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采用HNO3-HF-H2SO4分解钨矿石,钼矿石,柠檬酸-KI溶液掩蔽干扰,加入硫脲-抗坏血酸溶液还原后,应用氢化物发生-原子荧光光谱法测量溶液中Sb含量。通过优化仪器测定条件和酸度,配合柠檬酸和KI的使用有效地避免了干扰。方法检出限为4 ng/g,RSD为3.9%~8.3%,回收率为90%~106%。经8家实验室对钨钼矿石标准物质样品精密度、准确度验证,精密度满足要求,且方法偏倚不显著。方法可用于钨矿石、钼矿石中Sb的测定。
HNO3-HF-H2SO4 decomposition of tungsten ore, molybdenum ore, citric acid -KI solution masking interference, adding thiourea - ascorbic acid solution reduction, the use of hydride generation - atomic fluorescence spectrometry to measure the solution of Sb. By optimizing the instrument to determine the conditions and acidity, interference with citrate and KI is effectively avoided. The detection limit was 4 ng / g, RSD was 3.9% ~ 8.3%, and the recovery was 90% ~ 106%. After 8 laboratories to tungsten and molybdenum ore standard material samples precision, accuracy verification, precision to meet the requirements, and the method of bias is not significant. The method can be used for the determination of Sb in tungsten ore and molybdenum ore.