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采用HNO3+HCl+HF作为消解试剂,样品经微波消解后,用L-半胱氨酸预还原,以氢化物发生-原子荧光光谱法对二氧化钛中砷和锑进行了分析。探讨了盐酸、硼氢化钾溶液浓度以及样品还原处理对测定结果的影响,确定了实验的最佳测定条件。结果表明,砷、锑在0~25μg/L范围内线性关系良好,线性相关系数均为0.999 9,砷和锑的检出限分别为0.058μg/L和0.075μg/L。对5μg/L的砷、锑连续11次进样,测得结果的相对标准偏差分别为0.71%和0.78%。方法用于二氧化钛样品的测定,测定结果与ICP-AES测定结果相符,回收率为96%-108%。
HNO3 + HCl + HF was used as the digestion reagent. The samples were digested with microwave and pre-reduced with L-cysteine. The arsenic and antimony in titanium dioxide were analyzed by hydride generation-atomic fluorescence spectrometry. The effects of hydrochloric acid, potassium borohydride concentration and sample reduction on the determination results were discussed, and the best experimental conditions were determined. The results showed that arsenic and antimony had a good linearity in the range of 0-25 μg / L, the linear correlation coefficient was 0.999 9, and the detection limits of arsenic and antimony were 0.058 μg / L and 0.075 μg / L, respectively. The relative standard deviations (RSDs) of 5 μg / L arsenic and antimony were 11 injections, and the relative standard deviations were 0.71% and 0.78%, respectively. The method was applied to the determination of titanium dioxide. The determination results were consistent with those of ICP-AES. The recovery rate was 96% -108%.