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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
  • 期刊名称:岩矿测试, 2006, 25(4): 319-322
  • 时间:0
  • 分类:O657.75[理学—分析化学;理学—化学] O652.4[理学—分析化学;理学—化学]
  • 作者机构:[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
  • 相关基金: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
  • 相关项目:基于金属氧化物纳米颗粒的半胶束/吸附胶束行为研究及其在环境污染物固相萃取和固相微萃取中的应用
中文摘要:

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。

英文摘要:

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.

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