电感耦合等离子体原子发射光谱法测定金属锑及三氧化二锑中杂质元素

Determination of impurities in antimony and diantimony trioxide by inductively coupled plasma atomic emission spectrometry

金属锑及三氧化二锑样品经酸消解后，未经基体分离直接以高分辨率顺序扫描型电感耦合等离子体原子发射光谱仪测定其中杂质元素，发现只要控制好消解温度，铜、镉、铅、砷、铬、硒、锡、汞、铋等多种杂质元素都可以进行同时检测，简化了实验步骤。本文对样品的消解方法、溶液的酸度选择、光谱和基体干扰进行了试验，在优化仪器的工作条件下，通过基体匹配，有效地消除了基体干扰的影响。方法简便、快速，可满足工业分析要求，方法检出限均小于0．02μg／mL，回收率在96．0％～106．4％范围内，相对标准偏差〈3％（n=6），测定结果同认定值相符合。

After antimony and diantimony trioxide samples were dissolved with acid, the impurities in them were directly determined with high-resolution consecutive scanning inductively coupled plasma atomic emission spectrometer without matrix separation. It was found that if the digestion temperature could be well controlled, the simultaneous determination of many impurities including copper, cadmium, lead, arsenic, chromium, selenium, tin, mercury and bismuth could be achieved, with simplified experiment procedure. The sample digestion, selection of solution acidity, spectral and matrix interference were studied. Under the optimized working conditions, the interference of matrix could be effectively eliminated by matrix matching. Being simple and rapid, This method could meet the requirements of industrial analysis. Its recovery was between 96.0% -106.4 %. RSD was less than 3% （n= 6）, and the detection limit of method was lower than 0.02 μg/mL. The determination results were consistent with the certified values.