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聚乙烯醇-碘法在线测定表面处理槽液中硼酸含量OA

Polyvinyl Alcohol-Iodine Method for Online Determination of Boric Acid in Surface Treatment Bath

中文摘要英文摘要

为实现金属表面处理槽液中常量硼酸的在线快速检测,开发了一种基于反应动力学与原位光谱分析的新型测定方法.该方法系统研究了硼酸存在下聚乙烯醇(PVA)与碘三负离子(I3-)之间的显色反应动力学过程.通过调控反应物浓度、介质组成与温度等条件,监测溶液吸收光谱随时间的变化,发现体系中固有的硫酸与钠离子对PVA-I3-显色反应具有显著促进作用,且低温条件更有利于反应进行.基于上述发现,将反应温度精确控制在20 ℃,并优化介质中硫酸浓度与静电环境,在抑制槽液背景干扰的同时,显著加快了依赖于硼酸浓度的PVA-I3-显色反应速率.该方法在反应开始后120 s即可获得可用于定量分析的响应信号,在0~9 mmol/L硼酸浓度范围内线性关系良好,检出限为0.34 mmol/L.实际样品检测的相对误差<1%,表明该方法具有良好的准确性与实用价值.进一步集成高精度注射泵、多通道阀与自动流路系统,构建了全自动在线检测装置.该装置可在45 min内完成校准与样品检测全过程,无需前处理步骤,适用于工业现场对槽液硼酸含量的实时监测与闭环控制.

A novel method based on reaction kinetics and in-situ spectroscopic analysis was developed for the online rapid detection of boric acid in metal surface treatment bath solutions.This method systematically investigated the kinetic behavior of the chromogenic reaction between polyvinyl alcohol(PVA)and triiodide ions(I3-)in the presence of boric acid.By adjusting parameters such as reactant concentration,medium composition,and temperature,and monitoring the temporal changes in the solution absorption spectrum,it was found that the inherent sulfuric acid and sodium ions in the system significantly promote the PVA-I3 chromogenic reaction,with lower temperatures being more favorable for the reaction to proceed.Based on these findings,the reaction temperature was precisely controlled at 20 ℃,and the sulfuric acid concentration and electrostatic environment in the reaction medium were optimized.This approach significantly accelerated the boric acid concentration-dependent PVA-I3-chromogenic reaction while effectively suppressing interference from background components in the bath solution.A reliable analytical signal suitable for quantification was obtained within 120 s after reaction initiation.The method demonstrated a good linear relationship within the boric acid concentration range of 0~9 mmol/L,with a detection limit of 0.34 mmol/L.The relative error of actual sample testing was less than 1%,indicating good accuracy and practical utility.Furthermore,a fully automated online detection system was built by integrating high-precision syringe pumps,multi-port valves,and an automated flow path system.This setup completed the entire calibration and sample detection process within 45 minutes without any pre-treatment steps,making it applicable for real-time monitoring and closed-loop control of boric acid concentration in industrial settings.

马艳子;何芃;唐俊榕;王亚齐;王岩;赵美萍

北京大学化学与分子工程学院化学国家级实验教学示范中心,北京 100871北京大学化学与分子工程学院化学国家级实验教学示范中心,北京 100871上海飞机制造有限公司,上海 201324上海飞机制造有限公司,上海 201324北京大学化学与分子工程学院化学国家级实验教学示范中心,北京 100871北京大学化学与分子工程学院化学国家级实验教学示范中心,北京 100871

化学化工

硼酸表面处理槽液聚乙烯醇-碘光纤光谱原位快速检测

boric acidsurface treatment bathpolyvinyl alcohol-iodineoptical fiber spectrumin-situ rapid quantitative detection

《化学试剂》 2026 (1)

58-65,8

10.13822/j.cnki.hxsj.2025.0262

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