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ASTM D5258-02(2007)

(Practice)

Standard Practice for Acid-Extraction of Elements from Sediments Using Closed Vessel Microwave Heating

Standard Practice for Acid-Extraction of Elements from Sediments Using Closed Vessel Microwave Heating

SIGNIFICANCE AND USE
Partial extraction of soils and sediments can provide information on the availability of elements to leeching, water quality changes, or other site conditions.
Rapid heating, in combination with temperatures in excess of the atmospheric boiling point of nitric acid, reduces sample preparation or reaction times.
Little or no acids are lost to boiling or evaporation in the closed digestion vessel so additional portions of acid may not be required. Increased blank corrections from trace impurities in acid are minimized.
SCOPE
1.1 This practice covers the digestion of soils and sediments for subsequent determination of acid-extractable concentrations of certain elements by such techniques as atomic absorption and atomic emission spectroscopy.
1.1.1 Concentrations of arsenic, cadmium, copper, lead, magnesium, manganese, nickel, and zinc can be extracted from the preceding materials. Other elements may be determined using this practice.
1.2 The analytical sample is arbitrarily defined as that which passes a 10-mesh (approximately 2-mm openings) screen and is prepared according to Practice D 3974.
1.3 Actual element quantitation can be accomplished by following the various test methods under other appropriate ASTM standards for element(s) of interest.
1.4 The detection limit and linear concentration range for each element is dependent on the atomic absorption or emission spectrophotometric technique employed and may be found in the manual accompanying the instrument used.
1.5 Before selecting a digestion technique, the user should consult the appropriate quantitation standard(s) for any special analytical considerations, and Practice D 3974 for any special preparatory considerations.
1.6 The extent of extraction of elements from soils and sediments by this method is dependent upon the physical and mineralogic characteristics of the prepared sample.
1.7 The values stated in both inch-pound and SI units are to be regarded separately as the standard. The values given in parentheses are for information only.
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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.

General Information

Status
Historical
Publication Date
14-Jun-2007
ICS
13.080.10 - Chemical characteristics of soils
Technical Committee
D19 - Water
Drafting Committee
D19.07 - Sediments, Geomorphology, and Open-Channel Flow
Current Stage
Ref Project

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ASTM D5258-02(2007) - Standard Practice for Acid-Extraction of Elements from Sediments Using Closed Vessel Microwave HeatingASTM D5258-02(2007) - Standard Practice for Acid-Extraction of Elements from Sediments Using Closed Vessel Microwave Heating
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ASTM D5258-02(2007) - Standard Practice for Acid-Extraction of Elements from Sediments Using Closed Vessel Microwave Heating
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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: D5258 − 02(Reapproved 2007)
Standard Practice for
Acid-Extraction of Elements from Sediments Using Closed
1
Vessel Microwave Heating
This standard is issued under the fixed designation D5258; 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 bility of regulatory limitations prior to use. For specific hazard
statements, see Section 8.
1.1 Thispracticecoversthedigestionofsoilsandsediments
for subsequent determination of acid-extractable concentra-
2. Referenced Documents
tions of certain elements by such techniques as atomic absorp-
2
tion and atomic emission spectroscopy. 2.1 ASTM Standards:
1.1.1 Concentrations of arsenic, cadmium, copper, lead,
D1193Specification for Reagent Water
magnesium,manganese,nickel,andzinccanbeextractedfrom D3974Practices for Extraction of Trace Elements from
the preceding materials. Other elements may be determined
Sediments
using this practice. 3
2.2 Code of Federal Regulations:
1.2 Theanalyticalsampleisarbitrarilydefinedasthatwhich
CFR Title 21, Part 1030, and Title 47, Part 18
passes a 10-mesh (approximately 2-mm openings) screen and
is prepared according to Practice D3974.
3. Summary of Practice
1.3 Actual element quantitation can be accomplished by 3.1 The chemical portion of this practice involves acid
following the various test methods under other appropriate
digestion to dissociate the elements not interstitially bound in
ASTM standards for element(s) of interest. silicate lattices.
1.4 The detection limit and linear concentration range for
3.2 The sample is digested with nitric acid in a closed
each element is dependent on the atomic absorption or emis- fluoropolymer vessel using microwave heating to an internal
6 2
sionspectrophotometrictechniqueemployedandmaybefound
pressure of 100 psi (6.89×10 dynes/cm ).
in the manual accompanying the instrument used.
3.3 This practice provides a sample suitable for analysis by
1.5 Before selecting a digestion technique, the user should
atomic absorption or emission spectrophotometry.
consult the appropriate quantitation standard(s) for any special
analytical considerations, and Practice D3974 for any special
4. Significance and Use
preparatory considerations.
4.1 Partial extraction of soils and sediments can provide
1.6 The extent of extraction of elements from soils and
information on the availability of elements to leeching, water
sediments by this method is dependent upon the physical and
quality changes, or other site conditions.
mineralogic characteristics of the prepared sample.
4.2 Rapid heating, in combination with temperatures in
1.7 The values stated in both inch-pound and SI units are to
excess of the atmospheric boiling point of nitric acid, reduces
be regarded separately as the standard. The values given in
sample preparation or reaction times.
parentheses are for information only.
4.3 Littleornoacidsarelosttoboilingorevaporationinthe
1.8 This standard does not purport to address all of the
closed digestion vessel so additional portions of acid may not
safety concerns, if any, associated with its use. It is the
be required. Increased blank corrections from trace impurities
responsibility of the user of this standard to establish appro-
in acid are minimized.
priate safety and health practices and determine the applica-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This practice is under the jurisdiction ofASTM Committee D19 on Water and contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
isthedirectresponsibilityofSubcommitteeD19.07onSediments,Geomorphology, Standards volume information, refer to the standard’s Document Summary page on
and Open-Channel Flow. the ASTM website.
3
Current edition approved June 15, 2007. Published July 2007. Originally Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
approved in 1992. Last previous edition approved in 2002 as D5258–02. DOI: Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
10.1520/D5258-02R07. www.dodssp.daps.mil.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5258 − 02 (2007)
5
5. Interferences where such specifications are available. Other grades may be
used provided it is first ascertained that the reagent is of
5.1 No interferences to the digestion of soils and sediments
sufficiently high purity to permit its use without lessening the
using microwave heating have been observed.
accuracy of the determination.
5.2 Precautions should be e
...

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ASTM D5258-22(Practice)
Standard Practice for Acid-Extraction of Elements from Sediments Using Closed Vessel Microwave Heating

SIGNIFICANCE AND USE
4.1 Partial extraction of soils and sediments can provide information on the availability of elements to leeching, water quality changes, or other site conditions.  
4.2 Rapid heating, in combination with temperatures in excess of the atmospheric boiling point of nitric acid, reduces sample preparation or reaction times.  
4.3 Little or no acids are lost to boiling or evaporation in the closed digestion vessel so additional portions of acid may not be required. Increased blank corrections from trace impurities in acid are minimized.
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1.1 This practice covers the digestion of soils and sediments for subsequent determination of acid-extractable concentrations of certain elements by such techniques as atomic absorption and atomic emission spectroscopy.  
1.1.1 Concentrations of arsenic, cadmium, copper, lead, magnesium, manganese, nickel, and zinc can be extracted from the preceding materials. Other elements may be determined using this practice.  
1.2 The analytical sample is arbitrarily defined as that which passes a 10-mesh (approximately 2 mm openings) screen and is prepared according to Practice D3974.  
1.3 Actual element quantitation can be accomplished by following the various test methods under other appropriate ASTM standards for element(s) of interest.  
1.4 The detection limit and linear concentration range for each element is dependent on the atomic absorption or emission spectrophotometric technique employed and may be found in the manual accompanying the instrument used.  
1.5 Before selecting a digestion technique, the user should consult the appropriate quantitation standard(s) for any special analytical considerations, and Practice D3974 for any special preparatory considerations.  
1.6 The extent of extraction of elements from soils and sediments by this method is dependent upon the physical and mineralogic characteristics of the prepared sample.  
1.7 The values stated in both inch-pound and SI units are to be regarded separately as the standard. The values given in parentheses are for information purposes only.  
1.8 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. For specific hazard statements, see Section 8.  
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Standard Test Method for Determination of Parent and Alkyl Polycyclic Aromatics in Sediment Pore Water Using Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry in Selected Ion Monitoring Mode

SIGNIFICANCE AND USE
5.1 This method directly determines the concentrations of dissolved PAH concentrations in environmental sediment pore water samples. The method is important from an environmental regulatory perspective because it can achieve the analytical sensitivities to meet the goals of the USEPA narcosis model for protecting benthic organisms in PAH contaminated sediments. Regulatory methods using solvent extraction have not achieved the wide calibration ranges from nanograms to milligrams per litre and the required levels of detection in the nanogram-per-litre range. In addition, conventional solvent extraction methods require large aliquot volumes (litre or larger), use of large volumes of organic solvents, and filtration to generate the pore water. This approach entails the storage and processing of large volumes of sediment samples and loss of low molecular weight PAHs in the filtration and solvent evaporation steps.  
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1.1 The U.S. Environmental Protection Agency (USEPA) narcosis model for benthic organisms in sediments contaminated with polycyclic aromatic hydrocarbons (PAHs) is based on the concentrations of dissolved PAHs in the interstitial water or “pore water” in sediment. This test method covers the separation of pore water from PAH-impacted sediment samples, the removal of colloids, and the subsequent measurement of dissolved concentrations of the required 10 parent PAHs and 14 groups of alkylated daughter PAHs in the pore water samples. The “24 PAHs” are determined using solid-phase microextraction (SPME) followed by Gas Chromatography/Mass Spectrometry (GC/MS) analysis in selected ion monitoring (SIM) mode. Isotopically labeled analogs of the target compounds are introduced prior to the extraction, and are used as quantification references.  
1.2 Lower molecular weight PAHs are more water soluble than higher molecular weight PAHs. Therefore, USEPA-regulated PAH concentrations in pore water samples vary widely due to differing saturation water solubilities that range from 0.2 µg/L for indeno[1,2,3-cd]pyrene to 31 000 µg/L for naphthalene. This method can accommodate the measurement of microgram per litre concentrations for low molecular weight PAHs and nanogram per litre concentrations for high molecular weight PAHs.  
1.3 The USEPA narcosis model predicts toxicity to benthic organisms if the sum of the toxic units (ΣTUc) calculated for all “34 PAHs” measured in a pore water sample is greater than or equal to 1. For this reason, the performance limit required for the individual PAH measurements was defined as the concentration of an individual PAH that would yield 1/34 of a toxic unit (TU). However, the focus of this method is the 10 parent PAHs and 14 groups of alkylated PAHs (Table 1) that contribute 95 % of the toxic units based on the analysis of 120 background and impacted sediment pore water samples.3 The primary reasons for eliminating the rest of the 5-6 ring parent PAHs are: (1) these PAHs contribute insignificantly to the pore water TU, and (2) these PAHs exhibit extremely low saturation solubilities that will make the detection of these compounds difficult in pore water. This method can achieve the required detection limits, which range from approximately 0.01 µg/L, for high molecular weight PAHs, to approximately 3 µg/L for low molecular weight PAHs.  
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1.5 The values stated in ...

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Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating

SIGNIFICANCE AND USE
5.1 Solvent extraction of soils and sediments can provide information on the availability of petroleum hydrocarbons to leaching, water quality changes, or other site conditions.  
5.2 Rapid heating, in combination with temperatures in excess of the atmospheric boiling point of acetone/hexane, reduces sample preparation or extraction times.  
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SCOPE
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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).
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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.  
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Standard Practice for Screening Fuels in Soils

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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.  
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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.  
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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)).  
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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).  
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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.
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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.  
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Standard Test Method for Specific Gravity of Soil Solids by Gas Pycnometer

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5.1 The specific gravity value is used in many phase relation equations to determine relative volumes of particle, water, and gas mixtures.  
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SCOPE
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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1.3 All observed and calculated values shall conform to the guidelines for significant digits and rounding established in Practice D6026.  
1.3.1 For purposes of comparing a measured or calculated value(s) with specified limits, the measured or calculated value(s) shall be rounded to the nearest decimal or significant digits in the specified limits.  
1.3.2 The procedures used to specify how data are collected/recorded and calculated in this standard are regarded as the industry standard. In addition, they are representative of the significant digits that should generally 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 analysis methods for engineering design.  
1.4 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.  
1.4.1 The gravitational system of inch-pound units is used when dealing with inch-pound units. In this system, the pound (lbf) represents a unit of force (weight), while the unit for mass is slugs. The converted slug unit is not given, un...

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5.1 This guide offers several options for the determination of 99Tc in soil samples. Sample sizes of up to 200 g are possible, depending on the method chosen to extract Tc from the soil matrix. It is up to the user to determine if it is appropriate for the intended use of the final data.
SCOPE
1.1 This guide is intended to serve as a reference for laboratories wishing to perform 99Tc analyses in soil. Several options are given for selection of a tracer and for the method of extracting the Tc from the soil matrix. Separation of Tc from the sample matrix is performed using an extraction chromatography resin. Options are then given for the determination of the 99Tc activity in the original sample. It is up to the user to determine which options are appropriate for use, and to generate acceptance data to support the chosen procedure.  
1.2 Due to the various extraction methods available, various tracers used, variable detection methods used, and lack of certified reference materials for 99Tc in soil, there is insufficient data to support a single method written as a standard method.  
1.3 The values stated in SI units are to be regarded as standard, except where the non-SI unit of molar, M, is used for the concentration of chemicals and reagents. The values given in parentheses after SI units are provided for information only and are not considered standard.  
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 D4542-22(Test Method)
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.
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.
SCOPE
1.1 These test methods cover a rapid procedure for squeezing pore water from fine-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).2  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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.

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