TCEC2182019磷酸酯抗燃油中活性氯含量的测定自动电位滴定法

ICS27.100F20备案号：53939-2016准T/CEC218—2019磷酸酯抗燃油中活性氯含量的测定自动电位滴定法Automaticpotentiometrictitrationtestingmethodforactivechlorinecontentinthephosphateesterfire-resistantfluids2019-04-24发布2019-07-01实施中国电力企业联合会发布成品：210*297版心：166*238字数：45*43行天35地24订24切20T/CEC218—2019中国电力企业联合会标准磷酸酯抗燃油中活性氯含量的测定自动电位滴定法T/CEC218—2019*中国电力出版社出版、发行（北京市东城区北京站西街19号100005）北京传奇佳彩印刷有限公司印刷*2019年9月第一版2019年8月北京第一次印刷880毫米×1230毫米16开本0.5印张10千字*统一书号155198·1557定价15.00元版权专有侵权必究本书如有印装质量问题，我社营销中心负责退换20mm20mm10mm20mm5mm25mmT/CEC218—2019I目次前言···································································································································································II1范围······························································································································································12规范性引用文件··········································································································································13术语和定义··················································································································································14方法原理······················································································································································15试剂和材料··················································································································································16仪器与设备··················································································································································17试验步骤······················································································································································28精密度··························································································································································29报告······························································································································································3T/CEC218—2019II前言本标准按照GB/T1.1—2009《标准化工作导则第1部分：标准的结构和编写》给出的规则起草。请注意本文件的某些内容可能涉及专利。本文件的发布机构不承担识别这些专利的责任。本标准由中国电力企业联合会提出。本标准由电气化学标准化技术委员会归口。本标准主要起草单位：国网浙江省电力公司电力科学研究院、广东电网有限责任公司电力科学研究院、国网江苏省电力公司电力科学研究院、国网安徽省电力公司电力科学研究院、国网湖南省电力公司电力科学研究院、国网山东省电力公司电力科学研究院、江苏新高科分析仪器有限公司。本部分主要起草人：明菊兰、钱洲亥、祝郦伟、钱艺华、余璐静、沈晓明、曹求洋、洪灿飞、徐恒昌、李治国、朱洪斌、祁炯、万涛、吴俊杰、于乃海、张珉新、刘子恩。本标准为首次发布。本标准在执行过程中的意见或建议反馈至中国电力企业联合会标准化中心（北京市白广路二条一号，100761）。T/CEC218—20191磷酸酯抗燃油中活性氯含量的测定自动电位滴定法1范围本标准规定了磷酸酯抗燃油中活性氯含量的电位滴定测定方法原理、试剂材料、仪器设备、试验步骤、精密度。本标准适用于磷酸酯抗燃油中活性氯含量的测定，其检出限为1.00mg/kg，其他油品和有机液体的活性氯含量的测定可参照本标准进行。2规范性引用文件下列文件对于本文件的应用是必不可少的。凡是注日期的引用文件，仅注日期的版本适用于本文件。凡是不注日期的引用文件，其最新版本（包括所有的修改单）适用于本文件。GB/T601化学试剂标准滴定溶液的制备GB/T6682分析实验室用水规格和试验方法3术语和定义下列术语和定义适用于本文件。3.1活性氯activechlorine磷酸酯抗燃油中无机及试验条件下已水解的有机氯化物的总称。4方法原理将一定质量的磷酸酯抗燃油样品置于醋酸溶液中，以硝酸银为滴定剂，银电极为指示电极滴定，根据滴定终点计算磷酸酯抗燃油中的活性氯含量。5试剂和材料5.1硝酸银（AgNO3）溶液：浓度0.01mol/L，依据GB/T601规定制备。5.2氯化钠（NaCl）溶液：浓度0.01mol/L，依据GB/T601规定制备。5.3试剂水：应符合GB/T6682规定的三级试剂水要求。5.4乙酸（CH3COOH）溶液：25%，将1体积分析纯乙酸和3体积试剂水均匀混合配制。5.5平底短颈烧瓶：100mL，磨口24/29。5.6移液管（或移液器）：1mL～5mL。6仪器与设备6.1自动电位滴定仪应满足以下条件：a）电位测量分辨率：0.1mV；b）电位测量范围：±2000mV；c）最小进给量：0.002mL；d）加液误差：不超过±0.3%；e）电磁搅拌功能：搅拌强度可调。T/CEC218—201926.2电极：复合银电极或者银离子选择性电极-银/氯化银参比电极组成。6.3电子天平：感量0.1mg。7试验步骤7.1仪器准备按照仪器的说明书调整仪器，待仪器性能稳定后使用。7.2空白滴定7.2.1用移液管（或移液器）（见5.6）移取2.00mL氯化钠标准溶液（见5.2）于平底短颈烧瓶（见5.5）中，加乙酸溶液（见5.4）80mL，搅拌120s，然后启动滴定程序，记录滴定终点的体积V0。7.2.2重复步骤7.2.1。7.2.3计算滴定终点体积的平均值0V。7.3样品滴定7.3.1用电子天平（见6.3）称取20g（精确至0.1mg）磷酸酯抗燃油样品于平底短颈烧瓶（见5.5）中，用移液管（或移液器）（见5.6）移取2.00mL氯化钠标准溶液（见5.2），加乙酸溶液80mL，搅拌120s，然后启动滴定程序，记录滴定终点的体积V1，依据式（1）计算磷酸酯抗燃油的活性氯含量。310AgNO3()35.45310VVCCm－××＝×（1）式中：V1——样品的滴定体积，mL；0V——空白的滴定体积平均值，mL；C——样品的无机氯含量，mg/kg；3AgNOC——滴定剂硝酸银浓度，mol/L；m——样品质量，g；35.453——氯的原子量。7.3.2重复步骤7.3.1。7.3.3计算抗燃油的活性氯含量的平均值。8精密度8.1重复性重复性标准差：Sr＝1.9mg/kg。8.2再现性再现性标准差为SR＝0.054C＋1.975式中：SR——再现性方差，mg/kg；T/CEC218—20193C——活性氯检测结果的平均值，mg/kg。9报告取连续两次满足重复性要求的测试结果的算术平均值作为报告值。