碱性微波提取-ICP/MS法测定土壤中六价铬  

Determination of Hexavalent Chromium in Soil by Microwave-assisted Alkaline Digestion ICP/MS

作　　者：陈秀梅 王靖宜 CHEN Xiu-mei;WANG Jing-yi(Nantong Environmental Monitoring Center of Jiangsu Province,Nantong,Jiangsu 226000,China)

机构地区：[1]江苏省南通环境监测中心,江苏南通226000

出　　处：《环境监测管理与技术》2022年第6期56-59,共4页The Administration and Technique of Environmental Monitoring

基　　金：南通市“基于空间异质性模型的南通市土壤重金属溯源及污染源解析”科技基金资助项目(JC2021167)。

摘　　要：采用碱性微波提取法处理土壤样品,用电感耦合等离子体质谱(ICP/MS)法测定试样中的六价铬,以标准物质测定相对误差的绝对值作为试验指标建立正交模型,确定碱性微波消解的提取温度95℃、提取时间30 min、氯化镁用量0.05 g、提取液体积6 mL为最佳试验条件,采用He碰撞池技术和在线内标分别消除基体带来的质谱和非质谱干扰。条件优化后,方法检出限为0.10 mg/kg,实际样品6次测定结果的RSD分别为13.0%和5.7%,加标回收率为120%和106%。将该方法用于有证标准土壤样品的测定,测定结果均在标准值范围内。The soil was treated by microwave-assisted alkaline digestion,and Crin the samples was determined by ICP/MS.An orthogonal model was established by taking the absolute value of relative error of reference material measurements as test indexes,the optimum conditions of microwave-assisted alkaline digestion were determined as extraction temperature of 95 ℃,extraction time of 30 min,dosage of magnesium chloride of 0.05 g and extracting solution of 6 mL.He collision cell technology and on line internal standard were used to eliminate the interference of mass spectrometry and non-mass spectrometry caused by matrix respectively.Under the optimized conditions,the method detection limit was 0.10 mg/kg.The RSD of 6 measurements of actual samples were 13.0% and 5.7%,and the spiked recoveries were 120% and 106%,respectively.This method was applied to the determination of certified standard soil samples,and the results were all within the range of standard values.

关 键 词：六价铬 正交试验 碱性微波提取 ICP/MS法 土壤 

分 类 号：O657.63[理学—分析化学]