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Standard Test Method for Determination of Per- and Polyfluoroalkyl Substances (PFAS) in Aqueous Matrices by Co-solvation followed by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) 液相色谱-串联质谱法(LC/MS/MS)后用共溶剂化法测定水基质中全氟和多氟烷基物质(PFA)的标准试验方法
发布日期: 2025-01-01
1.1 本检测方法涵盖了使用液相色谱(LC)和串联质谱(MS/MS)检测水性基质中的全氟烷基物质和多氟烷基物质(PFASs)的测定。这些分析物通过1+1比例的样品和甲醇共溶剂化,然后通过该测试方法定性和定量测定。定量是通过选择反应监测(SRM)或有时称为多重反应监测(MRM)。 1.2 方法检测限(MDL)(见 附注1 )和报告范围(见 附注2 )的目标分析物列于表1中。该检测方法报告限度的目标浓度是根据制备样品最终体积的最低标准品浓度计算的整数值。由于样品采集和制备过程中使用的耗材/采集工具中的PFAS污染导致的零星PFAS命中,该值可能低于计算的MDL。所有样品应至少一式两份,以便比较两份制备样品之间的精密度,以帮助确保浓度/阳性结果可靠。 附注1: 根据联邦法规(CFR),40 CFR Part 136,附录B,利用稀释和过滤测定MDL。测定MDL的详细过程在参考文献中进行了解释,超出了本试验方法的范围。 附注2: 进样量变化和所用仪器的灵敏度将改变报告限度和范围。 1.2.1 认识到仪器灵敏度的持续进步、柱层析和此处未认识到的其他工艺的进步,假设满足该检测方法在较低浓度下的最低性能要求,报告限可能会降低。1.2.2 根据数据使用情况,您可以修改该测试方法,但仅限于在满足或超过方法质量验收标准的同时提高性能的修改。不允许仅仅为了节省时间而改变溶剂、溶剂与样品的比例或缩短色谱运行。使用实践 E2935 或类似的统计测试,以确认修改在非干扰样品上产生等效结果。另外,使用指南 E2857 或等效统计量来重新验证修改后的测试。 1.2.3 方法检测限和报告限之间的分析物检测为估计浓度。报告限度基于1级校准标准品的浓度,如表5所示。 1.3 以SI单位表示的值将被视为标准值。本标准不包括其他计量单位。 1.4 本标准并不旨在解决与其使用相关的所有安全性问题(如果有)。本标准的使用者有责任在使用前建立适当的安全、健康和环境实践并确定法规限制的适用性。 1.5 本国际标准是根据世界贸易组织技术性贸易壁垒(TBT)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 PFAS广泛用于各种工业和商业产品;它们是持久的,生物-累积的,在环境中无处不在。据报道,PFAS表现出发育毒性、肝毒性、免疫毒性和激素紊乱。在土壤、污泥、地表和饮用水中都检测到了PFAS。这是一种快速、简单且稳健的方法,可定量测定水基质中痕量水平的这些化合物。 5.2 对于选定的PFAS,使用试剂水和来自包括垃圾填埋场渗滤液、金属整理剂、POTW流出物、医院、POTW流入物、公共汽车清洗站、发电厂以及纸浆和造纸厂流出物在内的场所的水对该测试方法进行了验证,请参考精密度和偏差(第节 17 ).
1.1 This test method covers the determination of per- and polyfluoroalkyl substances (PFASs) in aqueous matrices using liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are co-solvated by a 1+1 ratio of sample and methanol then qualitatively and quantitatively determined by this test method. Quantitation is by selected reaction monitoring (SRM) or sometimes referred to as multiple reaction monitoring (MRM). 1.2 The method detection limit (MDL) (see Note 1 ) and reporting range (see Note 2 ) for the target analytes are listed in Table 1. The target concentration for the reporting limit for this test method is an integer value that is calculated from the concentration from the lowest standard from the final volume of the prepared sample. This value may be lower than the calculated MDL due to sporadic PFAS hits due to PFAS contamination in consumables/collection tools used during sample collection and preparation. All samples should be taken at a minimal as duplicates in order to compare the precision between the two prepared samples to help ensure the concentration/positive result is reliable. Note 1: The MDL is determined following the Code of Federal Regulations (CFR), 40 CFR Part 136, Appendix B utilizing dilution and filtration. A detailed process determining the MDL is explained in the reference and is beyond the scope of this test method. 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 re-validate the modified test. 1.2.3 Analyte detections between the method detection limit and the reporting limit are estimated concentrations. The reporting limit is based upon the concentration of the Level 1 calibration standard as shown in Table 5. 1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 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 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 water matrices. 5.2 This test method has been validated using reagent water and waters from sites that include landfill leachate, metal finisher, POTW Effluent, Hospital, POTW Influent, Bus washing station, Power Plant and Pulp and paper mill effluent for selected PFAS, refer to the Precision and Bias (Section 17 ).
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