ASTM D7979-15
(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.
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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D7979 −15
StandardTest Method for
Determination of Perfluorinated Compounds in Water,
Sludge, Influent, Effluent and Wastewater by Liquid
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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 priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1.1 This procedure covers the determination of selected
perfluorinated compounds (PFCs) in a water matrix using
2. Referenced Documents
liquid chromatography (LC) and detection with tandem mass
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2.1 ASTM Standards:
spectrometry (MS/MS). These analytes are qualitatively and
D1129Terminology Relating to Water
quantitativelydeterminedbythismethod.Thismethodadheres
D1193Specification for Reagent Water
to multiple reaction monitoring (MRM) mass spectrometry.
D2777Practice for Determination of Precision and Bias of
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1.2 The Method Detection Limit (MDL) and Reporting
Applicable Test Methods of Committee D19 on Water
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Range for the target analytes are listed in Table 1.
D3856Guide for Management Systems in Laboratories
1.2.1 Thereportinglimitinthistestmethodistheminimum
Engaged in Analysis of Water
value below which data are documented as non-detects. Ana-
D3694Practices for Preparation of Sample Containers and
lyte detections between the method detection limit and the
for Preservation of Organic Constituents
reporting limit are estimated concentrations and are not re-
D4841Practice for Estimation of Holding Time for Water
ported following this test method. In most cases, the reporting
Samples Containing Organic and Inorganic Constituents
limitistheconcentrationoftheLevel1calibrationstandardas
D5847Practice for Writing Quality Control Specifications
showninTable4fortheperfluorinatedcompoundsaftertaking
for Standard Test Methods for Water Analysis
into account the 50 % dilution with methanol. It is above the
E2554Practice for Estimating and Monitoring the Uncer-
Level 1 calibration concentration for PFOS, PFBS, FHEAand
tainty of Test Results of a Test Method Using Control
FOEA, these compounds can be identified at the Level 1
Chart Techniques
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concentration but the standard deviation among replicates at
2.2 Other Standards:
this lower spike level resulted in a higher reporting limit.
EPAPublicationSW-846,TestMethodsforEvaluatingSolid
Waste, Physical/Chemical Methods
1.3 Units—The values stated in SI units are to be regarded
The Code of Federal Regulations40 CFR Part 136,Appen-
asstandard.Nootherunitsofmeasurementareincludedinthis
dix B
standard.
1.4 This standard does not purport to address all of the 3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 Definitions:
responsibility of the user of this standard to establish appro-
3.1.1 For definitions of terms used in this standard, refer to
Terminology D1129.
3.2 Definitions of Terms Specific to This Standard:
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This test method is under the jurisdiction ofASTM Committee D19 on Water
3.2.1 perfluorinated compounds, n—in this test method, 11
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
perfluoroalkyl carboxylic acids, 3 perfluoroalkylsulfonates,
Organic Substances in Water.
Current edition approved Jan. 1, 2015. Published February 2015. DOI: 10.1520/ Decafluoro-4-(pentafluoroethyl)cyclohexanesulfonate and 6
D7979-15.
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The MDL is determined following the Code of Federal Regulations, 40 CFR
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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
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Reporting range concentration is calculated from Table 4 concentrations the ASTM website.
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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
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