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WITHDRAWN ASTM D7968-17a 1.9.2017 preview

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ASTM D7968-17a

Standard Test Method for Determination of Polyfluorinated Compounds in Soil by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) (Includes all amendments And changes 11/6/2023).

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STANDARD published on 1.9.2017

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The information about the standard:

Designation standards: ASTM D7968-17a
Note: WITHDRAWN
Publication date standards: 1.9.2017
SKU: NS-693669
The number of pages: 24
Approximate weight : 72 g (0.16 lbs)
Country: American technical standard
Category: Technical standards ASTM

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Chemical characteristics of soils

Annotation of standard text ASTM D7968-17a :

Keywords:

liquid chromatography, mass spectrometry, polyfluorinated compounds, soils,, ICS Number Code 13.080.10 (Chemical characteristics of soil)

Additional information

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)
Sample	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
Sample	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.,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 LimitTABLE 1 Method Detection Limit and Reporting Range^A

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

TABLE 2 Concentrations of Calibration Standards (ng/L)

Analyte/Surrogate

LV1

LV2

LV3

LV4

LV5

LV6

LV7

LV8

LV9

PFPeA, PFBA

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

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

EPA SW-846	Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
40 CFR Part 136 Appendix B	Definition and Procedure for the Determination of the Method Detection Limit
D653-22	Standard Terminology Relating to Soil, Rock, and Contained Fluids
D5847-22	Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
D1193-06(2018)	Standard Specification for Reagent Water
E2554-18e1	Standard Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques (Includes all amendments and changes 10/7/2019).
D3856-11	Standard Guide for Management Systems in Laboratories Engaged in Analysis of Water
D3740-23	Standard Practice for Minimum Requirements for Agencies Engaged in Testing and/or Inspection of Soil and Rock as Used in Engineering Design and Construction
D3694-96(2017)	Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
D2777-21	Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D5681-23	Standard Terminology for Waste and Waste Management

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