微波消解-原子荧光法测定土壤中铋
Determination of Bismuth in Soil Using Microwave Digestion by Atomic Fluorescence Spectrometry
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摘要:
目的 研究氢氟酸+王水体系微波消解和原子荧光光谱法测定土壤中铋的方法。 方法 观察硝酸+盐酸(体积比3:1)、王水、双氧水+王水(体积比1:3)、氢氟酸+王水(体积比2:1)等不同消解体系对土壤样品前处理的效果,比较工作曲线和标准曲线测得数据的差异,观察酸性介质和还原剂浓度以及常见干扰离子对原子荧光测定铋的影响,确立最佳的分析条件。 结果 适合土壤消解的氢氟酸+王水体系采用该测定方法,铋的线性范围为0.3~10.0 μg/L,相关系数 ≥ 0.999 9,检出限=0.1 μg/L,方法回收率为94.1%~109.0%,精密度为1.36%~4.93%。 结论 该方法消解土壤完全,试剂用量少,用标准曲线法测定结果准确度和精密度均高,检出限低,共存元素干扰少,适用于难消解土壤中铋的测定。 Abstract:Objective To establish a method for determination of bismuth concentration in soil using microwave digestion with hydrofluoric acid and aqua regia by atomic fluorescence spectrometry (AFS). Methods We compared the pretreatment effects of nitric acid+hydrochloric acid (3:1 v/v),aqua regia,hydrogen peroxide+aqua regia (1:3 v/v),and hydrofluoric acid+aqua regia (2:1 v/v).The differences of data derived by standard curve and working curve were compared,and the influences of acid medium,reducing agent concentration,and common interfering ions on the determination of bismuth were assessed to develop optimum experiment conditions. Results Hydrofluoric acid+aqua regia was chosen for soil digestion.The linear calibration curve for bismuth was within the range of 0.3-10.0 μg/L with correlation coefficient ≥ 0.999 9.The limit of detection was 0.1 μg/L.The recovery rate was in the range of 94.1%-109%.The relative standard deviations were 1.36%-4.93%. Conclusion In this method,the soil samples are digested completely with less reagent.The method proves to be of high accuracy and good precision with few common interfering ions,which make it effective in the determination of bismuth concentration in soilgroup
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