离子色谱法测定五氧化二铌和五氧化二钽中痕量氟氯和硫酸根离子的前处理方法  

Pretreatment Method for the Determination of Trace Fluoride,Chloride and Sulfate in Tantalum Pentoxide and Columbium Pentoxide by Ion Chromatography

作　　者：刘肖[1] 滕曼[1] 蔡亚岐[1] 牟世芬[1] 

机构地区：[1]中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室,北京100085

出　　处：《岩矿测试》2006年第4期319-322,共4页Rock and Mineral Analysis

基　　金：国家重点基础研究计划(973)资助项目(2003CB415001);国家自然科学基金资助项目(20577058);中国科学院优秀博士论文科研基金资助项目

摘　　要：采用马弗炉将样品与NaOH混合进行熔融煅烧，热去离子水提取、离心、稀释后过OnGuard Ⅱ H柱和过滤膜进行前处理，抑制型电导离子色谱法检测，测定了Ta2O5和Nb2O5的氟离子、氯离子和硫酸根离子。该方法对三种被测阴离子的检测限（s／N=3）在0．15～0．70μg／g（以固体样品实际浓度计）或0．136～0．623μg／L（以溶液浓度计），标准曲线线性范围均在两个数量级以上，方法的精密度（RSD，n=7）小于5．46％，回收率为88％～106％，具有灵敏度高、选择性好、重现性佳、对环境友好等特点，用于实际样品的检测，结果令人满意。The present paper introduces a method in which tantalum pentoxide and columbium pentoxide samples pretreated by calcining with NaOH in Muffle, extracting and diluting by DI water, passing sample solution through OnGuard Ⅱ H cartridges and 0.22 μm micropore nylon filtration membranes followed by separating analytes with ion chromatography and detecting trace anions by suppressed conductivity detector. The detection limits （s/N = 3） of the method for fluoride, chloride and sulfate are from 0.15 μg/g to 0.70 μg/g （calculated by the concentrations in solid samples） or from 0.136 μg/L to 0.623 μg/L （calculated by the concentration in solutions）. All three calibration curves are linear over two orders of magnitude. The recoveries for three analytes are between 88%～106% with precision of less than 5.46% RSD （n = 7）. This method possesses of the advantages of high sensitivity, distinguished selectivity, good reproductivity and being-friendly to the environment.

关 键 词：离子色谱法 氟 氯 硫酸根 前处理 五氧化二铌 五氧化二钽 

分 类 号：O657.75[理学—分析化学] O652.4[理学—化学]