电感耦合等离子体质谱法测定高纯二氧化碲中10种杂质元素

杂质元素含量对保证高纯二氧化碲产品的纯度具有重要的意义。采用1.0 mL硝酸-5.0 mL盐酸-3.0 mL酒石酸溶液溶解样品,以¹³³Cs为内标元素,用动能歧视碰撞池(KED)模式测定钙、铁和硒,采用标准模式测定其他元素,建立了采用电感耦合等离子体质谱法(ICP-MS)测定高纯二氧化碲中镁、铝、钙、铁、镍、铜、硒、锑、铅、铋等10种杂质元素含量的方法。方法检出限介于0.012～0.21 μg/L之间,方法定量限在0.040～0.59 μg/L之间。按照实验方法对高纯二氧化碲样品进行测定,每个样品平行测定7次,各元素测定结果的相对标准偏差在1.2%～3.4%之间,加标回收率在95%～106%之间。方法可用于纯度为99.999%二氧化碲材料的检测。

Determination of ten impurity elements in high purity tellurium dioxide by inductively coupled plasma mass spectrometry

The content of impurity elements was of great significance to guarantee the purity of high-purity tellurium dioxide products. The sample was dissolved with 1.0 mL of nitric acid-5.0 mL of hydrochloric acid-3.0 mL of tartaric acid solution. ¹³³Cs was selected as the internal standard element. The contents of calcium, iron and selenium were determined by kinetic energy discrimination (KED) collision cell mode, and the contents of other elements were determined by the standard mode. A determination method of ten impurity elements including magnesium, aluminum, calcium, iron, nickel, copper, selenium, antimony, lead and bismuth in high-purity tellurium dioxide by inductively coupled plasma mass spectrometry (ICP-MS) was established. The limits of detection of this method were between 0.012 μg/L and 0.21 μg/L. The limits of quantification were between 0.040 μg/L and 0.59 μg/L. The high-purity tellurium dioxide samples were determined according to the experimental method. Each sample was determination for seven times in parallel. The relative standard deviations of determination results were between 1.2% and 3.4%. The recoveries were between 95% and 106%. The proposed method was applicable for the determination of tellurium dioxide materials with purity of 99.999%.