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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) 用共溶剂化和液相色谱-串联质谱法(LC/MS/MS)测定水基质中全氟烷基和多氟烷基物质(PFAS)的标准试验方法
发布日期: 2024-06-01
1.1 本试验方法包括使用液相色谱法(LC)和串联质谱法(MS/MS)检测水性基质中的全氟烷基和多氟烷基物质(PFAS)。这些分析物通过样品和甲醇的1+1比例进行共溶剂化,然后通过该测试方法进行定性和定量测定。定量是通过选择性反应监测(SRM)或有时称为多重反应监测(MRM)进行的。 1.2 方法检测限(MDL)(参见 注1 )和报告范围(请参阅 注2 )在表1中列出了目标分析物的。该试验方法报告限值的目标浓度是一个整数值,该整数值是根据制备样品最终体积的最低标准浓度计算得出的。该值可能低于计算的MDL,因为在样品采集和制备过程中使用的耗材/采集工具中的PFAS污染导致了偶发的PFAS撞击。 为了比较两个制备的样品之间的精度,所有样品应至少作为副本进行采集,以帮助确保浓度/阳性结果是可靠的。 注1: MDL是根据《联邦法规》(CFR),40 CFR第136部分,附录B,利用稀释和过滤确定的。参考文献中解释了确定MDL的详细过程,该过程超出了本测试方法的范围。 注2: 所用仪器的注射量变化和灵敏度将改变报告限值和范围。 1.2.1 认识到仪器灵敏度的不断进步、柱色谱法的进步和其他未被认可的过程,假设在较低浓度下满足该测试方法的最低性能要求,则报告限值可能会降低。 1.2.2 根据数据使用情况,您可以修改此测试方法,但仅限于在满足或超过方法质量验收标准的情况下提高性能的修改。 不允许仅仅为了节省时间而修改溶剂、溶剂与样品的比例或缩短色谱运行时间。使用练习 E2935 或类似的统计测试,以确认修改在非干扰样本上产生等效结果。此外,请使用指南 E2857 或等效统计数据,以重新验证修改后的测试。 1.2.3 在方法检测极限和报告极限之间的分析物检测是估计的浓度。报告限值基于1级校准标准的浓度,如表5所示。 1.3 以国际单位制表示的数值应视为标准。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 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。PFAS已在土壤、污泥、地表水和饮用水中检测到。这是一种快速、简单、可靠的方法,可以定量测定水基质中微量化合物的含量。 5.2 该试验方法已通过使用试剂水和来自现场的水进行验证,包括选定PFAS的垃圾渗滤液、金属修整器、POTW污水、医院、POTW进水、公共汽车清洗站、发电厂以及纸浆厂和造纸厂污水,请参阅精度和偏差(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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