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Standard Test Method for Determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in Water by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS) 多重反应监测液相色谱/质谱法(LC/MS/MS)测定水中(三正丁基)正十四烷基氯化鏻(TTPC)的标准试验方法
发布日期: 2023-04-15
1.1 本试验方法包括通过丙酮稀释、过滤和液相色谱/串联质谱分析来测定水中的(三正丁基)-正十四烷基氯化鏻(TTPC)。本试验方法不适用于三丁基十四烷基氯化鏻异构体混合物的分析。TTPC是一种能强烈吸附在土壤中的杀生物剂。 2. 水样是在75%丙酮和25%水的溶液中制备的,因为TTPC对表面和颗粒具有亲和力。此方法的报告范围为100 ng/L至4000 纳克/升。该分析物通过该方法进行定性和定量测定。该测试方法遵循多重反应监测(MRM)质谱法。 1.2 满足实践要求的全面合作学习 777加元 尚未完成。此测试方法包含单个- 基于单个操作员数据的操作员精度和偏差。发布尚未完全验证的标准是为了让标准用户能够访问当前的技术,并征求用户社区的额外意见。 1.3 方法检测极限 3. (MDL)和报告范围 4. 对于目标分析物 表1 . 1.3.1 本测试方法中的报告限值是将数据记录为未检测的最小值。方法检测限和报告限之间的分析物检测为估计浓度,不按照本试验方法报告。报告限值是根据1级校准标准的浓度计算得出的,如 表4 在考虑了2.5 mL水样体积和10 mL(75%丙酮/25%水)的最终稀释样品体积后,用于TTPC。 最终溶液体积为10mL,因为将7.5mL体积的丙酮添加到每2.5mL水样中,该水样被摇动和过滤。 1.4 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。 1.5 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。 1.6 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 TTPC可用于各种工业和商业产品中,用作杀生物剂。含有TTPC的产品已被批准用于控制工业用水系统中的藻类、细菌和真菌泥。 2. TTPC不应在水中持久存在,但可能以令人担忧的浓度沉积在沉积物中。因此,需要一种快速、简单和稳健的方法来确定水基质中痕量TTPC的浓度,以了解受影响地区的来源和浓度水平。 5.2 该方法已用于测定试剂水中和河水中的TTPC( 表8 ). (A) 溶液A:根据第节制备的8级储备溶液 12 以及 表4 浓度。 (B) 溶液B:75%丙酮,25%水。 注1: 该测试方法已用于表征真实世界水样中的TTPC,并取得了成功,回收率类似,如 表8 .
1.1 This test method covers the determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in water by dilution with acetone, filtration and analysis by liquid chromatography/tandem mass spectrometry. This test method is not amenable for the analysis of isomeric mixtures of Tributyl-tetradecylphosphonium chloride. TTPC is a biocide that strongly adsorbs to soils. 2 The water samples are prepared in a solution of 75 % acetone and 25 % water because TTPC has an affinity for surfaces and particles. The reporting range for this method is from 100 ng/L to 4000 ng/L. This analyte is qualitatively and quantitatively determined by this method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry. 1.2 A full collaborative study to meet the requirements of Practice D2777 has not been completed. This test method contains single-operator precision and bias based on single-operator data. Publication of standards that have not been fully validated is done to make the current technology accessible to users of standards, and to solicit additional input from the user community. 1.3 The Method Detection Limit 3 (MDL) and Reporting Range 4 for the target analyte 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. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 4 for TTPC after taking into account a 2.5 mL water sample volume and a final diluted sample volume of 10 mL (75 % acetone/25 % water). The final solution volume is 10 mL because a 7.5 mL volume of acetone is added to each 2.5 mL water sample which is shaken and filtered. 1.4 Units— The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.5 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. 1.6 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 TTPC may be used in various industrial and commercial products for use as a biocide. Products containing TTPC have been approved for controlling algal, bacterial, and fungal slimes in industrial water systems. 2 TTPC should not be persistent in water but may be deposited in sediments at concentrations of concern. Hence, there is a need for quick, easy and robust method to determine TTPC concentration at trace levels in water matrices for understanding the sources and concentration levels in affected areas. 5.2 This method has been used to determine TTPC in reagent water and a river water ( Table 8 ). (A) Solution A: Level 8 stock solution prepared according to Section 12 and at Table 4 concentrations. (B) Solution B: 75 % Acetone, 25 % Water. Note 1: This test method has been used to characterize TTPC in real world water samples with success and similar recoveries as shown in Table 8 .
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