微波消解ICP-OES法测定土壤样品中22种元素

Determination of 22 elements in soil by ICP-OES with microwave digestion

采用微波消解辅助混酸(盐酸-硝酸-氢氟酸-高氯酸),讨论了加入草酸、柠檬酸、酒石酸、EDTA二钠盐等络合剂对土壤样品进行前处理的影响,根据加标回收实验和国家标准物质(GSS-1)验证实验,采用电感耦合等离子体发射光谱法(ICP-OES)同时分析土壤样品中的22种元素。结果表明:加入4 mL 10%的酒石酸络合剂的效果最好,22种元素测定结果的相对标准偏差在0.06%~4.0%范围内;检出限为0.024~0.846μg/mL;回收率良好。该方法可用于土壤样品前处理技术及土壤中元素含量测定。

Microwave digestion with mixed acid HNO3/HF/HCl04/HCl method was adopted for the determination of soil samples. The effects of addition of oxalic acid, citric acid, tartaric acid and EDTA disodium salt on the pretreatment of soil samples were discussed. The recoveries of standard addition of each element and the certified values of the national soil standard （ GSS-1 ） verified the method. The 22 elements in soil samples were determined by inductively coupled plasma optical emission spectrometry. Results showed that adding 4 mL of 10% tartaric acid complexing agent was the best. The method had good precision and high accuracy under the best conditions. The relative standard deviations（ RSDs, n = 10） for the samples were in the range of 0. 06% -4.02% , the limits of detection for these elements ranged between 0. 024 and 0. 846μg/mL, and the recoveries for the elements were good. This method was simple, rapid, efficient, and economic. So the method has practical application in the soil sample pretreatment technology and the determination of elemental content in the soil.