ASTM D7968-14
(Test Method)Standard Test Method for Determination of Perfluorinated Compounds in Soil by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
Standard Test Method for Determination of Perfluorinated Compounds in Soil 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.7 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 various soil matrices for understanding of the sources and pathways of exposure.
5.3 This method has been used to determine selected perfluorinated compounds in sand (Table 4) and four ASTM reference soils (Table 5).
SCOPE
1.1 This procedure covers the determination of selected perfluorinated compounds (PFCs) in a soil matrix using solvent extraction, filtration, followed by 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. This procedure utilizes a quick extraction and is not intended to generate an exhaustive accounting of the content of PFCs in difficult soil matrices. An exhaustive extraction procedure for polyfluoralkyl substances, such as published by Washington et al.2, for difficult matrices should be considered when analyzing PFCs.
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 The Method of Detection Limit3 and Reporting Range4 for the target analytes are listed in Table 1. (A) Abbreviations are defined in 3.2.
1.3.1 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 calculated from the concentration of the Level 1 calibration standard as shown in Table 2 for the perfluorinated compounds after taking into account a 2 g sample weight and a final extract volume of 10 mL, 50 % water/50 % MeOH with 0.1 % acetic acid. The final extract volume is assumed to be 10 mL because 10 mL of 50 % water/50 % MeOH with 0.1 % acetic acid was added to each soil sample and only the liquid layer after extraction is filtered leaving the solid and any residual solvent behind. It is raised above the Level 1 calibration concentration for PFOS, PFHxA, 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.
1.4 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:D7968 −14
Standard Test Method for
Determination of Perfluorinated Compounds in Soil by
Liquid Chromatography Tandem Mass Spectrometry (LC/
1
MS/MS)
This standard is issued under the fixed designation D7968; 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 compounds after taking into account a 2 g sample weight and
afinalextractvolumeof10mL,50%water/50%MeOHwith
1.1 This procedure covers the determination of selected
0.1%aceticacid.Thefinalextractvolumeisassumedtobe10
perfluorinatedcompounds(PFCs)inasoilmatrixusingsolvent
mL because 10 mL of 50% water/50% MeOH with 0.1%
extraction, filtration, followed by liquid chromatography (LC)
acetic acid was added to each soil sample and only the liquid
anddetectionwithtandemmassspectrometry(MS/MS).These
layer after extraction is filtered leaving the solid and any
analytesarequalitativelyandquantitativelydeterminedbythis
residual solvent behind. It is raised above the Level 1 calibra-
method. This method adheres to multiple reaction monitoring
tionconcentrationforPFOS,PFHxA,FHEA,andFOEA,these
(MRM) mass spectrometry. This procedure utilizes a quick
compounds can be identified at the Level 1 concentration but
extraction and is not intended to generate an exhaustive
the standard deviation among replicates at this lower spike
accounting of the content of PFCs in difficult soil matrices.An
level resulted in a higher reporting limit.
exhaustive extraction procedure for polyfluoralkyl substances,
2
1.4 This standard does not purport to address all of the
such as published by Washington et al. , for difficult matrices
safety concerns, if any, associated with its use. It is the
should be considered when analyzing PFCs.
responsibility of the user of this standard to establish appro-
1.2 Units—The values stated in SI units are to be regarded
priate safety and health practices and determine the applica-
asstandard.Nootherunitsofmeasurementareincludedinthis
bility of regulatory limitations prior to use.
standard.
3 4
2. Referenced Documents
1.3 The Method of Detection Limit and Reporting Range
5
for the target analytes are listed in Table 1.
2.1 ASTM Standards:
1.3.1 Thereportinglimitinthistestmethodistheminimum
D653Terminology Relating to Soil, Rock, and Contained
value below which data are documented as non-detects. Ana-
Fluids
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 calculated from the concentration of the Level 1
D3694Practices for Preparation of Sample Containers and
calibration standard as shown in Table 2 for the perfluorinated
for Preservation of Organic Constituents
D3740Practice for Minimum Requirements for Agencies
Engaged in Testing and/or Inspection of Soil and Rock as
1
This test method is under the jurisdiction ofASTM Committee D34 on Waste
Used in Engineering Design and Construction
Management and is the direct responsibility of Subcommittee D34.01.06 on
D3856Guide for Management Systems in Laboratories
Analytical Methods.
Engaged in Analysis of Water
Current edition approved Nov. 1, 2014. Published December 2014. DOI:
10.1520/D7968-14. D5681Terminology for Waste and Waste Management
2
Washington, J. W., Naile, J. E., Jenkins, T. M., and Lynch, D. G., “Character-
D5847Practice for Writing Quality Control Specifications
izing Fluorotelomer and Polyfluoroalkyl Substances in New and Aged
for Standard Test Methods for Water Analysis
Fluorotelomer-Based Polymers for Degradation Studies with GC/MS and LC/MS/
E2554Practice for Estimating and Monitoring the Uncer-
MS,” Environmental Science and Technology, Vol. 48, 2014, pp. 5762–5769.
3
The MDL is determined following the Code of Federal Regulations, 40 CFR
tainty of Test Results of a Test Method Using Control
Part 136, Appendix B utilizing solvent extraction of soil. Two gram sample of
Chart Techniques
Ottawa Sand was utilized.Adetailed process determining the MDLis explained in
the reference and is beyond the scope of this standard to be explained here.
4 5
Reporting range concentration is calculated from Table 2 concentrations For referenced ASTM standards, visit the ASTM website, www.astm.org, or
assuminga30µLinjectionoftheLevel1calibrationstandardforthePFCs,andthe contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
highest level calibration standard with a 10 mL final extract volume ofa2g s
...
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