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[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0.3~10.0μg/L,相关系数≥0.999 9,检出限=0.1μg/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。
[Objective] The research aimed to study the method of microwave digestion and atomic fluorescence spectrometry for the determination of bismuth in soil with hydrofluoric acid + aqua regia system. [Method] The effects of different digestion systems such as nitric acid + hydrochloric acid (3:1 in volume), aqua regia, aqua regia and aqua regia (volume ratio 1: 3), hydrofluoric acid + aqua regia The effect of pretreatment was compared with the difference between working curve and standard curve. The effects of acidic medium and reductant concentration and common interfering ions on bismuth determination by atomic fluorescence spectrometry were observed and the best analytical conditions were established. [Result] The method was suitable for the hydrofluoric acid + aqua regia system for soil digestion. The linear range of bismuth was 0.3-10.0 μg / L, the correlation coefficient was ≥0.999 9, the detection limit was 0.1 μg / L, the recovery was 94.1% ~ 109.0%, the precision of 1.36% ~ 4.93%. [Conclusion] The method was applied to the determination of bismuth in difficult to digest soil with the method of digesting the soil completely and using less reagent. The accuracy and precision of the method were both measured by standard curve method. The detection limit was low and the interference of coexisting elements was less.