碱溶液消解-电感耦合等离子体质谱法测定土壤中6价铬  

Determination of hexavalent chromium in soil by alkaline solution digestion-inductively coupled plasma mass spectrometry

作　　者：李小辉[1] 胡新颖 胡家祯[1] 孙慧莹[1] 袁润蕾[1] 于亚辉[1] 王曼曼 LI Xiao-hui;HU Xin-ying;HU Jia-zhen;SUN Hui-ying;YUAN Run-lei;YU Ya-hui;WANG Man-man(Precious Metals Analysis and Exploration Technology Key Laboratory of Ministry of Land and Resources,Henan Provincial Rock&Mineral Testing Centre,Zhengzhou 450012,China;Suzhou Gusu District Education Science Research Center,Suzhou 215000,China)

机构地区：[1]河南省岩石矿物测试中心自然资源部贵金属分析与勘查技术重点实验室,河南郑州450012 [2]苏州市姑苏区教育科学研究中心,江苏苏州215000

出　　处：《现代化工》2024年第12期240-243,共4页Modern Chemical Industry

基　　金：国家重点研发计划(2019YFC1804805);豫地矿青科创(2020)9号。

摘　　要：选择以碱溶液为消解体系,通过对氯化镁加入方式、消解温度、消解时间等样品前处理条件进行探讨确立了最佳消解条件,选用合适的内标元素及干扰扣除,建立了电感耦合等离子体质谱法快速测定土壤中6价铬的分析方法。6价铬的质量浓度在1.0 mg/L以内与对应的信号强度呈线性关系,相关系数为0.9999,方法检出限为0.11 mg/kg,测定下限为0.44 mg/kg。按照试验方法对国家标准物质中的6价铬进行测定,测定值与认定值一致,相对标准偏差RSD(n=6)为0.98%~2.81%,通过对实际样品进行加标回收试验,回收率为94%~105%。该方法具有稳定性好、准确度高,适用于土壤样品中痕量6价铬的分析。Taking alkaline solution digestion as the pre-treatment method,the optimal digestion conditions are determined through exploring the sample pre-treatment conditions such as magnesium chloride addition way,digestion temperature,and digestion time.The appropriate internal standard elements and interference deductions are selected out,and an analytical method is established for rapid determination of hexavalent chromium in soil by inductively coupled plasma mass spectrometry.The mass concentration of hexavalent chromium is linearly related to the corresponding signal intensity within 1.0 mg·L^(-1),with a correlation coefficient of 0.9999.The detection limit of the method is 0.11 mg·kg^(-1),and the lower limit of the determination is 0.44 mg·kg^(-1).According to the experimental method,hexavalent chromium in China's national standard substances is determined,and the measured value is consistent with the recognized value.The relative standard deviation(n=6)is 0.98%-2.81%.By conducting spiked recovery experiments on actual samples,the spiked recovery rate ranges from 94%to 105%.The established determination method has good stability and high accuracy,suitable for the analysis of trace hexavalent chromium in soil samples.

关 键 词：碱溶液消解 电感耦合等离子体质谱法 土壤 6价铬 

分 类 号：O657[理学—分析化学]