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ASTM D7858-13

(Test Method)

Standard Test Method for Determination of Bisphenol A in Soil, Sludge and Biosolids by Pressurized Fluid Extraction and Analyzed by Liquid Chromatography/Tandem Mass Spectrometry

Standard Test Method for Determination of Bisphenol A in Soil, Sludge and Biosolids by Pressurized Fluid Extraction and Analyzed by Liquid Chromatography/Tandem Mass Spectrometry

SIGNIFICANCE AND USE
5.1 This is a performance based method, and modifications are allowed to improve performance.  
5.1.1 Due to the rapid development of newer instrumentation and column chemistries, changes to the analysis described in this test method are allowed as long as better or equivalent performance data result. Any modifications shall be documented and performance data generated. The user of the data generated by this test method shall be made aware of these changes and given the performance data demonstrating better or equivalent performance.  
5.2 The first reported synthesis of BPA was by the reaction of phenol with acetone by Zincke.7 BPA has become an important high volume industrial chemical used in the manufacture of polycarbonate plastic and epoxy resins. Polycarbonate plastic and resins are used in numerous products including electrical and electronic equipment, automobiles, sports and safety equipment, reusable food and drink containers, electrical laminates for printed circuit boards, composites, paints, adhesives, dental sealants, protective coatings and many other products.8  
5.3 The environmental source of BPA is predominantly from the decomposition of polycarbonate plastics and resins. BPA is not classified as bio-accumulative by the U.S. Environmental Protection Agency and will biodegrade. BPA has been reported to have adverse effects in aquatic organisms and may be released into environmental waters directly at trace levels through landfill leachate and sewage treatment plant effluents. This method has been investigated for use with soil, sludge, and biosolids.  
5.4 The land application of biosolids has raised concerns over the fate of BPA in the environment and a standard method is needed to monitor concentrations. This method has been investigated for use with various soils.
SCOPE
1.1 This procedure covers the determination of Bisphenol A (BPA) in soil, sludge, and biosolids. This test method is based upon solvent extraction of a soil matrix by pressurized fluid extraction (PFE). The extract is filtered and analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). BPA is qualitatively and quantitatively determined by this test method.  
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 Detection Limit2 (MDL), electrospray ionization (ESI) mode, and Reporting Range3 for BPA are listed in Table 1.TABLE 1 Method Detection Limit and Reporting Range    
Analyte  
ESI Mode  
MDL (PPB)  
Reporting Range (PPB)  
Bisphenol A  
Negative  
2.8  
10-250
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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
31-Mar-2013
ICS
13.080.10 - Chemical characteristics of soils
Technical Committee
D34 - Waste Management
Drafting Committee
D34.01.06 - Analytical Methods
Current Stage
Ref Project

Relations

Replaced By
ASTM D7858-13(2018) - Standard Test Method for Determination of Bisphenol A in Soil, Sludge, and Biosolids by Pressurized Fluid Extraction and Analyzed by Liquid Chromatography/Tandem Mass Spectrometry
Effective Date
01-Sep-2018
Referred By
ASTM D8310-20 - Standard Test Method for Analysis of Target Phenols (TPs) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS)
Effective Date
01-Apr-2013

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ASTM D7858-13 - Standard Test Method for Determination of Bisphenol A in Soil, Sludge and Biosolids by Pressurized Fluid Extraction and Analyzed by Liquid Chromatography/Tandem Mass SpectrometryASTM D7858-13 - Standard Test Method for Determination of Bisphenol A in Soil, Sludge and Biosolids by Pressurized Fluid Extraction and Analyzed by Liquid Chromatography/Tandem Mass Spectrometry
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ASTM D7858-13 - Standard Test Method for Determination of Bisphenol A in Soil, Sludge and Biosolids by Pressurized Fluid Extraction and Analyzed by Liquid Chromatography/Tandem Mass Spectrometry
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Standards Content (Sample)

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: D7858 − 13
Standard Test Method for
Determination of Bisphenol A in Soil, Sludge and Biosolids
by Pressurized Fluid Extraction and Analyzed by Liquid
1
Chromatography/Tandem Mass Spectrometry
This standard is issued under the fixed designation D7858; 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 2. Referenced Documents
4
1.1 ThisprocedurecoversthedeterminationofBisphenolA 2.1 ASTM Standards:
(BPA) in soil, sludge, and biosolids. This test method is based D653Terminology Relating to Soil, Rock, and Contained
upon solvent extraction of a soil matrix by pressurized fluid Fluids
extraction (PFE).The extract is filtered and analyzed by liquid D1193Specification for Reagent Water
chromatography/tandem mass spectrometry (LC/MS/MS). D3694Practices for Preparation of Sample Containers and
BPAis qualitatively and quantitatively determined by this test for Preservation of Organic Constituents
method. D3740Practice for Minimum Requirements for Agencies
Engaged inTesting and/or Inspection of Soil and Rock as
1.2 Units—The values stated in SI units are to be regarded
Used in Engineering Design and Construction
asstandard.Nootherunitsofmeasurementareincludedinthis
D3856Guide for Management Systems in Laboratories
standard.
Engaged in Analysis of Water
2
1.3 The Method Detection Limit (MDL), electrospray
D5681Terminology for Waste and Waste Management
3
ionization (ESI) mode, and Reporting Range for BPA are
E2554Practice for Estimating and Monitoring the Uncer-
listed in Table 1.
tainty of Test Results of a Test Method Using Control
1.4 This standard does not purport to address all of the Chart Techniques
safety concerns, if any, associated with its use. It is the
2.2 Other Documents:
responsibility of the user of this standard to establish appro-
EPAPublication SW-846Test Methods for Evaluating Solid
5
priate safety and health practices and determine the applica- Waste, Physical/Chemical Methods
bility of regulatory limitations prior to use.
The Code of Federal Regulations40 CFR Part 136,Appen-
6
1.5 This international standard was developed in accor- dix B
dance with internationally recognized principles on standard-
3. Terminology
ization established in the Decision on Principles for the
3.1 Definitions:
Development of International Standards, Guides and Recom-
3.1.1 Bisphenol A (BPA), n—2,2-bis(4-hydroxyphenyl) pro-
mendations issued by the World Trade Organization Technical
pane.
Barriers to Trade (TBT) Committee.
3.1.2 Bisphenol A (propane-D ) (BPA-D ), n—deuterium
6 6
labeledBisphenolAwherethetwomethylmoietiescontainall
1
This test method is under the jurisdiction ofASTM Committee D34 on Waste 2
H and is used as a surrogate in this method.
Management and is the direct responsibility of Subcommittee D34.01.06 on
Analytical Methods.
4
Current edition approved April 1, 2013. Published May 2013. DOI: 10.1520/ For referenced ASTM standards, visit the ASTM website, www.astm.org, or
D7858-13. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
The MDL is determined following the Code of Federal Regulations, 40 CFR Standardsvolumeinformation,refertothestandard’sDocumentSummarypageon
Part 136, Appendix B utilizing solvent extraction of soil by PFE. 10 gram sample the ASTM website.
5
of Ottawa Sand was utilized.Adetailed process determining the MDLis explained Available from National Technical Information Service (NTIS), U.S. Depart-
in the reference and is beyond the scope of this test method to be explained here. ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
3
Reporting range concentration is calculated from Table 4 concentrations www.epa.gov/epawaste/hazard/testmethods/index.htm
6
assuming a 25 µL injection of the Level 1 calibration standard for BPA, and the AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
highestlevelcalibrationstandardwitha5mLfinalextractvolumeofa10gramsoil 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
sample. Volume variations will change the reporting limit and ranges. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7858 − 13
TABLE 1 Method Detection Limit and Reporting Range
5. Significance and Use
Reporting Range
Analyte ESI Mode MDL (PPB) 5.1 This is a performance based method, and modifications
(PPB)
are allowed to improve performance.
Bisphenol A Negative 2.8 10-250
5.1.1 Due to the rapid development of newer instrumenta-
tionandco
...

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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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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.  
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5.1 TDG is a Schedule 2 compound under the Chemical Weapons Convention (CWC). Schedule 2 chemicals include those that are precursors to chemical weapons, chemical weapons agents, or have a number of other commercial uses. They are used as ingredients to produce insecticides, herbicides, lubricants, and some pharmaceutical products. Schedule 2 chemicals can be found in applications unrelated to chemical weapons. TDG is both a mustard gas precursor and a degradant as well as an ingredient in water-based inks, ballpoint pen inks, dyes, and some pesticides.5  
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SCOPE
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SIGNIFICANCE AND USE
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SCOPE
1.1 This procedure covers the determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in a soil matrix by extraction with acetone, filtration, dilution with water, and analysis by liquid chromatography/tandem mass spectrometry. TTPC is a biocide that strongly adsorbs to soils.2 The sample extracts are prepared in a solution of 75 % acetone and 25 % water because TTPC has an affinity for surfaces and particles. The reporting range for this method is from 250 to 10 000 ng/kg. This analyte is qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
1.2 The method detection limit (Note 1) (MDL) and reporting range (Note 2) for the target analyte are listed in Table 1.  
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Note 2: Reporting range concentration is calculated from Table 2 concentrations assuming a 50-μL injection of the Level 1 calibration standard for TTPC, and the highest level calibration standard with a 20-mL final extract volume of a 2-g soil sample. Volume variations will change the reporting limit and ranges.  
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SIGNIFICANCE AND USE
5.1 This test method developed for the analysis of TPs in soil and sediment samples is based upon an LC/MS/MS analysis. Any type of coupled liquid chromatography/mass spectrometry system may be used that meets the study objectives of the individual project. These may include, but are not limited to: trap, single quadrupoles, time-of-flight, high resolution, and others not mentioned here.  
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SCOPE
1.1 This test method covers analysis of nonylphenol (NP), nonylphenol monoethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), octylphenol (OP), and bisphenol A (BPA), referred to collectively as target phenols (TPs), in soil, sediments, and biosolids by extraction with acetone, filtration, dilution with water, and analysis by liquid chromatography/tandem mass spectrometry. The sample extracts are prepared in a solution of 75 % acetone and 25 % water because TPs have an affinity for surfaces and particles that is more pronounced at lower concentrations. The range of applicability of the test method is shown in Table 1. The method may be extended outside of these ranges depending on additional performance studies not undertaken here.  
1.2 Units—The values stated in SI units are to be regarded as the 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 D7858-13(2018)(Test Method)
Standard Test Method for Determination of Bisphenol A in Soil, Sludge, and Biosolids by Pressurized Fluid Extraction and Analyzed by Liquid Chromatography/Tandem Mass Spectrometry

SIGNIFICANCE AND USE
5.1 This is a performance-based method, and modifications are allowed to improve performance.  
5.1.1 Due to the rapid development of newer instrumentation and column chemistries, changes to the analysis described in this test method are allowed as long as better or equivalent performance data result. Any modifications shall be documented and performance data generated. The user of the data generated by this test method shall be made aware of these changes and given the performance data demonstrating better or equivalent performance.  
5.2 The first reported synthesis of BPA was by the reaction of phenol with acetone by Zincke.7 BPA has become an important high-volume industrial chemical used in the manufacture of polycarbonate plastic and epoxy resins. Polycarbonate plastic and resins are used in numerous products, including electrical and electronic equipment, automobiles, sports and safety equipment, reusable food and drink containers, electrical laminates for printed circuit boards, composites, paints, adhesives, dental sealants, protective coatings, and many other products.8  
5.3 The environmental source of BPA is predominantly from the decomposition of polycarbonate plastics and resins. BPA is not classified as bio-accumulative by the U.S. Environmental Protection Agency and will biodegrade. BPA has been reported to have adverse effects in aquatic organisms and may be released into environmental waters directly at trace levels through landfill leachate and sewage treatment plant effluents. This method has been investigated for use with soil, sludge, and biosolids.  
5.4 The land application of biosolids has raised concerns over the fate of BPA in the environment, and a standard method is needed to monitor concentrations. This method has been investigated for use with various soils.
SCOPE
1.1 This procedure covers the determination of Bisphenol A (BPA) in soil, sludge, and biosolids. This test method is based upon solvent extraction of a soil matrix by pressurized fluid extraction (PFE). The extract is filtered and analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). BPA is qualitatively and quantitatively determined by this test method.  
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 detection limit (MDL),2 electrospray ionization (ESI) mode, and reporting range3 for BPA are listed in Table 1.  
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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 D5831-23(Practice)
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 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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