腔增强拉曼光谱法无损测定地浸溶液中的碳酸氢根和碳酸根  

Nondestructive determination of bicarbonate and carbonate ions in in-situ leaching solution by cavity-enhanced Raman spectroscopy

作　　者：陈士恒 黄蔷薇 杜志明[1] 丁海云[1] 龚明明[1] CHEN Shiheng;HUANG Qiangwei;DU Zhiming;DING Haiyun;GONG Mingming(Beijing Research Institute of Chemical Engineering Metallurgy,CNNC,Beijing 101149,China)

机构地区：[1]核工业北京化工冶金研究院,北京101101

出　　处：《化学分析计量》2023年第7期60-64,共5页Chemical Analysis And Meterage

基　　金：中核集团集中研发项目(2021144);中核集团创新青年科技创新团队项目。

摘　　要：利用腔增强型拉曼光谱仪两个抛物面反射镜和两个直角反射镜组合成多反射增强腔,实现了激光在检测池中心点的多次照射,提高了激光的使用效率及拉曼光谱效应,改善了拉曼光谱方法的灵敏度,并建立了地浸溶液中无损、免试剂、快速、同时测定HCO_(3)^(-)、CO_(3)^(2-)含量的方法,该方法对HCO_(3)^(-)、CO_(3)^(2-)的检出限分别为30、17 mg/L;HCO_(3)^(-)、CO_(3)^(2-)的线性范围分别为50~5000、28.3~2830 mg/L,相关系数分别为0.9999、0.9997。对HCO_(3)^(-)测量结果的相对标准偏差不大于1.8%(n=6),分析时长小于4 min。腔增强拉曼光谱法检测碳酸氢根和碳酸根加标样品时具有更好的准确性,其相对误差绝对值不大于3%,而常规滴定法则大于8%。腔增强拉曼光谱法无需配制任何试剂即可实现地浸溶液中HCO_(3)^(-)、CO_(3)^(2-)的快速检测,在CO_(2)+O_(2)原地浸出工艺中HCO_(3)^(-)、CO_(3)^(2-)的自动在线监测方面具有良好的应用前景。Two parabolic mirrors and two right angle mirrors of cavity-enhanced Raman spectrometer were combined to form a multi-reflection enhancement cavity,which was used to realize multiple laser irradiation at the central point of the detection cell,improved the efficiency of laser and Raman spectrum effect,and enhanced the sensitivity of Raman spectroscopy method.A method of non-destructive,reagent free,rapid and simultaneous determination of HCO_(3)^(-)and CO_(3)^(2-)in the in-situ leaching solution was established.The detection limits of HCO_(3)^(-)and CO_(3)^(2-)were 17 mg/L and 30 mg/L,respectively.The linear range of HCO_(3)^(-)was 50-5000 mg/L,and the linear range of CO_(3)^(2-)was 28.3-2830 mg/L.The correlation coefficient of HCO_(3)^(-)and CO_(3)^(2-)was 0.9999,0.9997,respectively.The relative standard deviations of HCO_(3)^(-)was not more than 1.8%,and the detection time was less than 4 min.The absolute value of the relative error of this method was not more than 3%,while the conventional titration method was more than 8%.Cavity-enhanced Raman spectroscopy had better accuracy in the determination of bicarbonate and carbonated in spiked samples.This method can realize the rapid detection of HCO_(3)^(-)and CO_(3)^(2-)in in-situ leaching solution without any preparation of reagents,which has a good application prospect in the automatic on-line monitoring of HCO_(3)^(-)and CO_(3)^(2-)in CO_(2)+O_(2)in-situ leaching industry.

关 键 词：腔增强 拉曼光谱 碳酸氢根 碳酸根 地浸溶液 

分 类 号：O657.2[理学—分析化学]