ICP-AES法同时测定铬酸钾中杂质元素  

Simultaneous Determination of Impurities in K_2CrO_4 by ICP-AES

作　　者：余志辉[1,2] 齐涛[1] 曲景奎[1] 初景龙[1] 王丽娜[1] 

机构地区：[1]中国科学院过程工程研究所绿色过程与工程重点实验室,北京100190 [2]中国科学院研究生院,北京100039

出　　处：《光谱学与光谱分析》2009年第8期2250-2253,共4页Spectroscopy and Spectral Analysis

基　　金：国家"十一五"科技支撑计划课题项目(2006BAC02A05);国家重点基础研究发展计划项目(2007CB613501);国家自然科学基金项目(20676136);中国化工集团科技基金项目(2006K02B)资助

摘　　要：应用电感耦合等离子发射光谱法(ICP-AES)同时测定K2CrO4中微量Ca,Mg,Ba,Co,Cd,Cu,Mn,Pb,Sr,Zn,Al,Fe,Ni,Ti,Si,V等杂质元素含量。通过选择合适的分析谱线,采用基体匹配法消除了样品中基体元素的干扰。结果表明,在选定的测定条件下,方法的标准曲线线性关系良好(R2=0.9986～1.000),实验测得16种元素的检出限在0.075～2.625mg·kg-1之间,两次测定的加标回收率在83.7%～113.0%之间,9次测定的RSD小于9.48%。实验表明该方法快速、简便、准确、可靠,可用于实际样品分析。通过对测定结果的分析,得出K2CrO4中含有较高含量的Ca,Mg,Al,Si,不能直接用来作为离子膜法电催化合成铬酸酐的原料,必须对K2CrO4进行进一步的精制。The trace elements, Ca, Mg, Ba, Co, Cd, Cu, Mn, Pb, Sr, Zn, Al, Fe, Ni, Ti, Si and V, in K2CrO4 were simultaneously determined by inductively coupled plasma atomic emission spectrometry （ICP-AES）. Optimum spectral lines were selected for each analyzed element. The matrix effect was studied and eliminated through matrix matching. The results show that the linear correlations of standard curves are good （R2 = 0. 998 6-1. 000） under the determined conditions. The recoveries of standard addition are in the range of 83. 7%-113.0%, and the relative standard deviations are lower than 9. 48%（n=9）. Detection limits of these impurities are in the range of 0. 075-2. 625 mg . kg^-2. The method is rapid, simple, accurate and credible, so it can be used for the determination of impurities in K2CrO4 product. The results also show that there is relatively high content of Ca, Mg, Al and Si in K2CrO4 product, so the K2CrO4 product can＇t be directly used for the ion membrane electrochemical synthesis of chromic anhydride and the product must be taken for further purification.

关 键 词：K2CrO4 基体匹配 微量元素 电感耦合等离子发射光谱法 

分 类 号：O657.3[理学—分析化学]