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ASTM D5831-23

(Practice)

Standard Practice for Screening Fuels in Soils

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.

General Information

Status
Published
Publication Date
31-Oct-2023
ICS
13.080.10 - Chemical characteristics of soils
Technical Committee
D34 - Waste Management
Drafting Committee
D34.01.05 - Screening Methods
Current Stage
Ref Project

Relations

Replaces
ASTM D5831-17 - Standard Practice for Screening Fuels in Soils
Effective Date
01-Nov-2023
Refers
ASTM D5681-23 - Standard Terminology for Waste and Waste Management
Effective Date
01-Nov-2023
Refers
ASTM D5681-22e1 - Standard Terminology for Waste and Waste Management
Effective Date
01-May-2022
Referred By
ASTM F2931-19a - Standard Guide for Analytical Testing of Substances of Very High Concern in Materials and Products
Effective Date
01-Nov-2023

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Standards Content (Sample)

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.
Designation: D5831 − 23
Standard Practice for
1
Screening Fuels in Soils
This standard is issued under the fixed designation D5831; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope Quantitative Analysis
E177 Practice for Use of the Terms Precision and Bias in
1.1 This practice is a screening procedure for assessing the
ASTM Test Methods
presence of fuels containing aromatic compounds in soils. If a
E275 Practice for Describing and Measuring Performance of
sample of the contaminant fuel is available, the concentration
Ultraviolet and Visible Spectrophotometers
of the fuel in the soil can be determined. If the contaminant fuel
E691 Practice for Conducting an Interlaboratory Study to
type is known but a sample of the contaminant fuel is not
Determine the Precision of a Test Method
available, an estimate of the concentration of the fuel in the soil
E925 Practice for Monitoring the Calibration of Ultraviolet-
can be made using average response factors based on compo-
Visible Spectrophotometers whose Spectral Bandwidth
sition of the fuel in the soil. If the kind of contaminant fuel is
does not Exceed 2 nm
unknown, this screening method can be used to identify the
presence of contamination.
3. Terminology
1.2 The values stated in SI units are to be regarded as
3.1 Definitions—For definitions of terms used in this screen-
standard. No other units of measurement are included in this
ing practice, refer to Terminologies D5681 and E131.
standard.
4. Summary of Practice
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.1 A sample of soil is extracted with isopropyl alcohol, and
responsibility of the user of this standard to establish appro-
the extract is filtered. The ultraviolet absorbance of the extract
priate safety, health, and environmental practices and deter-
is measured at 254 nm. If a sample of the contaminant fuel is
mine the applicability of regulatory limitations prior to use.
available, the approximate concentration of contamination can
1.4 This international standard was developed in accor-
be calculated. If the contaminant fuel type is known but a
dance with internationally recognized principles on standard-
sample of the contaminant fuel is not available, an estimate of
ization established in the Decision on Principles for the
the contaminant concentration is determined using average
Development of International Standards, Guides and Recom-
response factors based on composition of the fuel in the soil. If
mendations issued by the World Trade Organization Technical
the composition of the contaminant fuel is not known, the
Barriers to Trade (TBT) Committee.
absorbance value is used to indicate the presence or absence of
fuel contamination. Calcium oxide is added to the soil as a
2. Referenced Documents
conditioning agent to minimize interferences from humic
2
2.1 ASTM Standards: materials and moisture present in the soil. Particulate interfer-
D2777 Practice for Determination of Precision and Bias of ences are removed by passing the extract through a filter.
Applicable Test Methods of Committee D19 on Water
5. Significance and Use
D5681 Terminology for Waste and Waste Management
E131 Terminology Relating to Molecular Spectroscopy
5.1 This practice is a screening procedure for determining
E169 Practices for General Techniques of Ultraviolet-Visible
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
1
This practice is under the jurisdiction of ASTM Committee D34 on Waste
soil can be calculated. If the fuel type is known but a sample of
Management and is the direct responsibility of Subcommittee D34.01.05 on
the contaminant fuel is not available for calibration, an
Screening Methods.
estimate of the contaminant fuel concentration can be calcu-
Current edition approved Nov. 1, 2023. Published November 2023. Originally
lated using average response factors based on composition of
approved in 1995. Last previous edition approved in 2017 as D5831 – 17. DOI:
10.1520/D5831-23.
the fuel in the soil. If the composition of the contaminant fuel
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
is unknown, a contaminant concentration cannot be calculated,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
an
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5831 − 17 D5831 − 23
Standard Practice for
1
Screening Fuels in Soils
This standard is issued under the fixed designation D5831; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 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 performed.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.
2. Referenced Documents
2
2.1 ASTM Standards:
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D5681 Terminology for Waste and Waste Management
E131 Terminology Relating to Molecular Spectroscopy
E169 Practices for General Techniques of Ultraviolet-Visible Quantitative Analysis
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E275 Practice for Describing and Measuring Performance of Ultraviolet and Visible Spectrophotometers
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E925 Practice for Monitoring the Calibration of Ultraviolet-Visible Spectrophotometers whose Spectral Bandwidth does not
Exceed 2 nm
3. Terminology
3.1 Definitions—For definitions of terms used in this screening practice, refer to Terminologies D5681 and E131.
1
This practice is under the jurisdiction of ASTM Committee D34 on Waste Management and is the direct responsibility of Subcommittee D34.01.05 on Screening Methods.
Current edition approved Dec. 1, 2017Nov. 1, 2023. Published December 2017November 2023. Originally approved in 1995. Last previous edition approved in 20092017
as D5831 – 09.D5831 – 17. DOI: 10.1520/D5831-17.10.1520/D5831-23.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5831 − 23
TABLE 1 Approximate Quantitation Limits for Various Fuel Types
in Soils Based on 0.036 AU
Limit of Quantitation (LOQ),
Material
mg/kg
Coal Oil 21
Crude Oil 61
Diesel Fuel 75
Weathered Diesel Fuel 21
Used Motor Oil 162
Weathered Gasoline 170
Unleaded Gasoline 316
Jet Fuel JP-2 378
Motor Oil 533
Aviation Gasoline 1066
Synthetic Motor Oil 1382
4. Summary of Practice
4.1 A sample of soil is extracted with isopropyl alcohol, and the extract is filtered. The ultraviolet absorbance of the extract is
measured at 254 nm. If a sample of the contaminant fuel is available, the approximate concentration of contamination can be
calculated. If the contaminant fuel type is known but a sample of the contaminant fuel is not available, an estimate of the
contaminant concentration is determined using average response factors based on composition of the fuel in the soil. If the
composition of the contaminant fuel is not known, the absorbance value is used to indicate the presence or absence of fuel
contamination. Calcium oxide is added to the soil as a condition
...

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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.  
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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.  
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.  
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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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ASTM E2787-21(Test Method)
Standard Test Method for Determination of Thiodiglycol in Soil Using Pressurized Fluid Extraction Followed by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

SIGNIFICANCE AND USE
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  
5.2 This method has been investigated for use with soil.
SCOPE
1.1 This procedure covers the determination of thiodiglycol (TDG) in soil using pressurized fluid extraction (PFE). A commercially available PFE system2 is used, followed by analysis using liquid chromatography (LC), and detected with tandem mass spectrometry (MS/MS). TDG is qualitatively and quantitatively determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry.  
1.2 The method detection limit (MDL) and reporting range for TDG are listed in Table 1.  
1.2.1 The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B.  
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ASTM E2866-21(Test Method)
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SIGNIFICANCE AND USE
5.1 This is a performance-based method, and modifications are allowed to improve performance.  
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Standard Test Method for Analysis of Target Phenols (TPs) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS)

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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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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.  
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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.  
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 D5831-17(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 performed. 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 D7968-17a(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 PFCs are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFCs 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 PFCs 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 polyfluorinated compounds in sand (Table 4) and four ASTM reference soils (Table 5).
TABLE 4 Single-Laboratory Recovery Data in Ottawa Sand    
Sample  
Measured ng/kg from Ottawa Sand P&A Data (400 ng/kg spike for all PFCs except 2000 ng/kg for PFBA and PFPeA and 8000 ng/kg spike for FHEA, FDEA, and FOEA)  
PFTreA  
PFTriA  
PFDoA  
PFUnA  
PFDA  
PFNA  
PFOA  
PFHpA  
PFHxA  
PFPeA  
PFBA  
Unspiked 1  
Unspiked 2  
P&A 1  
389.6  
394.3  
384.7  
376.7  
362.1  
347.6  
345.8  
232.9  
222.2  
1614.9  
1344.5  
P&A 2  
462.1  
424.6  
397.2  
379.1  
378.4  
376.9  
365.9  
247.9  
229.8  
1710.1  
1388  
P&A 3  
402.7  
387.7  
383.1  
365.9  
374.7  
363.3  
347.1  
242.4  
222.9  
1658.9  
1376  
P&A 4  
403.9  
397.1  
395.4  
381.5  
379  
359.4  
342.7  
246.8  
225.8  
1693.6  
1401.9  
P&A 5  
467.2  
445.8  
412.6  
388.5  
376.8  
370.3  
369.7  
249.3  
231.4  
1716.5  
1433.4  
P&A 6  
392.1  
385.3  
374.2  
370.9  
353.2  
351.7  
340.3  
236.7  
220.5  
1659  
1366.4  
Mean R...
SCOPE
1.1 This procedure covers the determination of selected polyfluorinated compounds (PFCs) 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 PFCs in difficult soil matrices. An exhaustive extraction procedure for polyfluoralkyl substances, such as published by Washington et al.,2 for difficult matrices should be considered when analyzing PFCs.  
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.
TABLE 1 Method Detection Limit and Reporting RangeA    
Analyte  
MDL
(ng/kg)  
Reporting Limit
(ng/kg)  
PFTreA  
6.76  
25–1000  
PFTriA  
5.26  
25–1000  
PFDoA  
3.56  
25–1000  
PFUnA  
2.45  
25–1000  
PFDA  
5.54  
25–1000  
PFOS  
18.83  
50–1000  
PFNA  
2.82  
25–1000  
PFecHS  
2.41  
25–1000  
PFOA  
6.24  
25–1000  
PFHxS  
7.75  
25–1000  
PFHpA  
5.80  
25–1000  
PFHxA  
15.44  
50–1000  
PFBS  
6.49  
25–1000  
PFPeA  
20.93  
125–5000  
PFBA  
22.01  
125–5000  
FHEA  
199.04  
600–20 000  
FOEA  
258.37  
750–20 000  
FDEA  
137.46  
500–20 000  
FOUEA  
4.85  
25–1000  
FhpPa  
5.09  
25–1000  
FHUEA  
3.50  
25–1000(A) Abbreviations are defined in 3.2.  
TABLE 2 Concentrations of Calibration Standards (ng/L)    
Analyte/Surrogate  
LV1  
LV2  
LV3  
LV4  
LV5  
LV6  
LV7  
LV8  
LV9  
PFPeA, PFBA  
25  
50  
100  
200  
300  
400  
500  
750  
1000  ...

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ASTM
ASTM D7968-17(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 PFCs are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFCs 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 PFCs 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 polyfluorinated compounds in sand (Table 4) and four ASTM reference soils (Table 5).
SCOPE
1.1 This procedure covers the determination of selected polyfluorinated compounds (PFCs) 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 PFCs in difficult soil matrices. An exhaustive extraction procedure for polyfluoralkyl substances, such as published by Washington et al.,2 for difficult matrices should be considered when analyzing PFCs.  
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. (A) Abbreviations are defined in 3.2.    
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 polyfluorinated compounds 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 and health 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 E2866-12(2016)(Test Method)
Standard Test Method for Determination of Diisopropyl Methylphosphonate, Ethyl Methylphosphonic Acid, Isopropyl Methylphosphonic Acid, Methylphosphonic Acid and Pinacolyl Methylphosphonic Acid in Soil 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 standard 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 Standard shall be made aware of these changes and given the performance data demonstrating better or equivalent performance.  
5.2 Organophosphate pesticides affect the nervous system by disrupting the enzyme that regulates acetylcholine, a neurotransmitter. They were developed during the early 19th century, but their effects on insects, which were similar to their effects on humans, were discovered in 1932. Some are poisonous and were used as chemical weapon agents. Organophosphate pesticides are usually not persistent in the environment.7,8  
5.3 This test method is for the analysis of selected organophosphorous based pesticide degradation products.  
5.4 This method has been investigated for use with various soils.
SCOPE
1.1 This procedure covers the determination of Diisopropyl Methylphosphonate (DIMP), Ethyl Methylphosphonic Acid (EMPA), Isopropyl Methylphosphonic Acid (IMPA), Methylphosphonic Acid (MPA) and Pinacolyl Methylphosphonic Acid (PMPA), referred to collectively as organophosphonates (OPs) in this test method, in soil. This method is based upon solvent extraction of a soil by pressurized fluid extraction (PFE). The extract is filtered and analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). OPs are qualitatively and quantitatively determined by this 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 the OPs are listed in Table 1.  
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.

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