ASTM D7979-20
(Test Method)Standard Test Method for Determination of Per- and Polyfluoroalkyl Substances in Water, Sludge, Influent, Effluent, and Wastewater by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
Standard Test Method for Determination of Per- and Polyfluoroalkyl Substances in Water, Sludge, Influent, Effluent, and Wastewater by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
SIGNIFICANCE AND USE
5.1 PFASs are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFASs 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.6 PFASs have been detected in soils, sludges, surface, and drinking waters. Hence, there is a need for quick, easy, and robust method to determine these compounds at trace levels in water matrices for understanding of the sources and pathways of exposure.
5.2 This test method has been investigated for use with reagent, surface, sludge and wastewaters for selected PFASs. This test method has not been evaluated on drinking water matrices.
SCOPE
1.1 This procedure covers the determination of selected per- and polyfluoroalkyl substances (PFASs) in a water matrix using liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this test method. This test method adheres to a technique known as selected reaction monitoring (SRM) or sometimes referred to as multiple reaction monitoring (MRM). This is not a drinking water method; performance of this test method has not been evaluated on drinking water matrices.
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 was 10 ng/L for most of the target analytes at the time of development.
1.2.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The reporting limit may be lowered providing your lab meets the minimum performance requirements of this test method at the lower concentrations, this test method is performance based and modifications are allowed to improve performance. 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 the concentration of the Level 1 calibration standard as shown in Table 4 for the PFASs after taking into account the 50 % dilution with methanol. It is above the Level 1 calibration concentration for 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.
1.3 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.
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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:D7979 −20
Standard Test Method for
Determination of Per- and Polyfluoroalkyl Substances in
Water, Sludge, Influent, Effluent, and Wastewater by Liquid
1
Chromatography Tandem Mass Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation D7979; 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 tion concentration for FHEAand FOEA, these compounds can
be identified at the Level 1 concentration but the standard
1.1 Thisprocedurecoversthedeterminationofselectedper-
deviation among replicates at this lower spike level resulted in
and polyfluoroalkyl substances (PFASs) in a water matrix
a higher reporting limit.
using liquid chromatography (LC) and detection with tandem
mass spectrometry (MS/MS). These analytes are qualitatively 1.3 The values stated in SI units are to be regarded as
and quantitatively determined by this test method. This test standard. No other units of measurement are included in this
method adheres to a technique known as selected reaction standard.
monitoring (SRM) or sometimes referred to as multiple reac-
1.4 This standard does not purport to address all of the
tion monitoring (MRM). This is not a drinking water method;
safety concerns, if any, associated with its use. It is the
performance of this test method has not been evaluated on
responsibility of the user of this standard to establish appro-
drinking water matrices.
priate safety, health, and environmental practices and deter-
2
mine the applicability of regulatory limitations prior to use.
1.2 The method detection limit (MDL) and reporting
3
1.5 This international standard was developed in accor-
range for the target analytes are listed in Table 1. The target
dance with internationally recognized principles on standard-
concentration for the reporting limit for this test method was
ization established in the Decision on Principles for the
10 ng/L for most of the target analytes at the time of
Development of International Standards, Guides and Recom-
development.
mendations issued by the World Trade Organization Technical
1.2.1 Thereportinglimitinthistestmethodistheminimum
Barriers to Trade (TBT) Committee.
value below which data are documented as non-detects. The
reporting limit may be lowered providing your lab meets the
2. Referenced Documents
minimum performance requirements of this test method at the
4
lower concentrations, this test method is performance based 2.1 ASTM Standards:
and modifications are allowed to improve performance. Ana- D1129Terminology Relating to Water
lyte detections between the method detection limit and the D1193Specification for Reagent Water
reporting limit are estimated concentrations and are not re- D2777Practice for Determination of Precision and Bias of
ported following this test method. In most cases, the reporting Applicable Test Methods of Committee D19 on Water
limit is the concentration of the Level 1 calibration standard as D3856Guide for Management Systems in Laboratories
shown in Table 4 for the PFASs after taking into account the Engaged in Analysis of Water
50 % dilution with methanol. It is above the Level 1 calibra- D3694Practices for Preparation of Sample Containers and
for Preservation of Organic Constituents
D4841Practice for Estimation of Holding Time for Water
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
Samples Containing Organic and Inorganic Constituents
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
D5847Practice for Writing Quality Control Specifications
Organic Substances in Water.
Current edition approved Aug. 15, 2020. Published August 2020. Originally for Standard Test Methods for Water Analysis
approved in 2015. Last previous edition approved in 2019 as D7979–19. DOI:
E2554Practice for Estimating and Monitoring the Uncer-
10.1520/D7979-20.
tainty of Test Results of a Test Method Using Control
2
The MDLis determined following the Code of Federal Regulations (CFR) , 40
Chart Techniques
CFRPart136,AppendixButilizingdilutionandfiltration.Five-mLsampleofwater
was utilized.Adetailed process determining the MDLis explained in the reference
and is beyond the scope of this test method to be explained here.
3 4
Reporting range concentration is calculated from Table 4 concentrations For referenced ASTM standards, visit the ASTM website, www.astm.org, or
assuming a 30-µL injection of the Level 1 calibration standard for PFASs, and the contact
...
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: D7979 − 19 D7979 − 20
Standard Test Method for
Determination of Per- and Polyfluoroalkyl Substances in
Water, Sludge, Influent, Effluent, and Wastewater by Liquid
1
Chromatography Tandem Mass Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation D7979; 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 per- and polyfluoroalkyl substances (PFASs) in a water matrix using liquid
chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively
determined by this test method. This test method adheres to a technique known as selected reaction monitoring (SRM) or
sometimes referred to as multiple reaction monitoring (MRM). This is not a drinking water method; performance of this test
method has not been evaluated on drinking water matrices.
2 3
1.2 The method detection limit (MDL) and reporting range for the target analytes are listed in Table 1. The target concentration
for the reporting limit for this test method was 10 ng/L for most of the target analytes at the time of development.
1.2.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The reporting
limit may be lowered providing your lab meets the minimum performance requirements of this test method at the lower
concentrations, this test method is performance based and modifications are allowed to improve performance. 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 the concentration of the Level 1 calibration standard as shown in Table 4 for the PFASs
after taking into account the 50 % dilution with methanol. It is above the Level 1 calibration concentration for 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.
1.3 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.
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, 2019Aug. 15, 2020. Published November 2019August 2020. Originally approved in 2015. Last previous edition approved in 20172019
as D7979 – 17.D7979 – 19. DOI: 10.1520/D7979-19.10.1520/D7979-20.
2
The MDL is determined following the Code of Federal Regulations (CFR) , 40 CFR Part 136, Appendix B utilizing dilution and filtration. Five-mL sample of water was
utilized. A detailed process determining the MDL is explained in the reference and is beyond the scope of this test method to be explained here.
3
Reporting range concentration is calculated from Table 4 concentrations assuming a 30-μL injection of the Level 1 calibration standard for PFASs, and the highest level
calibration standard with a 10-mL final extract volume of a 5-mL water sample. Volume variations will change the reporting limit and ranges.
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D7979 − 20
TABLE 1 Method Detection Limit and Reporting Range
MDL Reporting Ranges
A
Analyte
(ng/L) (ng/L)
B
PFTreA 1.2 10 – 400
B
PFTriA 0.7 10 – 400
B
PFDoA 1.2 10 – 400
B
PFUnA 1.2 10 – 400
B
PFDA 1.4 10 – 400
B
PFOS 2.2 10 – 400
B
PFNA 1.1 10 – 400
B
PFecHS
...
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