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    氢氧化铁共沉淀-电感耦合等离子体原子发射光谱法测定钨精矿中磷

    ICP-AES Determination of Phosphorus in Tungsten Concentrate with Ferric Hydroxide Coprecipitation

    • 摘要: 钨精矿样品经盐酸和硝酸-氢氟酸-高氯酸(体积比为1:1:1)混合溶液于聚四氟乙烯溶样罐中进行消解,在氨水介质中,样品中的微量磷与氢氧化铁形成共沉淀,从而与基体中钨和铜进行分离,再用电感耦合等离子体原子发射光谱法(ICP-AES)测定其中磷的含量。试验选择214.914 nm谱线作为磷的分析谱线,结合干扰系数校正法消除了钨对磷的光谱干扰。磷的质量浓度在10 mg·L-1以内与其光谱强度呈线性关系,检出限(3σ)为28 μg·g-1。方法应用于钨精矿样品中磷的测定,测定值的相对标准偏差(n=12)为2.4%~5.1%,测定结果与国家标准方法的测定结果有良好的一致性。

       

      Abstract: The sample of tungsten concentrate was digested with HCl and HNO3-HF-HClO4 (by volume ratio of 1:1:1) mixed solution in a closed PTFE sample dissolving tank. In ammonia, the trace phosphorus was separated with tungsten and copper in the matrix by coprecipitation with Fe(OH)3. ICP-AES was used to determine the concentration of phosphorus. The 214.914 nm spectral line was selected as the phosphorus analysis spectral line, and the spectral interference of tungsten to phosphorus was eliminated by the interference coefficient correction method.Linear relationship between values of spectral intensity and mass concentration of phosphorus was kept in the range within 10 mg·L-1, with detection limit (3σ) of 28 μg·g-1. The proposed method was applied to the determination of phosphorus in tungsten concentrate samples, values of RSD (n=12) found were in the range of 2.4%-5.1%. The results obtained by the proposed method were consistent with those of the national standard method.

       

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