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Standard Test Method for Analysis of Target Phenols (TPs) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS) 用多重反应监测液相色谱/质谱法(LC/MS/MS)分析土壤中目标酚(TPs)的标准试验方法
发布日期: 2020-02-01
1.1 本试验方法包括通过丙酮萃取、过滤、用水稀释和液相色谱/串联质谱分析土壤、沉积物和生物固体中的壬基酚(NP)、壬基酚单乙氧基化物(NP1EO)、壬基酚二乙氧基化物(NP2EO)、辛基酚(OP)和双酚A(BPA),统称为目标酚(TPs)。样品提取物在75%的溶液中制备 % 丙酮和25 % 水,因为TPs对表面和颗粒有亲和力,在较低浓度下更明显。试验方法的适用范围如所示 表1 . 根据此处未进行的其他性能研究,该方法可能会扩展到这些范围之外。 1.2 单位- 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。 1.3 本标准并非旨在解决与其使用相关的所有安全问题(如有)。 本标准的用户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。 1.4 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》中确立的国际公认标准化原则制定的。 ====意义和用途====== 5.1 本试验方法是基于液相色谱/质谱/质谱分析,用于分析土壤和沉积物样品中的TPs。可以使用任何类型的耦合液相色谱/质谱系统,以满足单个项目的研究目标。这些可能包括但不限于:陷阱、单四极、飞行时间、高分辨率以及此处未提及的其他。 5.2 TPs的MDL和报告范围列于 表1 . 本SOP已在渥太华砂、四种ASTM土壤类型、生物固体样品和一种商业土壤上进行了测试。P&A QC验收标准列于 表3 . 表4- 17 显示各种土壤类型中的TC和替代回收率。40 CFR第136部分附录B用作确定MDL的指南。NP2EO不符合40 CFR第136部分MDL标准;这不会影响该方法,因为SOP仅向RL报告,不是一种监管方法。使用该方法,所有现场样本结果均未报告在RL以下。RLC浓度可能低于RL,因为它们在RL处或附近出现峰值。 (A) 基于95%置信区间和双尾学生的不确定性计算 t 分配 不确定性=学生 t 值[(标准偏差)/(LCS数) 1. / 2. ]. (A) 损益值在减去MB平均值后,如果 ≥ RL。 (A) 损益值在减去MB平均值后,如果 ≥ RL。 (A)
1.1 This test method covers analysis of nonylphenol (NP), nonylphenol monoethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), octylphenol (OP), and bisphenol A (BPA), referred to collectively as target phenols (TPs), in soil, sediments, and biosolids by extraction with acetone, filtration, dilution with water, and analysis by liquid chromatography/tandem mass spectrometry. The sample extracts are prepared in a solution of 75 % acetone and 25 % water because TPs have an affinity for surfaces and particles that is more pronounced at lower concentrations. The range of applicability of the test method is shown in Table 1 . The method may be extended outside of these ranges depending on additional performance studies not undertaken here. 1.2 Units— The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard. 1.3 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. 1.4 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 developed for the analysis of TPs in soil and sediment samples is based upon an LC/MS/MS analysis. Any type of coupled liquid chromatography/mass spectrometry system may be used that meets the study objectives of the individual project. These may include, but are not limited to: trap, single quadrupoles, time-of-flight, high resolution, and others not mentioned here. 5.2 The MDL and reporting range for TPs are listed in Table 1 . This SOP has been tested on Ottawa sand, four ASTM soil types, biosolid sample, and one commercial soil. The P&A QC acceptance criteria are listed in Table 3 . Tables 4- 17 display the TC and surrogate recoveries in the various soil types. 40 CFR Part 136, Appendix B was used as a guide to determine the MDLs. The 40 CFR Part 136 MDL criteria were not met for NP2EO; this does not affect the method because the SOP only reports to the RL and is not a regulatory method. All site sample results are not reported below the RL using this method. RLCS concentrations may be reported below the RL because they are spiked at or near the RL. (A) Uncertainty calculation based upon 95 % confidence interval and a two-tailed Student t distribution. Uncertainty = Student t Value [(standard deviation) / (number of LCS) 1 / 2 ]. (A) P&A values are after subtraction of average of MB if ≥ RL. (A) P&A values are after subtraction of average of MB if ≥ RL. (A)
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