ASTM D7979-15e1
(Test Method)Standard Test Method for Determination of Perfluorinated Compounds in Water, Sludge, Influent, Effluent and Wastewater by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
Standard Test Method for Determination of Perfluorinated Compounds in Water, Sludge, Influent, Effluent and Wastewater by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
SIGNIFICANCE AND USE
5.1 This test method has been developed by the US 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.6 PFCs 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.
5.3 This method has been investigated for use with reagent, surface, sludge and wastewaters for selected perfluorinated compounds.
SCOPE
1.1 This procedure covers the determination of selected perfluorinated compounds (PFCs) 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 method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry.
1.2 The Method Detection Limit (MDL)2 and Reporting Range3 for the target analytes are listed in Table 1. (A) Acronyms are defined in 3.3.
1.2.1 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 the concentration of the Level 1 calibration standard as shown in Table 4 for the perfluorinated compounds after taking into account the 50 % dilution with methanol. It is above the Level 1 calibration concentration for PFOS, PFBS, 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 Units—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 and health practices and determine the applicability of regulatory limitations prior to use.
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´1
Designation:D7979 −15
StandardTest Method for
Determination of Perfluorinated Compounds 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
ε NOTE—Editorial corrections were made throughout in November 2015.
1. Scope responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 This procedure covers the determination of selected
bility of regulatory limitations prior to use.
perfluorinated compounds (PFCs) in a water matrix using
liquid chromatography (LC) and detection with tandem mass
2. Referenced Documents
spectrometry (MS/MS). These analytes are qualitatively and
4
2.1 ASTM Standards:
quantitativelydeterminedbythismethod.Thismethodadheres
D1129Terminology Relating to Water
to multiple reaction monitoring (MRM) mass spectrometry.
D1193Specification for Reagent Water
2
1.2 The Method Detection Limit (MDL) and Reporting
D2777Practice for Determination of Precision and Bias of
3
Range for the target analytes are listed in Table 1.
Applicable Test Methods of Committee D19 on Water
1.2.1 Thereportinglimitinthistestmethodistheminimum
D3856Guide for Management Systems in Laboratories
value below which data are documented as non-detects. Ana-
Engaged in Analysis of Water
lyte detections between the method detection limit and the
D3694Practices for Preparation of Sample Containers and
reporting limit are estimated concentrations and are not re-
for Preservation of Organic Constituents
ported following this test method. In most cases, the reporting
D4841Practice for Estimation of Holding Time for Water
limitistheconcentrationoftheLevel1calibrationstandardas
Samples Containing Organic and Inorganic Constituents
showninTable4fortheperfluorinatedcompoundsaftertaking
D5847Practice for Writing Quality Control Specifications
into account the 50 % dilution with methanol. It is above the
for Standard Test Methods for Water Analysis
Level 1 calibration concentration for PFOS, PFBS, FHEAand
E2554Practice for Estimating and Monitoring the Uncer-
FOEA, these compounds can be identified at the Level 1
tainty of Test Results of a Test Method Using Control
concentration but the standard deviation among replicates at
Chart Techniques
this lower spike level resulted in a higher reporting limit.
5
2.2 Other Standards:
1.3 Units—The values stated in SI units are to be regarded
EPAPublicationSW-846,TestMethodsforEvaluatingSolid
asstandard.Nootherunitsofmeasurementareincludedinthis
Waste, Physical/Chemical Methods
standard.
The Code of Federal Regulations40 CFR Part 136,Appen-
1.4 This standard does not purport to address all of the dix B
safety concerns, if any, associated with its use. It is the
3. Terminology
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
3.1 Definitions:
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
3.1.1 For definitions of terms used in this standard, refer to
Organic Substances in Water.
Terminology D1129.
Current edition approved Jan. 1, 2015. Published February 2015. DOI: 10.1520/
D7979-15E01.
2
The MDL is determined following the Code of Federal Regulations, 40 CFR
4
Part 136, Appendix B utilizing dilution and filtration. 5 mL sample of water was For referenced ASTM standards, visit the ASTM website, www.astm.org, or
utilized.Adetailed process determining the MDLis explained in the reference and contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
is beyond the scope of this test method to be explained here. Standards volume information, refer to the standard’s Document Summary page on
3
Reporting range concentration is calculated from Table 4 concentrations the ASTM website.
5
assuming a 30 µL injection of the Level 1 calibration standard for PFCs, and the Available from National Technical Information Service (NTIS), U.S. Depart-
highestlevelcalibrationstandardwitha10mLfinalextractvolumeofa5mLwater ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
sample. Volume variations will change the reporting limit and ranges. www.epa.gov/epawaste/hazard/testmethods/index.htm
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D7979−15
13
TABLE 1 Method Detection Limit and Reporting Range
3.3.11.1 MPFBA, n— C -Perfluorobutanoate
4
13
MDL Reporting Ranges
A
3.3.
...
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.
´1
Designation: D7979 − 15 D7979 − 15
Standard Test Method for
Determination of Perfluorinated Compounds 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
ε NOTE—Editorial corrections were made throughout in November 2015.
1. Scope
1.1 This procedure covers the determination of selected perfluorinated compounds (PFCs) 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 method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry.
2 3
1.2 The Method Detection Limit (MDL) and Reporting Range for the target analytes are listed in Table 1.
1.2.1 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 the concentration of the Level 1 calibration standard as shown in Table 4Table
4 for the perfluorinated compounds after taking into account the 50 % dilution with methanol. It is above the Level 1 calibration
concentration for PFOS, PFBS, 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 Units—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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
4
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
D4841 Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic Constituents
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
E2554 Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques
5
2.2 Other Standards:
EPA Publication SW-846, Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
The Code of Federal Regulations 40 CFR Part 136, Appendix B
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 Jan. 1, 2015. Published February 2015. DOI: 10.1520/D7979-15.10.1520/D7979-15E01.
2
The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B utilizing dilution and filtration. 5 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 PFCs, 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.
4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
5
Available from National Technical Information Service (NTIS), U.S. Department of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://www.epa.gov/
epawaste/hazard/testmethods/index.htm
Copyright © ASTM Internatio
...
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