1.1 本程序包括通过丙酮萃取、过滤、用水稀释和液相色谱/串联质谱分析测定土壤基质中的（三正丁基）-n-十四烷基氯化鏻（TTPC）。TTPC是一种对土壤有强烈吸附的杀菌剂。 2. 样品提取物在75%的溶液中制备 % 丙酮和25 % 水，因为TTPC对表面和颗粒有亲和力。该方法的报告范围为250到10 000纳克/千克。该分析物通过该方法定性和定量测定。 该方法遵循多反应监测（MRM）质谱法。 1.2 方法检测限( 注1 )（MDL）和报告范围( 注释2 )对于目标分析物，见 表1 . 注1: MDL根据联邦法规40 CFR第136部分附录B确定，作为使用土壤溶剂萃取的指南。使用两克渥太华砂样品。参考文件中解释了确定MDL的详细过程，超出了本标准的范围。 注2: 报告范围浓度根据 表2 浓度假设为50μL注射TTPC的1级校准标准液，以及最高水平的校准标准液，最终提取体积为20 mL的2-g土壤样品。数量变化将改变报告限制和范围。 1.2.1 本试验方法中的报告极限是记录为未检测数据的最小值。方法检测限和报告限之间的分析物检测是估计浓度，在本试验方法之后不报告。 根据1级校准标准的浓度计算报告限值，如所示 表2 对于TTPC，考虑2 g样品重量和20%的最终提取体积 75毫升 % 丙酮/25 % 水最终提取体积为20 因为向每个土壤样品中添加15毫升体积的丙酮，并且仅过滤提取后的液层，留下固体，然后向丙酮提取物中添加5毫升水。 1.3 单位- 以国际单位制表示的数值应视为标准值。 本标准不包括其他计量单位。 1.4 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。 1.5 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》中确立的国际公认标准化原则制定的。 ====意义和用途====== 5.1 本试验方法由美国环保局芝加哥地区实验室（CRL）开发。 5.2 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、细菌和真菌粘液。 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各种土壤基质中痕量TTPC浓度，以了解受影响土壤和沉积物中的来源和浓度水平。 5.3 该方法已用于测定沙子、商业表土和四种ASTM参考土壤中的TTPC( 表4 ).

1.1 This procedure covers the determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in a soil matrix by extraction with acetone, filtration, dilution with water, and analysis by liquid chromatography/tandem mass spectrometry. TTPC is a biocide that strongly adsorbs to soils. 2 The sample extracts 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 250 to 10 000 ng/kg. This analyte is qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry. 1.2 The method detection limit ( Note 1 ) (MDL) and reporting range ( Note 2 ) for the target analyte are listed in Table 1 . Note 1: The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B, as a guide utilizing solvent extraction of soil. Two-gram sample of Ottawa sand was utilized. A detailed process determining the MDL is explained in the reference and is beyond the scope of this standard to be explained here. Note 2: Reporting range concentration is calculated from Table 2 concentrations assuming a 50-μL injection of the Level 1 calibration standard for TTPC, and the highest level calibration standard with a 20-mL final extract volume of a 2-g soil sample. Volume variations will change the reporting limit and ranges. 1.2.1 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 2 for TTPC after taking into account a 2-g sample weight and a final extract volume of 20 mL in 75 % acetone/25 % water. The final extract volume is 20 mL because a 15-mL volume of acetone is added to each soil sample and only the liquid layer after extraction is filtered leaving the solid behind followed by the addition of 5 mL of water to the acetone extract. 1.3 Units— 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 This test method has been developed by the U.S. EPA Region 5 Chicago Regional Laboratory (CRL). 5.2 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 various soil matrices for understanding the sources and concentration levels in affected soils and sediments. 5.3 This method has been used to determine TTPC in sand, a commercial top soil, and four ASTM reference soils ( Table 4 ).