ASTM D7968 - 17a

    Standard Test Method for Determination of Polyfluorinated Compounds in Soil by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)

    Active Standard ASTM D7968 | Developed by Subcommittee: D34.01.06

    Book of Standards Volume: 11.04


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    Significance and Use

    5.1 This test method has been developed by the U.S. 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, and surface and drinking waters. Hence, there is a need for a 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 polyfluorinated compounds in sand (Table 4) and four ASTM reference soils (Table 5).

    TABLE 4 Single-Laboratory Recovery Data in Ottawa Sand

    Sample

    Measured ng/kg from Ottawa Sand P&A Data (400 ng/kg spike for all PFCs except 2000 ng/kg for PFBA and PFPeA and 8000 ng/kg spike for FHEA, FDEA, and FOEA)

    PFTreA

    PFTriA

    PFDoA

    PFUnA

    PFDA

    PFNA

    PFOA

    PFHpA

    PFHxA

    PFPeA

    PFBA

    Unspiked 1

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    Unspiked 2

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    P&A 1

    389.6

    394.3

    384.7

    376.7

    362.1

    347.6

    345.8

    232.9

    222.2

    1614.9

    1344.5

    P&A 2

    462.1

    424.6

    397.2

    379.1

    378.4

    376.9

    365.9

    247.9

    229.8

    1710.1

    1388

    P&A 3

    402.7

    387.7

    383.1

    365.9

    374.7

    363.3

    347.1

    242.4

    222.9

    1658.9

    1376

    P&A 4

    403.9

    397.1

    395.4

    381.5

    379

    359.4

    342.7

    246.8

    225.8

    1693.6

    1401.9

    P&A 5

    467.2

    445.8

    412.6

    388.5

    376.8

    370.3

    369.7

    249.3

    231.4

    1716.5

    1433.4

    P&A 6

    392.1

    385.3

    374.2

    370.9

    353.2

    351.7

    340.3

    236.7

    220.5

    1659

    1366.4

    Mean Recovery (ng/kg)

    419.6

    405.8

    391.2

    377.1

    370.7

    361.5

    351.9

    242.7

    225.4

    1675.5

    1385

    % Mean Recovery

    104.9

    101.4

    97.8

    94.3

    92.7

    90.4

    88

    60.7

    56.4

    83.8

    69.3

    Standard Deviation

    35.4

    24.1

    13.5

    8

    10.6

    11.1

    12.6

    6.6

    4.4

    38.5

    30.7

    RSD (%)

    8.4

    5.9

    3.5

    2.1

    2.9

    3.1

    3.6

    11

    1.9

    2.3

    2.2

     

     

     

     

     

     

     

     

     

     

     

     

    Sample

    PFBS

    PFHxS

    PFOS

    PFechS

    FOUEA

    FHpPA

    FHUEA

    FHEA

    FOEA

    FDEA

     

    Unspiked 1

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

     

    Unspiked 2

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

    <RL

     

    P&A 1

    337.4

    349.1

    340.3

    342.8

    389.5

    371.3

    372.5

    7023.5

    8202.6

    8564.9

     

    P&A 2

    347.3

    358.3

    345.9

    347.2

    408.7

    377.2

    387.1

    7346.1

    8542.6

    9308

     

    P&A 3

    366.3

    330.1

    331.7

    345.4

    401.5

    361.4

    379

    6844.3

    7402.4

    8989.2

     

    P&A 4

    348.2

    343.6

    338.3

    347.6

    404.9

    377.5

    388.1

    7258.2

    7551.9

    9173.4

     

    P&A 5

    351.8

    361.7

    365.6

    362.6

    417.5

    395.1

    391.8

    7461.3

    7821.2

    9287.4

     

    P&A 6

    336.7

    343.4

    363.7

    342.5

    394.5

    356.9

    374.5

    7559.3

    8002.2

    8367.1

     

    Mean Recovery (ng/kg)

    347.9

    347.7

    347.7

    348

    402.7

    373.2

    382.1

    7248.8

    7920.5

    8948.3

     

    % Mean Recovery

    87

    86.9

    86.9

    87

    100.7

    93.3

    95.5

    90.6

    99

    111.9

     

    Standard Deviation

    10.9

    11.5

    13.9

    7.4

    10

    13.6

    7.9

    270.4

    421.3

    395.3

     

    RSD (%)

    3.1

    3.3

    4

    2.1

    2.5

    3.6

    2.1

    3.7

    5.3

    4.4

     

    TABLE 5 Single-Laboratory Surrogate Recovery Data in Ottawa Sand

    Sample

    Measured ng/kg from Ottawa Sand – 400 ng/kg spike

    MPFBA

    MPFHxA

    MPFHxS

    MPFOA

    MPFNA

    MPFOS

    MPFDA

    MPFUnA

    MPFDoA

    Unspiked 1

    420.0

    433.5

    431.8

    428.0

    439.4

    429.2

    442.6

    443.3

    447.7

    Unspiked 2

    366.5

    396.8

    378.5

    384.9

    389.8

    373.6

    404.9

    400.8

    425.8

    P&A 1

    361.1

    364.3

    356.3

    377.0

    376.6

    354.4

    384.9

    391.3

    409.3

    P&A 2

    383.6

    378.4

    357.3

    389.4

    379.7

    375.7

    395.7

    399.2

    412.2

    P&A 3

    374.5

    378.5

    375.4

    390.5

    378.6

    372.4

    382.5

    386.9

    402.2

    P&A 4

    370.1

    384.4

    366.1

    396.3

    384.4

    374.2

    397.8

    406.2

    420.5

    P&A 5

    370.1

    386.8

    372.0

    395.7

    381.1

    372.8

    394.4

    399.9

    421.5

    P&A 6

    363.6

    384.8

    356.1

    397.9

    384.9

    368.6

    389.5

    392.3

    402.9

    Mean Recovery (ng/kg dry weight)

    376.2

    388.4

    374.2

    394.9

    389.3

    377.6

    399.0

    402.5

    417.7

    % Mean Recovery

    94.0

    97.1

    93.5

    98.7

    97.3

    94.4

    99.8

    100.6

    104.4

    Standard Deviation

    19.0

    20.4

    24.9

    15.0

    20.7

    21.9

    19.0

    17.6

    14.9

    RSD (%)

    5.1

    5.3

    6.7

    3.8

    5.3

    5.8

    4.8

    4.4

    3.6

    1. Scope

    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). 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.

    TABLE 1 Method Detection Limit and Reporting RangeA

    Analyte

    MDL
    (ng/kg)

    Reporting Limit
    (ng/kg)

    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

    (A) Abbreviations are defined in 3.2.

    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

    1.3.1 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 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.

    1.4 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.


    2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

    ASTM Standards

    D1193 Specification for Reagent Water

    D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water

    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

    Other Documents

    40 CFR Part 136 Appendix B Definition and Procedure for the Determination of the Method Detection Limit

    EPA SW-846


    ICS Code

    ICS Number Code 13.080.10 (Chemical characteristics of soil)

    UNSPSC Code

    UNSPSC Code 11111501(Soil)


    Referencing This Standard
    Link Here
    Link to Active (This link will always route to the current Active version of the standard.)

    DOI: 10.1520/D7968-17A

    Citation Format

    ASTM D7968-17a, Standard Test Method for Determination of Polyfluorinated Compounds in Soil by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS), ASTM International, West Conshohocken, PA, 2017, www.astm.org

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