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用扫描式电感耦合等离子体光谱仪测定红矾钾产品中的杂质
引用本文:李玉平,张懿,齐涛,刘克玲.用扫描式电感耦合等离子体光谱仪测定红矾钾产品中的杂质[J].光谱学与光谱分析,2004,24(11):1428-1431.
作者姓名:李玉平  张懿  齐涛  刘克玲
作者单位: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,北京,100080;中国科学院研究生院,北京,100039
2. 中国科学院过程工程研究所绿色过程与工程重点实验室,北京,100080
基金项目:国家“863”计划项目(2001AA6407010,2003AA6407010),国家自然科学基金重点基金项目(50234040)资助
摘    要:应用电感耦合等离子体发射光谱法测定了铬盐清洁工艺红矾钾产品中的微量元素硅、铝、铁、钙、锰、镁和氯。采用基体匹配法消除了大量基体的干扰。实验的优化条件为RF发生器的入射功率095kW;载气压力013MPa,流量12L·min-1;辅助气流量02L·min-1。元素氯用氯化银沉淀间接测定,在6%的硝酸体系中氯离子形成氯化物完全沉淀,在50℃陈化2h后进行测定。样品的加标回收率在90%~104%,RSD<4%,检出限在10-4%~10-5%。随机抽样的分析结果与标准加入法吻合较好,相对误差在-427%~ 526%。本方法用于实际样品分析,快速简单,结果令人满意。

关 键 词:电感耦合等离子体原子发射光谱  基体匹配  红矾钾产品  间接测量
文章编号:1000-0593(2004)11-1428-04
修稿时间:2003年9月6日

Determination of Impurities in K2Cr2O7 by an Inductively Coupled Plasma Spectrometer
Yu-ping Li,Yi Zhang,Tao Qi,Ke-ling Liu.Determination of Impurities in K2Cr2O7 by an Inductively Coupled Plasma Spectrometer[J].Spectroscopy and Spectral Analysis,2004,24(11):1428-1431.
Authors:Yu-ping Li  Yi Zhang  Tao Qi  Ke-ling Liu
Institution:Key Laboratory of Green Process and Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100080, China.
Abstract:The trace elements Si, Al, Fe, Ca, Mn, Mg, and Cl in the K2Cr2O7 produced by chromate cleaner production were determined by a sequential inductively coupled plasma spectrometer in this paper. Matrix effect was studied and eliminated through matrix matching. The analytical conditions for the elements were optimized. Incident power of the RF generator was 0.95 kW. Pressure of carrier gas flow was 0.13 MPa, and its flow rate was 1.2 L x min(-1). Auxiliary gas flow rate was 0.2 L x min(-1). The element Cl was indirectly determined by the method of AgCl precipitation. The ion Cl- can be completely precipitated in 6% nitric acid system, and then determined after keeping the solution at 50 degrees C for two hours. The recoveries of the studied impurities range from 95% to 104%, and the relative standard deviations are lower than 4% (n = 10). Detection limits of these impurities are in a range 0.0001%-0.00001% (w/w). The analytical results of random samples agree well with the results using the standard-adding method, and the relative error varies from -4.27% to +5.26%. The developed method has been applied to the determination of impurities in K2Cr2O7 product with satisfactory results.
Keywords:ICP AES  Matrix match  K_2Cr_2O_7  Indirect determination
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