【国外标准】 Standard Test Method for Analysis of Target Phenols (TPs) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS)

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)  5.3 The RL for a specific soil sample may differ from that listed depending on the nature of the interferences in the sample matrix. Variability in historical LCS spike recovery may be used to estimate uncertainty. The estimate of minimum laboratory contribution to measurement uncertainty of this test method for each analyte is listed in Table 3. These values are derived from P&A samples from the initial IDOC study for this test method. The uncertainty will be greater near the RL and much greater near the DL. Also, uncertainty estimated based on variability in LCS recovery is conservative because some sources of variability are not included, such as subsample variability and matrix analyte recovery. This SOP covers multiple soil matrices and the uncertainty among the various matrices is variable. 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.