ASTM D7968-17
(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 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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Designation:D7968 −17
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.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope calibrationstandardasshowninTable2forthepolyfluorinated
compounds after taking into account a 2-g sample weight and
1.1 This procedure covers the determination of selected
afinalextractvolumeof10mL,50%water/50%MeOHwith
polyfluorinated compounds (PFCs) in a soil matrix using
0.1% acetic acid. The final extract volume is assumed to be
solvent extraction, filtration, followed by liquid chromatogra-
10mLbecause 10 mLof 50% water/50% MeOH with 0.1%
phy (LC) and detection with tandem mass spectrometry (MS/
acetic acid was added to each soil sample and only the liquid
MS). These analytes are qualitatively and quantitatively deter-
layer after extraction is filtered, leaving the solid and any
mined by this method. This method adheres to multiple
residual solvent behind. It is raised above the Level 1 calibra-
reaction monitoring (MRM) mass spectrometry. This proce-
tionconcentrationforPFOS,PFHxA,FHEA,andFOEA;these
dure utilizes a quick extraction and is not intended to generate
compounds can be identified at the Level 1 concentration but
anexhaustiveaccountingofthecontentofPFCsindifficultsoil
the standard deviation among replicates at this lower spike
matrices. An exhaustive extraction procedure for polyfluo-
2 level resulted in a higher reporting limit.
ralkyl substances, such as published by Washington et al., for
1.4 This standard does not purport to address all of the
difficult matrices should be considered when analyzing PFCs.
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-
asstandard.Nootherunitsofmeasurementareincludedinthis
priate safety and health practices and determine the applica-
standard.
bility of regulatory limitations prior to use.
3 4
1.3 The Method of Detection Limit and Reporting Range
1.5 This international standard was developed in accor-
for the target analytes are listed in Table 1.
dance with internationally recognized principles on standard-
1.3.1 Thereportinglimitinthistestmethodistheminimum
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
reporting limit are estimated concentrations and are not re-
Barriers to Trade (TBT) Committee.
ported following this test method. In most cases, the reporting
limit is calculated from the concentration of the Level 1 2. Referenced Documents
5
2.1 ASTM Standards:
D653Terminology Relating to Soil, Rock, and Contained
1
This test method is under the jurisdiction ofASTM Committee D34 on Waste
Fluids
Management and is the direct responsibility of Subcommittee D34.01.06 on
D1193Specification for Reagent Water
Analytical Methods.
D2777Practice for Determination of Precision and Bias of
Current edition approved May 1, 2017. Published May 2017. Originally
approved in 2014. Last previous edition approved in 2014 as D7968–14. DOI:
Applicable Test Methods of Committee D19 on Water
10.1520/D7968-17.
D3694Practices for Preparation of Sample Containers and
2
Washington, J. W., Naile, J. E., Jenkins, T. M., and Lynch, D. G., “Character-
for Preservation of Organic Constituents
izing Fluorotelomer and Polyfluoroalkyl Substances in New and Aged
Fluorotelomer-Based Polymers for Degradation Studies with GC/MS and LC/MS/ D3740Practice for Minimum Requirements for Agencies
MS,” Environmental Science and Technology, Vol 48, 2014, pp. 5762–5769.
Engaged in Testing and/or Inspection of Soil and Rock as
3
The MDL is determined following the Code of Federal Regulations, 40 CFR
Used in Engineering Design and Construction
Part 136, Appendix B utilizing solvent extraction of soil. Two-gram sample of
Ottawa sand was utilized.Adetailed 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 concentration is calculated from Table 2 concentrations For referenced ASTM standards, visit the ASTM website, www.astm.org, or
assuminga30-µLinjectionoftheLevel1calibrationstandardforthePFCs,andthe contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
...
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 − 14 D7968 − 17
Standard Test Method for
Determination of PerfluorinatedPolyfluorinated Compounds
in Soil by Liquid Chromatography Tandem Mass
1
Spectrometry (LC/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 perfluorinatedpolyfluorinated 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
2
by Washington et al.al., , 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.
3 4
1.3 The Method of Detection Limit and Reporting 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 perfluorinatedpolyfluorinated compounds after taking into account a 2 g 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 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,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.
2. Referenced Documents
5
2.1 ASTM Standards:
D653 Terminology Relating to Soil, Rock, and Contained Fluids
D1193 Specification for Reagent Water
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 Nov. 1, 2014May 1, 2017. Published December 2014May 2017. Originally approved in 2014. Last previous edition approved in 2014 as
D7968 – 14. DOI: 10.1520/D7968-14.10.1520/D7968-17.
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.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 Two-gram sample of
Ottawa Sandsand 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, and the highest
level calibration stan
...
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