李珊珊 刘国庆 赵鹏 徐晓妮

摘 要：传统方法测定汞含量时，荧光光谱仪的设定炉温较高、延迟时间较长，影响了测定结果的精密度和准确度。为此，提出建筑用胶粘剂中汞含量测定方法。干燥研磨胶粘剂，放入消解罐中，析出胶粘剂中的汞元素，使其溶解在H2O2和HNO3消解液中，使用减压蒸馏装置进行蒸馏，得到汞含量测定液，设置光谱仪器的测定参数和性能指标，上机测试汞标准使用溶液和测定液，绘制标准工作曲线，记录仪器读数和测定液荧光强度，计算胶粘剂汞含量。进行对比实验，结果表明，设计方法降低了汞含量检出率，扩大了汞含量的浓度测定范围，同时降低了测定值的相对标准偏差，提高了汞离子回收率，表明其精密度和准确度都要优于传统方法，测定结果更加可靠。

关键词：胶粘剂;汞含量;测定液;原子光谱;标准溶液

中图分类号：TQ436.1 文献标识码：A 文章编号：1001-5922（2021）04-0020-05

Abstract：When the mercury content is determined by traditional method， the setting furnace temperature of fluorescence spectrometer is higher and the delay time is longer， which affects the precision and accuracy of the determination results. Therefore， the determination method of mercury content in building adhesives is proposed. Dry and grind the adhesive， put it into the digestion tank， separate out the mercury element in the adhesive， make it dissolve in the H2O2 and HNO3 digestion solution， use the vacuum distillation device to distill， get the mercury content determination solution， set the measurement parameters and performance indicators of the spectrometer， test the mercury standard solution and measuring liquid on the computer， draw the standard working curve， record the instrument reading and the fluorescence intensity of the measuring liquid， and the mercury content of adhesive was calculated. A comparative experiment is carried out， and the results show that the design method reduces the detection rate of mercury content， expands the determination range of mercury content， reduces the relative standard deviation of the measured value， and improves the recovery rate of mercury ion. It shows that the precision and accuracy of the design method are better than those of the traditional method， and the determination results are more reliable.

Key words：adhesive; mercury content; determination solution; atomic spectrum; standard solution

0 引言

汞元素具有生物蓄積性和不可降解性，会阻碍细胞的正常代谢，影响免疫功能、心血管系统、神经系统等，对人体造成不可逆的损伤，而建筑用胶粘剂则通常用于制作家具，是人体能够直接接触的物品，因此对胶粘剂中的汞含量进行测定，避免重金属危害身体健康，具有重要意义[1]。文献[2]提出光谱法的测定方式，对延迟时间、载气流量和负高压等仪器条件进行考察，配制不同浓度的硼氢化钾与氢氧化钾，将其作为测定介质，检测汞元素的原子荧光，在此基础上，选取双硫……