ASTM D8535-23 PDF
Standard Test Method for Determination of Per- and Polyfluoroalkyl Substances (PFAS) in Soil/Biosolid Matrices by Solvent Extraction, Filtering, and Followed by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
Standard Test Method for Determination of Per- and Polyfluoroalkyl Substances (PFAS) in Soil/Biosolid Matrices by Solvent Extraction, Filtering, and Followed by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
- Статус документа:
- Действующий
- Формат:
- Электронный (PDF)
- Количество страниц:
- 34
- Дата публикации:
- 1 ноября 2023 г.
- Издание:
- D8535
- Технический комитет:
- D34 - Waste Management
SIGNIFICANCE AND USE 5.1 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. PFAS have been detected in soils, sludges, surface, and drinking waters. This is a quick, easy, and robust method to quantitatively determine these compounds at trace levels in soil/biosolid matrices. 5.2 This test method has been validated using four ASTM reference soils (CH-1, ML-1, CL-1, and SP-1). ASTM reference soil CH-1 is Fat Clay (CH)—Vicksburg Buckshot Clay; ASTM reference soil ML-1 is silt (ML)—Vicksburg silt; ASTM reference soil CL-1 is lean clay (CL)—Annapolis clay; and ASTM reference soil SP-1 is sand (SP)—Frederick sand and four biosolids (Missouri, California, Idaho, and Georgia). Refer to the Precision and Bias (Section 17). SCOPE 1.1 This test method covers the determination of per- and polyfluoroalkyl substances (PFAS) in soil/biosolid matrices by solvent extraction, filtering, separation using liquid chromatography (LC), and detection with tandem mass spectrometry (MS/MS). These analytes are extracted from soil/biosolids with basic water and methanol then qualitatively and quantitatively determined by this test method. Quantitation is by selected reaction monitoring (SRM), sometimes referred to as multiple reaction monitoring (MRM). 1.2 The reporting limit (RL) and reporting range (see Note 2) for the target analytes are listed in Table 1. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 5 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. Sporadic PFAS hits due to PFAS contamination in consumables/collection tools used during sample collection and preparation is possible while executing this standard and must be monitored. All samples should be taken at a minimum as duplicates in order to compare the precision between the two prepared samples to help ensure the concentration/positive result is reliable. Note 1: This standard only includes the determination of the analytes listed in Table 1 and is only applicable to soil and biosolid matrices; any added compost or soil additives may contain PFAS that may be bound and not able to be determined by this method. Analysis of packaging materials and polymeric PFAS moieties are not amenable to this standard. Note 2: Injection volume variations and sensitivity of the instrument used will change the reporting limit and ranges. 1.2.1 Recognizing continual advancements in the sensitivity of instrumentation, advancements in column chromatography, and other processes not recognized here, the reporting limit may be lowered assuming the minimum performance requirements of this test method at the lower concentrations are met. 1.2.2 Depending on data usage, you may modify this test method but limit to modifications that improve performance while still meeting or exceeding the method quality acceptance criteria. Modifications to the solvents, ratio of solvent to sample, or shortening the chromatographic run simply to save time are not allowed. Use Practice E2935 or similar statistical tests to confirm that modifications produce equivalent results on non-interfering samples. In addition, use Guide E2857 or equivalent statistics to revalidate the modified test. 1.2.3 Analyte detections under the reporting limit are estimated concentrations. If results are to be reported below the RL using this standard and following the method detection limit procedure in 40 CFR Part 136 Appen...
Abstract
Overview
ASTM D8535-23 is the recognized international standard for the determination of Per- and Polyfluoroalkyl Substances (PFAS) in soil and biosolid matrices. Developed by ASTM International, this robust method utilizes solvent extraction, filtration, and quantitative analysis through Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS). Given the persistent, bioaccumulative, and ubiquitous nature of PFAS in the environment, accurate and rapid detection at trace levels is vital for environmental monitoring, regulatory compliance, and scientific research.
PFAS are a class of synthetic chemicals found in a variety of industrial and consumer products, including firefighting foams, coatings, textiles, and cleaning agents. Their toxicity and environmental persistence have led to increased scrutiny and regulatory concern worldwide. ASTM D8535-23 provides laboratories and environmental professionals with a validated procedure to detect a comprehensive range of PFAS compounds in complex solid matrices.
Key Topics
- Detection of PFAS in Soils and Biosolids: The method targets both perfluoroalkyl and polyfluoroalkyl substances across various sample types.
- Solvent Extraction & Filtration: Samples undergo extraction with a water-methanol mixture, followed by filtration to isolate PFAS from solids.
- Quantitation by LC/MS/MS: Utilizes advanced tandem mass spectrometry, specifically selected reaction monitoring (SRM) or multiple reaction monitoring (MRM), to ensure sensitivity and specificity for PFAS detection.
- Precision & Validation: The method has been validated using ASTM reference soils (CH-1, ML-1, CL-1, SP-1) and biosolids from multiple US states, ensuring broad applicability and reliability.
- Reporting Limits & Quality Control: Recommends duplicate sampling to monitor precision; includes specific guidance for reporting limits, estimated concentrations below RL, and contamination control in labware and consumables.
- Modification Allowance: Flexibility to enhance method performance under conditions that meet or exceed quality criteria, with requirements for statistical validation of any changes.
Applications
ASTM D8535-23 is essential for:
- Environmental Site Assessment: Identifying and quantifying PFAS contamination in soils at manufacturing sites, landfills, military installations, and agricultural settings.
- Regulatory Compliance: Supporting efforts to meet local, national, or international regulations regarding PFAS limits in soils and biosolids.
- Wastewater and Sludge Monitoring: Providing reliable data for biosolid application programs and sludge treatment facilities.
- Remediation Projects: Informing cleanup strategies by providing accurate PFAS profiles and concentration measurements.
- Research and Development: Facilitating studies on PFAS fate, transport, and transformation in terrestrial environments.
- Public Health and Risk Assessment: Supplying critical data used in evaluating human exposure potential and ecological risks associated with PFAS in the environment.
Related Standards
Several related ASTM and regulatory standards support or complement ASTM D8535-23, including:
- ASTM D1129 – Terminology Relating to Water
- ASTM D1193 – Specification for Reagent Water
- ASTM D2777 – Practice for Determination of Precision and Bias of Applicable Test Methods
- ASTM D8272 – Guide for Developing and Optimizing Analytical Methods
- ASTM E2857 – Guide for Validating Analytical Methods
- ASTM E2935 – Practice for Evaluating Equivalence of Two Testing Processes
- EPA SW-846 – Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
- 40 CFR Part 136, Appendix B – Regulatory method detection limits
Practical Value
This standard delivers a proven methodology for the sensitive, accurate, and reproducible determination of PFAS in challenging matrices. Laboratories implementing ASTM D8535-23 benefit from reduced false positives, clear guidance on contamination control, comprehensive compound lists, and compatibility with evolving regulatory frameworks. Its adoption facilitates consistency in PFAS data reporting, essential for environmental stewardship and protection of public health.
Технические детали
- SKU
- ASTM D8535-23
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