【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OnGuardⅡH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。更多还原

【Abstract】 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.更多还原