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    电感耦合等离子体原子发射光谱法测定高纯五氧化二钒中11种元素的含量

    Determination of 11 Elements in High Purity Vanadium Pentoxide by Inductively Coupled Plasma Atomic Emission Spectrometry

    • 摘要: 取0.050 0~0.100 0 g高纯五氧化二钒样品置于铂金坩埚中,加入1.000 0~1.200 0 g助熔剂(质量比1∶2的硼酸-碳酸钾混合物),搅拌均匀,于950 ℃熔融15 min,冷却后将坩埚置于含40 mL 20%(体积分数)盐酸溶液的烧杯中,浸出完毕后转移至100 mL容量瓶,用水定容,采用电感耦合等离子体原子发射光谱法测定钠、铝、钙、铁、镁、锰、铬、砷、钛、硅、磷等11种元素的含量,其中钠、硅、钙采用基质匹配法定量,其余8种元素采用外标法定量。结果显示,各元素的质量浓度在2.0 mg·L−1以内与对应的响应强度呈线性关系,检出限(3s)为0.001 3~0.027 mg·L−1。实际样品测定值的相对标准偏差(n=10)均小于0.50%,按照标准加入法进行回收试验,回收率为95.5%~100%。采用标准样品进行准确度验证,测定值与认定值基本一致。

       

      Abstract: The high purity vanadium pentoxide sample (0.050 0-0.100 0 g) was taken and placed in a platinum crucible, and 1.000 0~1.200 0 g of a fluxing agent (a mixture of boric acid and potassium carbonate at a mass ratio of 1∶2) was added. The mixture was stirred evenly and melted at 950 ℃ for 15 min. After cooled, the crucible was placed in a beaker containing 40 mL of 20% (volume fraction) hydrochloric acid solution. After the leaching was completed, the mixture was transferred to a 100 mL-volumetric flask, and made its volume up with water. The 11 elements including sodium, aluminum, calcium, iron, magnesium, manganese, chromium, arsenic, titanium, silicon, and phosphorus in the solution were determined by inductively coupled plasma atomic emission spectrometry. Among them, sodium, silicon, and calcium were quantified using matrix matching method, while the remaining 8 elements were quantified using external standard method. As shown by the results, linear relationships between the corresponding response intensities and mass concentrations of 11 elements were kept within 2.0 mg · L−1, with detection limits (3s) in the range of 0.001 3-0.027 mg · L−1. RSDs (n=10) of the determined values of actual samples were less than 0.50%. Test for recovery was made according to the standard addition method, giving results in the range of 95.5%-100%. Standard samples were used for accuracy verification, and the determined values were basically consistent with the certified values.

       

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