氢化物发生-原子荧光光谱法测定多金属矿中的微量锗

摘要

以HNO3+HF+H2 SO4+HClO4混合酸溶解多金属矿，采用氢化物发生-原子荧光光谱法（AFS）测定多金属矿中的微量锗。实验讨论了H3PO4介质浓度和KBH4浓度等因素对分析结果的影响，确定了仪器最佳实验条件。本方法的检出限为0.024μg/g，精密度（RSD，n=12）为4.79%～5.53%，加标回收率为93.5%～107.3%，多金属矿测定结果与标准值吻合。该方法可以较好地满足多金属矿样品中锗的分析。%The germanium in polymetallic ores was dissolved by HNO3+HF+H2SO4+HClO4 and was measured by hydride generation-atomic fluorescence spectrometry (AFS).The effects of some parameters such as the H3PO4 concentration and KBH4 concentration,working parameters of the AFS instrument on the determination were studied and optimized by experiments.The allowable quantities of the interference elements were also invested. The detection limit of this method was 0.024μg/g,RSD was in the range of 4.79%to 5.53%and the recovery of standard addition was 93.5%to 107.3%.The method was validated by determination of Ge in National Standard Reference Materials and the results were in agreement with certified values.