ASTM D 7968 : 2017 : REV A
Superseded
A superseded Standard is one, which is fully replaced by another Standard, which is a new edition of the same Standard.
View Superseded by
Standard Test Method for Determination of Polyfluorinated Compounds in Soil by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
Hardcopy , PDF
09-11-2023
English
07-09-2017
1.1 This procedure covers the determination of selected polyfluorinated compounds (PFCs) in a soil matrix using solvent extraction, filtration, followed by liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS).
Committee |
D 34
|
DocumentType |
Test Method
|
Pages |
24
|
PublisherName |
American Society for Testing and Materials
|
Status |
Superseded
|
SupersededBy | |
Supersedes |
1.1This procedure covers the determination of selected polyfluorinated 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.
1.2Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3The Method of Detection Limit3 and Reporting Range4 for the target analytes are listed in Table 1.
TABLE 1 Method Detection Limit and Reporting RangeA
Analyte | MDL | Reporting Limit |
PFTreA | 6.76 | 25–1000 |
PFTriA | 5.26 | 25–1000 |
PFDoA | 3.56 | 25–1000 |
PFUnA | 2.45 | 25–1000 |
PFDA | 5.54 | 25–1000 |
PFOS | 18.83 | 50–1000 |
PFNA | 2.82 | 25–1000 |
PFecHS | 2.41 | 25–1000 |
PFOA | 6.24 | 25–1000 |
PFHxS | 7.75 | 25–1000 |
PFHpA | 5.80 | 25–1000 |
PFHxA | 15.44 | 50–1000 |
PFBS | 6.49 | 25–1000 |
PFPeA | 20.93 | 125–5000 |
PFBA | 22.01 | 125–5000 |
FHEA | 199.04 | 600–20 000 |
FOEA | 258.37 | 750–20 000 |
FDEA | 137.46 | 500–20 000 |
FOUEA | 4.85 | 25–1000 |
FhpPa | 5.09 | 25–1000 |
FHUEA | 3.50 | 25–1000 |
TABLE 2 Concentrations of Calibration Standards (ng/L)
Analyte/Surrogate | LV1 | LV2 | LV3 | LV4 | LV5 | LV6 | LV7 | LV8 | LV9 |
PFPeA, PFBA | 25 | 50 | 100 | 200 | 300 | 400 | 500 | 750 | 1000 |
PFTreA, PFTriA, PFDoA, PFUnA, PFDA, PFOS, PFNA, PFHxA, PFHpA, PFBS, PFechS, PFOA, PFHxS, FOUEA, FHUEA, FHpPA, MPFBS, MPFHxA, MPFUnA, MPFOA, MPFDA, MPFOS, MPFNA, MPFHxS, MPFBA | 5 | 10 | 20 | 40 | 60 | 80 | 100 | 150 | 200 |
FHEA, FOEA, FDEA | 100 | 200 | 400 | 800 | 1200 | 1600 | 2000 | 3000 | 4000 |
1.3.1The 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 polyfluorinated 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.
1.4This 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.
1.5This 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.
ASTM F 2931 : 2019 | Standard Guide for Analytical Testing of Substances of Very High Concern in Materials and Products |
ASTM E 3358 : 2023 : REV A | Standard Guide for Per- and Polyfluoroalkyl Substances Site Screening and Initial Characterization |
ASTM F 2931 : 2019 : REV A | Standard Guide for Analytical Testing of Substances of Very High Concern in Materials and Products |
ASTM E 3302 : 2022 | Standard Guide for PFAS Analytical Methods Selection |
ASTM D 5847 : 1999 : REV A : EDT 1 | Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis |
ASTM D 2777 : 2012 | Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water |
ASTM D 1193 : 1977 : R1983 : EDT 1 | Standard Specification for Reagent Water |
ASTM D 5847 : 2002 : R2007 | Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis |
ASTM D 2777 : 2003 | Standard Practice for Determination of Precision and Bias of Applicable Methods of Committee D-19 on Water |
ASTM D 2777 : 2021 | Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water |
ASTM D 2777 : 2013 | Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water |
ASTM E 2554 : 2013 | Standard Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques |
ASTM D 5847 : 2002 : R2012 | Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis |
ASTM D 2777 : 1998 | Standard Practice for Determination of Precision and Bias of Applicable Methods of Committee D-19 on Water |
ASTM D 1193 : 2006 : R2011 | Standard Specification for Reagent Water |
ASTM D 5847 : 2002 : R2020 | Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis |
ASTM E 2554 : 2018 : EDT 1 | Standard Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques |
ASTM D 1193 : 1991 | Standard Specification for Reagent Water |
ASTM D 5847 : 2022 | Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis |
ASTM D 2777 : 2008 | Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water |
ASTM E 2554 : 2007 | Standard Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method in a Single Laboratory Using a Control Sample Program |
ASTM D 2777 : 2006 | Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water |
ASTM E 2554 : 2018 | Standard Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques |
ASTM D 5847 : 2002 | Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis |
ASTM D 1193 : 1970 | Standard Specification For Reagent Water |
ASTM D 1193 : 2006 | Standard Specification for Reagent Water |
ASTM D 1193 : 1999 | Standard Specification for Reagent Water |
ASTM D 1193 : 2006 : R2018 | Standard Specification for Reagent Water |
ASTM D 2777 : 2008 : EDT 1 | Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water |
Access your standards online with a subscription
Features
-
Simple online access to standards, technical information and regulations.
-
Critical updates of standards and customisable alerts and notifications.
-
Multi-user online standards collection: secure, flexible and cost effective.