电感耦合等离子体原子发射光谱法测定光致发光材料钼酸钙中19种微量杂质元素

准确、快速地测定光致发光材料钼酸钙中钨、钒、铜、锰、镍、铁、锡、锑、镁、镉、铝、铅、铋、铬、砷、钛、钴、钡、硅等19种微量杂质元素,对光致发光材料钼酸钙的质量判定有重要意义。选择过氧化氢-盐酸溶解体系对样品进行前处理;采用钼基体匹配法消除基体效应对测定的影响;通过选择合适的谱线消除光谱干扰;使用电感耦合等离子体原子发射光谱法(ICP-AES)测定光致发光材料钼酸钙中上述19种微量杂质元素。方法中各待测元素校准曲线的线性相关系数均大于0.999 0;方法中各元素检出限为0.2~4.4 μg/g。按照实验方法测定光致发光材料钼酸钙中钨、钒、铜、锰、镍、铁、锡、锑、镁、镉、铝、铅、铋、铬、砷、钛、钴、钡、硅,结果的相对标准偏差(RSD,n=8)为0.61%～6.8%;加标回收率为95%～105%。按照实验方法测定实验室内控样品,测定结果与电感耦合等离子体质谱法(ICP-MS)测定结果一致。

Determination of nineteen trace impurities in photoluminescent material of calcium molybdate by inductively coupled plasmaatomic emission spectrometry

The accurate and rapid determination of 19 trace impurity elements in photoluminescent calcium molybdate, including tungsten, vanadium, copper, manganese, nickel, iron, silicon, tin, antimony, magnesium, cadmium, aluminum, lead, bismuth, chromium, arsenic, titanium, cobalt and barium, is of great significance for the quality determination of photoluminescent calcium molybdate. Hydrogen peroxide-hydrochloric acid system was selected for the pretreatment of samples. The influence of matrix effect on the determination was eliminated by the molybdenum matrix matching method. Appropriate analytical lines were selected to eliminate the spectral interference. The contents of 19 trace impurity elements in photoluminescent calcium molybdate were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The correlation coefficients of calibration curves of testing elements were all greater than 0.999 0. The limits of detection of testing elements were in range of 0.2-4.4 μg/g.The contents of tungsten, vanadium, copper, manganese, nickel, iron, silicon, tin, antimony, magnesium, cadmium, aluminum, lead, bismuth, chromium, arsenic, titanium, cobalt and barium in photoluminescent calcium molybdate were determined according to the experimental method. The relative standard deviations (RSD, n=8) of determination results were between 0.61% and 6.8%. The spiked recoveries were between 95% and 105%. The internal control samples in laboratory were determined according to the experimental method, and the found results were consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS).