ASTM D7968-23
(Test Method)Standard Test Method for Determination of Polyfluorinated Compounds in Soil by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
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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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: D7968 − 23
Standard Test Method for
Determination of Polyfluorinated Compounds in Soil by
Liquid Chromatography Tandem Mass Spectrometry (LC/
1
MS/MS)
This standard is issued under the fixed designation D7968; 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 reporting limit are estimated concentrations and are not re-
ported following this test method. In most cases, the reporting
1.1 This procedure covers the determination of selected
limit is calculated from the concentration of the Level 1
polyfluorinated alkyl substances (PFAS) in a soil matrix using
calibration standard as shown in Table 2 for the PFAS after
solvent extraction, filtration, followed by liquid chromatogra-
taking into account a 2 g sample weight and a final extract
phy (LC) and detection with tandem mass spectrometry (MS/
volume of 10 mL, 50 % water/50 % MeOH with 0.1 % acetic
MS). These analytes are qualitatively and quantitatively deter-
acid. The final extract volume is assumed to be 10 mL because
mined by this method. This method adheres to multiple
10 mL of 50 % water/50 % MeOH with 0.1 % acetic acid was
reaction monitoring (MRM) mass spectrometry. This proce-
added to each soil sample and only the liquid layer after
dure utilizes a quick extraction and is not intended to generate
extraction is filtered, leaving the solid and any residual solvent
an exhaustive accounting of the content of PFAS in difficult
behind. It is raised above the Level 1 calibration concentration
soil matrices. An exhaustive extraction procedure for PFAS,
2 for PFOS, PFHxA, FHEA, and FOEA; these compounds can
such as published by Washington et al., for difficult matrices
be identified at the Level 1 concentration but the standard
should be considered when analyzing PFAS. The approach
deviation among replicates at this lower spike level resulted in
from this standard was utilized to screen laboratory coats
a higher reporting limit.
(textiles) to identify if PFAS would be leached from the
1.4 This standard does not purport to address all of the
materials.
safety concerns, if any, associated with its use. It is the
1.2 Units—The values stated in SI units are to be regarded
responsibility of the user of this standard to establish appro-
as standard. No other units of measurement are included in this
priate safety, health, and environmental practices and deter-
standard.
mine the applicability of regulatory limitations prior to use.
3 4
1.3 The method of detection limit and reporting range for
1.5 This international standard was developed in accor-
the target analytes are listed in Table 1.
dance with internationally recognized principles on standard-
1.3.1 The reporting limit in this test method is the minimum
ization established in the Decision on Principles for the
value below which data are documented as non-detects. Ana-
Development of International Standards, Guides and Recom-
lyte detections between the method detection limit and the
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
1
This test method is under the jurisdiction of ASTM Committee D34 on Waste
5
Management and is the direct responsibility of Subcommittee D34.01.06 on
2.1 ASTM Standards:
Analytical Methods.
D1193 Specification for Reagent Water
Current edition approved Nov. 1, 2023. Published November 2023. Originally
D2777 Practice for Determination of Precision and Bias of
approved in 2014. Last previous edition approved in 2017 as D7968 – 17a. DOI:
10.1520/D7968-23. Applicable Test Methods of Committee D19 on Water
2
Washington, J. W., Naile, J. E., Jenkins, T. M., and Lynch, D. G., “Character-
D5847 Practice for Writing Quality Control Specifications
izing Fluorotelomer and Polyfluoroalkyl Substances in New and Aged
for Standard Test Methods for Water Analysis
Fluorotelomer-Based Polymers for Degradation Studies with GC/MS and LC/MS/
E2554 Practice for Estimating and Monitoring the Uncer-
MS,” Environmental Science and Technology, Vol 48, 2014, pp. 5762–5769.
3
The MDL is determined following the Code of Federal Regulations, 40 CFR
tainty of Test Results of a Test Method Using Control
Part 136, Appendix B utilizing solvent extraction of soil. A 2 g sample of Ottawa
Chart Techniques
sand was utilized. A detailed process determining the MDL is explained in the
reference and is beyond the scope of this standard to be explained here.
4 5
Reporting range
...
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: D7968 − 17a D7968 − 23
Standard Test Method for
Determination of Polyfluorinated Compounds in Soil by
Liquid Chromatography Tandem Mass Spectrometry (LC/
1
MS/MS)
This standard is issued under the fixed designation D7968; 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 procedure covers the determination of selected polyfluorinated compounds (PFCs) 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 PFCsPFAS in difficult soil matrices. An exhaustive extraction procedure for polyfluoralkyl substances,
2
PFAS, such as published by Washington et al., for difficult matrices should be considered when analyzing PFCs.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.
3 4
1.3 The Method of Detection Limitmethod of detection limit and Reporting Rangereporting range 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 polyfluorinated compounds PFAS after taking into account a 2-g2 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
This test method is under the jurisdiction of ASTM Committee D34 on Waste Management and is the direct responsibility of Subcommittee D34.01.06 on Analytical
Methods.
Current edition approved Sept. 1, 2017Nov. 1, 2023. Published September 2017November 2023. Originally approved in 2014. Last previous edition approved in 2017 as
D7968 – 17.D7968 – 17a. DOI: 10.1520/D7968-17A.10.1520/D7968-23.
2
Washington, J. W., Naile, J. E., Jenkins, T. M., and Lynch, D. G., “Characterizing Fluorotelomer and Polyfluoroalkyl Substances in New and Aged Fluorotelomer-Based
Polymers for Degradation Studies with GC/MS and LC/MS/MS,” Environmental Science and Technology, Vol 48, 2014, pp. 5762–5769.
3
The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B utilizing solvent extraction of soil. Two-gram A 2 g sample of Ottawa
sand was utilized. A detailed process determining the MDL is explained in the reference and is beyond the scope of this standard to be explained here.
4
Reporting range concentration is calculated from Table 2 concentrations assuming a 30-μL 30 μL injection of the Level 1 calibration standard for the PFCs,PFAS, and
the highest level calibration standard with a 10-mL 10 mL final extract volume of a 2-g2 g soil sample. Volume variations will change the reporting limit and ranges.
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D7968 − 23
A
TABLE 1 Method Detection Limit and Reporting Range
MDL Reporting Limit
Analyte
(ng/kg) (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
P
...
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