ASTM D8421-21

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)2 and reporting range3 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.  
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 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: Historical
• Publication Date: 31-Oct-2021
• 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)

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:D8421 −21
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 criteria. Modifications to the solvents, ratio of solvent to
sample, or shortening the chromatographic run simply to save
1.1 This test method covers the determination of per- and
time are not allowed. Use Practice E2935 or similar statistical
polyfluoroalkyl substances (PFASs) in aqueous matrices using
tests to confirm that modifications produce equivalent results
liquid chromatography (LC) and detection with tandem mass
on non-interfering samples. In addition, use Guide E2857 or
spectrometry (MS/MS). These analytes are co-solvated by a
equivalent statistics to re-validate the modified test.
1+1 ratio of sample and methanol then qualitatively and
1.2.3 Analytedetectionsbetweenthemethoddetectionlimit
quantitatively determined by this test method. Quantitation is
and the reporting limit are estimated concentrations. The
by selected reaction monitoring (SRM) or sometimes referred
reporting limit is based upon the concentration of the Level 1
to as multiple reaction monitoring (MRM).
calibration standard as shown in Table 5.
2
1.2 The method detection limit (MDL) and reporting
3
1.3 The values stated in SI units are to be regarded as
range for the target analytes are listed in Table 1. The target
standard. No other units of measurement are included in this
concentration for the reporting limit for this test method is an
standard.
integervaluethatiscalculatedfromtheconcentrationfromthe
1.4 This standard does not purport to address all of the
lowest standard from the final volume of the prepared sample.
safety concerns, if any, associated with its use. It is the
This value may be lower than the calculated MDL due to
responsibility of the user of this standard to establish appro-
sporadic PFAS hits due to PFAS contamination in
priate safety, health, and environmental practices and deter-
consumables/collection tools used during sample collection
mine the applicability of regulatory limitations prior to use.
and preparation. All samples should be taken at a minimal as
1.5 This international standard was developed in accor-
duplicates in order to compare the precision between the two
dance with internationally recognized principles on standard-
prepared samples to help ensure the concentration/positive
ization established in the Decision on Principles for the
result is reliable.
Development of International Standards, Guides and Recom-
1.2.1 Recognizingcontinualadvancementsinthesensitivity
mendations issued by the World Trade Organization Technical
of instrumentation, advancements in column chromatography
Barriers to Trade (TBT) Committee.
and other processes not recognized here, the reporting limit
may be lowered assuming the minimum performance require-
2. Referenced Documents
ments of this test method at the lower concentrations are met.
4
1.2.2 Depending on data usage, you may modify this test
2.1 ASTM Standards:
method but limit to modifications that improve performance
D1129Terminology Relating to Water
whilestillmeetingorexceedingthemethodqualityacceptance
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
D3856Guide for Management Systems in Laboratories
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water. Engaged in Analysis of Water
Current edition approved Nov. 1, 2021. Published December 2021. DOI:
D4841Practice for Estimation of Holding Time for Water
10.1520/D8421-21.
2
The MDLis determined following the Code of Federal Regulations (CFR), 40
CFR Part 136, Appendix B utilizing dilution and filtration. A detailed process
4
determining the MDL is explained in the reference and is beyond the scope of this For referenced ASTM standards, visit the ASTM website, www.astm.org, or
test method. contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
3
Injection volume variations, and sensitivity of the instrument used will change Standards volume information, refer to the standard’s Document Summary page on
the reporting limit and ranges. the ASTM website.
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