电感耦合等离子体质谱法测定消落带土壤中总砷%Determination of Total Arsenic in Soil of Hydro-fluctuation Belt by ICP-MS
河南省科学院地理研究所河南省土壤与地下水污染预警及修复工程技术研究中心,河南 郑州 450052 中国市政工程华北设计研究总院有限公司,天津 300070 河南省科学院地理研究所河南省遥感与地理信息系统重点实验室,河南 郑州 450052
2025-11-11
消落带 土壤 总砷 电感耦合等离子体质谱法
[目的]建立一种基于电感耦合等离子体质谱法(ICP-MS)测定水库消落带土壤中总砷的分析方法.[方法]通过改变土壤样品前处理消解方式,确定了添加(1+1)王水消解液并置于沸水浴消解2h的土壤样品前处理方法,电感耦合等离子体质谱法以Rh为内标液消除仪器基体干扰,选择He气碰撞模式消除仪器质谱干扰,并在仪器最佳工作条件下测定消落带土壤样品中总砷.[结果]在 0~20 μg/L线性范围内,砷元素的相关系数(R2)为0.999 9,线性关系良好;方法检出限为0.024 mg/kg,定量限为0.096 mg/kg;通过对土壤成分标准物质GBW07426、GBW07448 和GBW07455 进行方法学验证,标准土样测定结果均在标准值范围内,加标回收率为 95.0%~102.8%,方法准确度高;RSD为2.0%~3.8%(n=6),方法精密度较高,满足实验室分析要求.[结论]该方法操作简单、成本低、检测结果准确度和精密度较高,适用于实验室大批量土壤样品中痕量砷的快速检测.%[Objective]To establish an analytical method based on inductively coupled plasma mass spectrometry(ICP-MS)for the determi-nation of total arsenic in soil of hydro-fluctuation belt.[Method]By changing the soil sample pretreatment digestion method,it was determined that adding(1+1)aqua regia digestion solution and placing it in a boiling water bath for 2 h was an effective soil sample pretreatment method.ICP-MS used Rh as internal standard solution to eliminate the interference of instrument matrix,and selected He gas collision mode to elimi-nate the interference of instrument mass spectrometry,and determined the total arsenic in soil samples in the water-level fluctuation zone under the best working conditions of the instrument.[Result]In the linear range of 0-20 μg/L,the correlation coefficient R2 of arsenic was 0.999 9,and the linear relationship is good.The detection limit of the method was 0.024 mg/kg,and the limit of quantitaion was 0.096 mg/kg;through the methodological verification of soil composition standard materials GBW07426,GBW07448,and GBW07455,the determination results of standard soil samples were all within the standard value range,the method has high accuracy with spiked recovery rates ranging from 95%to 102.8%;the RSD was 2.0%-3.8%(n=6).The method has high precision and meets the requirements of laboratory analysis.[Conclusion]This method is simple in operation,low in cost and high in accuracy and precision.It is suitable for the rapid detection of trace arsenic in a large number of soil samples in the laboratory.
