ASTM D8421-22

Standard Test Method for Determination of Per- and Polyfluoroalkyl Substances (PFAS) in Aqueous Matrices by Co-solvation followed by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)

SIGNIFICANCE AND USE
5.1 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. PFAS have been detected in soils, sludges, surface, and drinking waters. This is a quick, easy, and robust method to quantitatively determine these compounds at trace levels in water matrices.  
5.2 This test method has been validated using reagent water and waters from sites that include landfill leachate, metal finisher, POTW Effluent, Hospital, POTW Influent, Bus washing station, Power Plant and Pulp and paper mill effluent for selected PFAS, refer to the Precision and Bias (Section 17).
SCOPE
1.1 This test method covers the determination of per- and polyfluoroalkyl substances (PFASs) in aqueous matrices using liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are co-solvated by a 1+1 ratio of sample and methanol then qualitatively and quantitatively determined by this test method. Quantitation is by selected reaction monitoring (SRM) or sometimes referred to as multiple reaction monitoring (MRM).  
1.2 The method detection limit (MDL) (see Note 1) and reporting range (see Note 2) for the target analytes are listed in Table 1. The target concentration for the reporting limit for this test method is an integer value that is calculated from the concentration from the lowest standard from the final volume of the prepared sample. This value may be lower than the calculated MDL due to sporadic PFAS hits due to PFAS contamination in consumables/collection tools used during sample collection and preparation. All samples should be taken at a minimal as duplicates in order to compare the precision between the two prepared samples to help ensure the concentration/positive result is reliable.
Note 1: The MDL is determined following the Code of Federal Regulations (CFR), 40 CFR Part 136, Appendix B utilizing dilution and filtration. A detailed process determining the MDL is explained in the reference and is beyond the scope of this test method.
Note 2: Injection volume variations, and sensitivity of the instrument used will change the reporting limit and ranges.  
1.2.1 Recognizing continual advancements in the sensitivity of instrumentation, advancements in column chromatography and other processes not recognized here, the reporting limit may be lowered assuming the minimum performance requirements of this test method at the lower concentrations are met.  
1.2.2 Depending on data usage, you may modify this test method but limit to modifications that improve performance while still meeting or exceeding the method quality acceptance criteria. Modifications to the solvents, ratio of solvent to sample, or shortening the chromatographic run simply to save time are not allowed. Use Practice E2935 or similar statistical tests to confirm that modifications produce equivalent results on non-interfering samples. In addition, use Guide E2857 or equivalent statistics to re-validate the modified test.  
1.2.3 Analyte detections between the method detection limit and the reporting limit are estimated concentrations. The reporting limit is based upon the concentration of the Level 1 calibration standard as shown in Table 5.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on P...

General Information

• Status: Published
• Publication Date: 30-Apr-2022
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

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:D8421 −22
Standard Test Method for
Determination of Per- and Polyfluoroalkyl Substances
(PFAS) in Aqueous Matrices by Co-solvation followed by
Liquid Chromatography Tandem Mass Spectrometry (LC/
1
MS/MS)
This standard is issued under the fixed designation D8421; 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 1.2.2 Depending on data usage, you may modify this test
method but limit to modifications that improve performance
1.1 This test method covers the determination of per- and
whilestillmeetingorexceedingthemethodqualityacceptance
polyfluoroalkyl substances (PFASs) in aqueous matrices using
criteria. Modifications to the solvents, ratio of solvent to
liquid chromatography (LC) and detection with tandem mass
sample, or shortening the chromatographic run simply to save
spectrometry (MS/MS). These analytes are co-solvated by a
time are not allowed. Use Practice E2935 or similar statistical
1+1 ratio of sample and methanol then qualitatively and
tests to confirm that modifications produce equivalent results
quantitatively determined by this test method. Quantitation is
on non-interfering samples. In addition, use Guide E2857 or
by selected reaction monitoring (SRM) or sometimes referred
equivalent statistics to re-validate the modified test.
to as multiple reaction monitoring (MRM).
1.2.3 Analytedetectionsbetweenthemethoddetectionlimit
1.2 The method detection limit (MDL) (see Note 1) and
and the reporting limit are estimated concentrations. The
reportingrange(seeNote2)forthetargetanalytesarelistedin
reporting limit is based upon the concentration of the Level 1
Table1.Thetargetconcentrationforthereportinglimitforthis
calibration standard as shown in Table 5.
test method is an integer value that is calculated from the
1.3 The values stated in SI units are to be regarded as
concentration from the lowest standard from the final volume
standard. No other units of measurement are included in this
of the prepared sample. This value may be lower than the
standard.
calculated MDL due to sporadic PFAS hits due to PFAS
1.4 This standard does not purport to address all of the
contamination in consumables/collection tools used during
safety concerns, if any, associated with its use. It is the
samplecollectionandpreparation.Allsamplesshouldbetaken
responsibility of the user of this standard to establish appro-
at a minimal as duplicates in order to compare the precision
priate safety, health, and environmental practices and deter-
between the two prepared samples to help ensure the
mine the applicability of regulatory limitations prior to use.
concentration/positive result is reliable.
1.5 This international standard was developed in accor-
NOTE 1—The MDL is determined following the Code of Federal
dance with internationally recognized principles on standard-
Regulations (CFR), 40 CFR Part 136, Appendix B utilizing dilution and
ization established in the Decision on Principles for the
filtration. A detailed process determining the MDL is explained in the
Development of International Standards, Guides and Recom-
reference and is beyond the scope of this test method.
mendations issued by the World Trade Organization Technical
NOTE 2—Injection volume variations, and sensitivity of the instrument
used will change the reporting limit and ranges.
Barriers to Trade (TBT) Committee.
1.2.1 Recognizingcontinualadvancementsinthesensitivity
2. Referenced Documents
of instrumentation, advancements in column chromatography
2
and other processes not recognized here, the reporting limit 2.1 ASTM Standards:
may be lowered assuming the minimum performance require- D1129Terminology Relating to Water
ments of this test method at the lower concentrations are met. D1193Specification for Reagent Water
D2777Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
2
Organic Substances in Water. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2022. Published June 2022. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 2021. Last previous edition approved in 2021 as D8421–21. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D8421-22. the ASTM w
...

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: D8421 − 21 D8421 − 22
Standard Test Method for
Determination of Per- and Polyfluoroalkyl Substances
(PFAS) in Aqueous Matrices by Co-solvation followed by
Liquid Chromatography Tandem Mass Spectrometry (LC/
1
MS/MS)
This standard is issued under the fixed designation D8421; 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 test method covers the determination of per- and polyfluoroalkyl substances (PFASs) in aqueous matrices using liquid
chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are co-solvated by a 1+1 ratio of
sample and methanol then qualitatively and quantitatively determined by this test method. Quantitation is by selected reaction
monitoring (SRM) or sometimes referred to as multiple reaction monitoring (MRM).
1.2 The method detection limit (MDL) (see Note 1) and reporting range (see Note 2) for the target analytes are listed in Table 1.
The target concentration for the reporting limit for this test method is an integer value that is calculated from the concentration
from the lowest standard from the final volume of the prepared sample. This value may be lower than the calculated MDL due
to sporadic PFAS hits due to PFAS contamination in consumables/collection tools used during sample collection and preparation.
All samples should be taken at a minimal as duplicates in order to compare the precision between the two prepared samples to help
ensure the concentration/positive result is reliable.
NOTE 1—The MDL is determined following the Code of Federal Regulations (CFR), 40 CFR Part 136, Appendix B utilizing dilution and filtration. A
detailed process determining the MDL is explained in the reference and is beyond the scope of this test method.
NOTE 2—Injection volume variations, and sensitivity of the instrument used will change the reporting limit and ranges.
1.2.1 Recognizing continual advancements in the sensitivity of instrumentation, advancements in column chromatography and
other processes not recognized here, the reporting limit may be lowered assuming the minimum performance requirements of this
test method at the lower concentrations are met.
1.2.2 Depending on data usage, you may modify this test method but limit to modifications that improve performance while still
meeting or exceeding the method quality acceptance criteria. Modifications to the solvents, ratio of solvent to sample, or shortening
the chromatographic run simply to save time are not allowed. Use Practice E2935 or similar statistical tests to confirm that
modifications produce equivalent results on non-interfering samples. In addition, use Guide E2857 or equivalent statistics to
re-validate the modified test.
1.2.3 Analyte detections between the method detection limit and the reporting limit are estimated concentrations. The reporting
limit is based upon the concentration of the Level 1 calibration standard as shown in Table 5.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved Nov. 1, 2021May 1, 2022. Published December 2021June 2022. Originally approved in 2021. Last previous edition approved in 2021 as
D8421 – 21. DOI: 10.1520/D8421-21.10.1520/D8421-22.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D8421 − 22
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards
...