基于微波消解的ICP-MS/ICP-OES方法测定环境土壤中总磷

Determination of Total Phosphorus in Environmental Soil by Microwave Digestion with ICP-MS and ICP-OES

基于HNO3-HF-H2O2消解体系进行微波消解后,利用ICP-MS/ICP-OES进行环境土壤中总磷测试。通过优化仪器参数及采取干扰校正措施,两台仪器校准曲线r均大于0.999,其中ICP-MS方法检出限0.05μg/g,RSD在0.67%～1.22%之间,加标回收率106%～114%;ICP-OES方法检出限在5μg/g,RSD在0.29%～0.61%之间,加标回收率105%～108%。用GSS-13和GSS-10标准样品验证,两台仪器的磷测定值与标准值吻合,微波消解ICP-MS/ICP-OES方法可以满足环境土壤中总磷分析的要求。

Based on the HNO 3 -HF-H2O2 microwave digestion system, determined total phosphorus in environmental soil by ICP-MS/ICP-OES, through optimizing instrument parameters and adopting interference correction measures, the calibration curve of both instrument were greater than 0.999, the detection limit of the ICP-MS was 0.05 μg/g and RSD was 0.67%~1.22%, the recovery rate was 106%~114%, the detection limit of the ICP-OES was 5 μg/g and RSD was 0.29%~0.61%, the recovery rate was 105%~108%. Analyzed the national standard soil samples of GSS-13 and GSS- 10, the measured value of both instrument were consistent with the standard value. The microwave digestion ICP-MS/ICP-OES method could meet the standard of the environmental soil total phos- phorus analysis.