ASTM D7968-23 PDF
Standard Test Method for Determination of Polyfluorinated Compounds in Soil by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
Standard Test Method for Determination of Polyfluorinated Compounds in Soil by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
- Статус документа:
- Действующий
- Формат:
- Электронный (PDF)
- Количество страниц:
- 24
- Дата публикации:
- 1 ноября 2023 г.
- Издание:
- D7968
- ICS:
- 13.080.10
SIGNIFICANCE AND USE 5.1 This test method has been developed by the U.S. EPA Region 5 Chicago Regional Laboratory (CRL). 5.2 PFAS are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFAS 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 PFAS 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 PFAS in sand (Table 4) and four ASTM reference soils (Table 5). SCOPE 1.1 This procedure covers the determination of selected polyfluorinated alkyl substances (PFAS) 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 PFAS in difficult soil matrices. An exhaustive extraction procedure for PFAS, such as published by Washington et al.,2 for difficult matrices should be considered when analyzing PFAS. The approach from this standard was utilized to screen laboratory coats (textiles) to identify if PFAS would be leached from the materials. 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. 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 PFAS 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.
Abstract
Overview
ASTM D7968-23 is the internationally recognized standard test method for the determination of polyfluorinated compounds, also known as per- and polyfluoroalkyl substances (PFAS), in soil. Developed by ASTM International under the jurisdiction of Committee D34 on Waste Management, this standard outlines procedures for qualitative and quantitative analysis of selected PFAS using solvent extraction and liquid chromatography tandem mass spectrometry (LC/MS/MS), with multiple reaction monitoring (MRM).
PFAS are synthetic chemicals commonly used in industrial and commercial products due to their resistance to heat, water, and oil. However, their persistence, bioaccumulation, and mobility in the environment have raised significant health and environmental concerns. Detecting and quantifying PFAS at trace levels in soil is necessary for risk assessment, remediation, and regulatory compliance.
Key Topics
-
Purpose and Scope
- Provides a quick, robust, and sensitive method to detect trace-level PFAS in various soil matrices.
- Utilizes solvent extraction, filtration, and LC/MS/MS for comprehensive PFAS analysis.
-
Analyte Coverage
- Focuses on a targeted suite of perfluorinated carboxylic acids, sulfonates, and fluorotelomer acids (see Table 1 of the standard for details).
- Method detection limits and reporting ranges are specified for each compound.
-
Performance-Based Methodology
- Allows use of alternative instrumentation or procedures if data quality objectives are achieved.
- Adheres to stringent quality assurance and calibration requirements to ensure data reliability.
-
Sampling and Quality Control
- Emphasizes contamination avoidance by using PFAS-free sample containers and equipment.
- Involves routine use of field blanks, surrogates, and matrix spike samples.
-
Trace Analysis
- Specifically suitable for low-level detection of PFAS in soil and sand, providing valuable data for environmental monitoring and pathway exposure studies.
-
Health and Safety
- Stipulates laboratory safety practices, including the use of appropriate PPE and reference to Safety Data Sheets (SDS).
Applications
-
Environmental Site Assessment
- Identifying and quantifying PFAS contamination in soils at waste management facilities, industrial sites, and brownfields.
- Supports site characterization, human health risk assessment, and the development of appropriate remediation strategies.
-
Regulatory Compliance
- Meets data requirements for federal, regional (e.g., U.S. EPA), and international regulatory frameworks.
- Facilitates monitoring required under environmental protection statutes for persistent organic pollutants.
-
Research and Product Testing
- Used to screen consumer products (e.g., textiles, lab coats) for PFAS leaching potential.
- Assists in understanding the environmental fate, transport, and persistence of PFAS compounds.
-
Soil Quality Monitoring
- Enables regular environmental surveillance to track PFAS trends over time, aiding government agencies and private companies in managing long-term soil quality.
Related Standards
- ASTM D1193 - Specification for Reagent Water used in analytical testing.
- ASTM D2777 - Practice for Determination of Precision and Bias of Applicable Test Methods.
- ASTM D5847 - Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis.
- EPA SW-846 - Test Methods for Evaluating Solid Waste, Physical/Chemical Methods.
- 40 CFR Part 136 Appendix B - Procedures for determining method detection limits.
Summary
ASTM D7968-23 is a crucial analytical standard that enables accurate, sensitive, and reproducible measurement of PFAS in soils by employing LC/MS/MS technology. Its robust procedures and quality assurance requirements make it essential for laboratories, regulators, and stakeholders engaged in environmental monitoring, contamination assessment, and remediation planning related to polyfluorinated compounds. By following this standard, organizations can ensure reliable PFAS data to inform decisions and comply with evolving environmental regulations.
Keywords: ASTM D7968-23, PFAS in soil, LC/MS/MS, environmental analysis, polyfluorinated compounds, perfluoroalkyl substances, soil testing standard, PFAS contamination, environmental compliance.
Технические детали
- Технический комитет
- D34 - Waste Management
- SKU
- ASTM D7968-23
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