimate of the concentration of the fuel in the soil can be made using average response factors based on composition of the fuel in the soil. If the kind of contaminant fuel is unknown, this screening method can be used to identify the presence of contamination.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

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ASTM
ASTM G51-23(Test Method)
Standard Test Method for Measuring pH of Soil for Use in Corrosion Evaluations

SIGNIFICANCE AND USE
4.1 Information on pH of soil is used as an aid in evaluating the corrosivity of a soil environment. Some metals are more sensitive to the pH of their environment than others, and information on the stability of a metal as a function of pH and potential is available in the literature.3
SCOPE
1.1 This test method covers a procedure for determining the pH of a soil in corrosion evaluations. The principle use of the test is to supplement soil resistivity measurements and thereby identify conditions under which the corrosion of metals in soil may be accentuated (see G57 – 78 (2012)).  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

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ASTM
ASTM D7968-23(Test Method)
Standard Test Method for Determination of Polyfluorinated Compounds in Soil by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)

SIGNIFICANCE AND USE
5.1 This test method has been developed by the U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
5.2 PFAS are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFAS have been reported to exhibit developmental toxicity, hepatotoxicity, immunotoxicity, and hormone disturbance. A draft Toxicological Profile for Perfluoroalkyls from the U.S. Department of Health and Human Services is available.7 PFAS have been detected in soils, sludges, and surface and drinking waters. Hence, there is a need for a quick, easy, and robust method to determine these compounds at trace levels in various soil matrices for understanding of the sources and pathways of exposure.  
5.3 This method has been used to determine selected PFAS in sand (Table 4) and four ASTM reference soils (Table 5).
SCOPE
1.1 This procedure covers the determination of selected polyfluorinated alkyl substances (PFAS) in a soil matrix using solvent extraction, filtration, followed by liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry. This procedure utilizes a quick extraction and is not intended to generate an exhaustive accounting of the content of PFAS in difficult soil matrices. An exhaustive extraction procedure for PFAS, such as published by Washington et al.,2 for difficult matrices should be considered when analyzing PFAS. The approach from this standard was utilized to screen laboratory coats (textiles) to identify if PFAS would be leached from the materials.  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 The method of detection limit3 and reporting range4 for the target analytes are listed in Table 1.    
1.3.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. Analyte detections between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test method. In most cases, the reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 2 for the PFAS after taking into account a 2 g sample weight and a final extract volume of 10 mL, 50 % water/50 % MeOH with 0.1 % acetic acid. The final extract volume is assumed to be 10 mL because 10 mL of 50 % water/50 % MeOH with 0.1 % acetic acid was added to each soil sample and only the liquid layer after extraction is filtered, leaving the solid and any residual solvent behind. It is raised above the Level 1 calibration concentration for PFOS, PFHxA, FHEA, and FOEA; these compounds can be identified at the Level 1 concentration but the standard deviation among replicates at this lower spike level resulted in a higher reporting limit.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

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ASTM
ASTM D8459-23(Test Method)
Standard Test Methods for Detecting Water Soluble Sulfates in Construction Soils

SIGNIFICANCE AND USE
5.1 Where sulfates are suspected, subgrade soils should be tested as an integral part of a geotechnical evaluation because the possibility that sulfate induced heave may occur if calcium containing stabilizers are used to improve the soils and sulfate reactions may also cause deterioration in concrete structures. When planning to treat a soil used in construction with lime, testing the soil for water soluble sulfates prior to treatment becomes very important (Note 2).  
5.2 When sulfate containing cohesive soils are treated with calcium-based stabilizers for foundation improvements, sulfates and free alumina in natural soils react with calcium and free hydroxide to form crystalline minerals, such as ettringite and thaumasite.4 Thaumasite forms when ettringite undergoes changes in the presence of carbonates at low temperatures.5 The sulfate minerals expand considerably when they are hydrated.
Note 2: For more information on the effect of treating soils containing water soluble sulfates, refer to the following publication: Little, D.N., Stabilization of Pavement Subgrades and Base Course with Lime, Kendal/Hunt Publishing Co., Dubuque, IA, 1995.
Note 3: 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.
SCOPE
1.1 These methods determine the water soluble sulfate content of cohesive soils used in construction by using the colorimetric technique. Two methods are presented in this standard. Method A is for use in the field and Method B is for use in the laboratory. The colorimetric technique involves measuring the scattering of a light beam through a solution that contains suspended particulate matter. Measurements of sulfate concentrations in construction soils can be used to guide professionals in the selection of appropriate stabilization methods and to assist in assessment of potential deterioration in concrete structures.
Note 1: These test methods are partially based on the research conducted by Texas A & M University.  
1.2 The field method, Method A, is used as a screening test for the presence of sulfates and their concentration. The laboratory method, Method B, provides better resolution than the field method.  
1.3 Ion chromatography is also an acceptable alternative method that can be used to evaluate results, however, it is outside the scope of this standard.  
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 All observed and calculated values shall conform to the guidelines for significant digits and rounding established in Practice D6026, unless superseded by this test method.  
1.5.1 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.  
1.6 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 appropri...

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