基于碘量法的自动滴定分析仪开发与应用

Development and Application of Auto-titration Analyzer Based on Iodometric Method

基于碘量法的检测分析原理设计在线自动滴定分析仪,选用高精度且稳定性好的进料泵,采用间接接触式视觉传感器检测技术实现滴定终点即时判断,避免传感器与物料直接接触。在溴素氧化工艺现场进行的大量对比实验表明:仪器分析结果的精度比人工化验结果平均高出30%以上。分析误差来源,发现了溴素生产的操作漏洞,即人工取样实验室化验过程中会导致过量氯气挥发,致使样品失真,解决了该行业传统操作的痛点,在提升检测频率和检测精度的同时,实现了机器代人,自动完成在线取样、添加前置试剂、滴定分析、计算结果及清洗排废等流程,整个分析过程用时7 min,相比人工化验时间大幅缩短。仪器安装在溴素生产装置氧化工艺段,可实现氧化卤水溴氯总值的在线检测,为氯气加料阀门的自动联锁控制提供基础数据。

In this paper,having iodometric method based to design an online auto-titration analyzer was implemented,which adopts high-precision and reliable feeding pump and indirect contact visual sensor to immediately determine the titration endpoints and avoid the contact between the sensor and materials.Lots of comparative experiments on bromine oxidation process show that,the accuracy of instrumental analysis is on average over 30%higher than that of manual test results.Analyzing the source of error revealed the loophole of operation in bromine production,i.e.the manual sampling may lead to excessive chlorine gas volatilization in laboratory tests and the sample distortion;the analyzer can solve traditional pain points of the industry;and while raising detection frequency and precision,the machine instead of manual operation,auto-sampling,online adding pre-reagents,titration analysis,calculation results and cleaning waste discharge process can be realized;the whole analysis process will take 7 min,and compared with the manual tests,the time can be greatly shortened.The instrument installed in the oxidation process section of bromine production unit can realize online measurement of the total value of bromine and chlorine in oxidized brine and provide basic data for automatic interlocking control of chlorine gas feeding valve.