碱液提取-树脂除盐结合电感耦合等离子体发射光谱法测定土壤中Cr(Ⅵ)  

Determination of Cr(Ⅵ) in Soil by Lye Extraction-Resin Desalination Combined with ICP-OES

作　　者：石勇丽 夏辉 曹宁宁 李佳昊 李和平 石晓丽 张凯 SHI Yongli;XIA Hui;CAO Ningning;LI Jiahao;LI Heping;SHI Xiaoli;ZHANG Kai(Henan Provincial Coal Geological Survey and Research Institute,Zhengzhou 450052;Key Laboratory of Regional Environment and Eco-restoration(Shenyang University),Ministry of Education,Shenyang 110044)

机构地区：[1]河南省煤炭地质勘察研究总院,河南郑州450052 [2]沈阳大学区域污染环境生态修复教育部重点实验室,辽宁沈阳110044

出　　处：《分析科学学报》2021年第6期771-776,共6页Journal of Analytical Science

基　　金：河南省科技攻关项目(No.212102310081)。

摘　　要：本文对环境标准(HJ 1082-2019)中土壤Cr(Ⅵ)测定方法存在高盐基体干扰和结果不稳定等问题进行了改进,建立了碱液提取-树脂除盐,结合电感耦合等离子体发射光谱法(ICP-OES)测定土壤中Cr(Ⅵ)。利用阳离子交换和稀释法降低高盐的负面效应,当树脂投放量为3 g,振荡频率为200 r/min,阳离子交换时间为30 min时,能够去除体系90%以上盐分。采用灵敏度高、成本低、线性范围宽的ICP-OES测试技术,提高了方法适用性。方法学研究显示,改进后的方法的检出限为0.04 mg/kg,检出下限为0.16 mg/kg,优于标准方法。将此方法应用于国家标准物质分析,其Cr(Ⅵ)测定结果均位于推荐值的不确定度范围之内,精密度和准确度较好,可应用于实际环境土壤样品中Cr(Ⅵ)的测定。A simple and effective method with the combination of ICP-OES and alkali extraction and resin desalination was proposed for the determination of Cr(Ⅵ) in soil,which solved the problems of high salt matrix interference and unstable results in the China Environmental Industry Standard(HJ 1082-2019) Method.On the one hand,it was clear that more than 90% salt in the system was removed at resin dosage of 3 g,oscillation frequency of 200 r/min,and time 30 min,indicating that the negative effects of high salt was reduced by the pretreatment process of cation exchange-dilution.On the other hand,ICP-OES was used to improve the applicability of the method due to its high sensitivity,low cost,and wide linear range.The limit of detection was 0.04 mg/kg,and the limit of quantification was 0.16 mg/kg,which was more sensitive than standard method(HJ 1082-2019).Furthermore,the method was applied to the analysis of national reference materials,and the determination results of Cr(Ⅵ) were all within the uncertainty range of the recommended value.The developed method has better accuracy and precision,and can be suitable for the Cr(Ⅵ) determination in actual environmental soil samples.

关 键 词：Cr(Ⅵ) 土壤 阳离子交换树脂 电感耦合等离子体发射光谱法 

分 类 号：O657.31[理学—分析化学]