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Standard Test Method for Determination of Polyfluorinated Compounds in Soil by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) 用液相色谱-串联质谱法(LC/MS/MS)测定土壤中多氟化合物的标准试验方法
发布日期: 2023-11-01
1.1 本程序包括使用溶剂萃取、过滤、液相色谱法(LC)和串联质谱法(MS/MS)检测土壤基质中选定的多氟烷基物质(PFAS)。这些分析物可通过该方法进行定性和定量测定。该方法坚持多重反应监测(MRM)质谱法。该程序采用快速提取,并不旨在对难处理土壤基质中PFAS的含量进行详尽的统计。Washington等人发表的PFAS的详尽提取程序。, 2. 对于困难的矩阵,在分析PFAS时应考虑。本标准中的方法用于筛选实验室涂层(纺织品),以确定PFAS是否会从材料中浸出。 1.2 单位-- 以国际单位制表示的数值应视为标准。本标准中不包括其他计量单位。 1.3 检测限的方法 3. 和报告范围 4. 中列出了目标分析物 表1 。 1.3.1 本测试方法中的报告限值是记录为未检测数据的最小值。方法检测限值和报告限值之间的分析物检测值为估计浓度,不按照本试验方法报告。在大多数情况下,报告限值是根据1级校准标准的浓度计算得出的,如 表2 对于PFAS,在考虑了2 g样品重量,最终提取物体积为10mL,50 % 水/50 % MeOH与0.1 % 乙酸。假设最终提取体积为10 mL,因为50中有10 mL % 水/50 % MeOH与0.1 % 将乙酸添加到每个土壤样品中,并且仅过滤提取后的液体层,留下固体和任何残留溶剂。它被提高到全氟辛烷磺酸、全氟氯化氢、FHEA和FOEA的1级校准浓度以上; 这些化合物可以在1级浓度下鉴定,但在该较低尖峰水平下重复的标准偏差导致较高的报告限。 1.4 本标准并非旨在解决与其使用相关的所有安全问题(如有)。本标准的使用者有责任在使用前制定适当的安全、健康和环境实践,并确定监管限制的适用性。 1.5 本国际标准是根据世界贸易组织技术性贸易壁垒委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认的标准化原则制定的。 ===意义和用途====== 5.1 该测试方法由美国环保局芝加哥地区实验室(CRL)开发。 5.2 PFAS广泛应用于各种工业和商业产品中; 它们具有持久性、生物累积性,在环境中普遍存在。据报道,PFAS表现出发育毒性、肝毒性、免疫毒性和激素紊乱。可从美国卫生与公众服务部获得全氟烷基的毒理学简介草案。 7. PFAS已在土壤、污泥、地表水和饮用水中检测到。因此,需要一种快速、简单、可靠的方法来测定各种土壤基质中微量的这些化合物,以了解暴露的来源和途径。 5.3 该方法已用于测定沙子中选定的PFAS( 表4 )和四种ASTM参考土壤( 表5 )。
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 limit 3 and reporting range 4 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. ====== 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 ).
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