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二氧化钛中砷的检测方法中,样品前处理多数采用硝酸‐盐酸‐氢氟酸混酸体系溶解,而采用此法处理样品,会存在钛容易水解且消解时间较长的问题。实验提出了硫酸‐硫酸铵体系溶解二氧化钛样品的方法,不仅解决了上述问题且反应温和,并据此建立了氢化物发生‐原子荧光光谱法(HG‐AFS)测定二氧化钛样品中砷的方法。实验表明,砷的质量浓度在0.50~20μg/L范围内与其对应的吸光度呈线性关系,线性相关系数为0.9998,方法检出限为0.05μg/L。干扰试验表明,基体钛样品中的共存元素均不干扰测定。方法用于二氧化钛实际样品分析,测定结果与电感耦合等离子体质谱法(ICP‐MS)相符,相对标准偏差(RSD ,n=11)小于5%,加标回收率为95%~101%。

For the detection of arsenic in titanium dioxide ,the sample was usually dissolved with nitric acid‐hydrochloric acid‐hydrofluoric acid system .However ,this pretreatment method had the following prob‐lems :the titanium was easily hydrolyzed;the digestion time was relatively long .In the experiment ,the dissolution method of titanium dioxide sample with sulfuric acid‐ammonium sulfate system was proposed . The problems above were solved .Moreover ,the reaction was mild .Accordingly ,the determination meth‐od of arsenic in titanium dioxide by hydride generation atomic fluorescence spectroscopy (HG‐AFS) was established .The results showed that the mass concentration of arsenic in range of 0.50‐20 μg/L had good linear relationship with the corresponding absorbance .The linear correlation coefficient was 0.999 8 .The detection limit of method was 0.05 μg/L .The interference test results indicated that the coexisting ele‐ments in matrix titanium sample did not interfere with the determination .The proposed method was ap‐plied to the analysis of actual sample ,and the found results were consistent with those obtained by induc‐tively coupled plasma mass spectrometry (ICP‐MS) .The relative standard deviation (RSD ,n=11) was less than 5% .The recoveries of standard addition were between 95% and 101% .

参考文献

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