作者：邢书才, 杨永, 岳亚萍

作者单位：国家环境保护污染物计量和标准样品研究重点实验室 环境保护部标准样品研究所, 北京 100029

关键词：硼;姜黄素;分光光度法;测定条件

摘要：

针对姜黄素光度法测定水中硼分析方法存在的问题，研究和优化分析测定的实验条件。采用方法研究的方式，对样品显色反应的蒸发条件进行改良，用普通烘箱替代水浴条件，对样品进行显色和蒸发处理；同时，通过对分析方法校准曲线标准点的重新设置，拓宽方法测定范围，也使校准曲线的线性以及精密度得以显著提高。补充试剂空白试验，增加测定下限处的标准点；并从分析测定质量控制角度，对校准曲线制备中，0.10~1.00 mL标准溶液过小的加入量进行改进，变为统一体积量的一致性加入，减小了分析误差的几率。研究结果表明，改良后的实验条件，分析方法的检出限为0.019 mg/L，测定下限为0.076 mg/L；测定范围为0.080~1.4 mg/L，比改进前拓宽了40%。精密度测定结果相对标准偏差小于3.0%，准确度的检验结果符合方法学的技术要求。改进后的分析方法，测定下限低，范围广，灵敏度高；适合于水和废水中硼的分析测定。

Study on the optimizing conditions for determining boron in water by curcumin spectrophotometry
XING Shucai, YANG Yong, YUE Yaping
State Environmental Protection Key Laboratory of Environmental Pollutant Metrology and Reference Materials Study, Institute for Environmental Reference Materials of Ministry of Environmental Protection, Beijing 100029, China
Abstract: Addressing the existing problems in the determination of boron in water by curcumin spectrophotometry, the experimental conditions of assay determination were studied and optimized. Using method research, the evaporation condition of the color reaction of the sample was improved. The water bath condition was replaced by a common oven, and the sample was subjected to color development and evaporation. At the same time, the method was further adjusted by re-setting the standard point of calibration curve of the assay to expand the measurement range, as well as significantly increase the linearity and precision of the calibration curve. The reagent blank test was added to increase the standard point at the lower limit of the measurement. From the perspective of quality control of assay determination, the addition amount of the 0.10-1.00 mL standard solution was improved in the calibration curve preparation, from an amount too small to a uniform amount at one time, avoiding and reducing the chance of assay errors. The results showed that the detection limit of the improved experimental conditions was 0.019 mg/L, the lower limit of measurement 0.076 mg/L, and the measurement range 0.080-1.4 mg/L, which was 40% wider than that before the improvement. The relative standard deviation of the precision measurement results was less than 3.0%, and the accuracy test results were in accordance with the technical requirements of the methodology. The improved assay method with a lower limit of measurement, wide measurement range, and High sensitivity, is suitable for the assay determination of boron in water and wastewater.
Keywords: boron;curcumin;spectrophotometry;determination condition
2019, 45(6):65-69  收稿日期: 2019-01-22;收到修改稿日期: 2019-03-05
基金项目: 生态环境部国家标准制修订项目（2018-16）
作者简介: 邢书才(1958-),男,北京市人,教授级高级工程师,主要从事环境监测和国家标准的研究
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