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敞开酸溶-电感耦合等离子体光谱法测定钨矿石和钼矿石中微量元素

Simultaneous Determination of Trace Elements in Tungsten Ore and Molybdenum Ore with Open Acid Digestion by Inductively Coupled Plasma-Atomic Emission Spectrometry

  • 摘要: 钨矿石和钼矿石具有丰富的共生或伴生元素,检测共生或伴生元素的含量有利于矿产资源的综合利用。在国家标准方法中钨矿石和钼矿石的共生或伴生元素含量是按元素分别检测,效率很低。本文在敞开体系中用盐酸+硝酸+氢氟酸+高氯酸消解样品,以7%盐酸溶解盐类,电感耦合等离子体发射光谱同时测定钨矿石和钼矿石中铋、钴、铜、锂、镍、磷、铅、锶、钒、锌等10种微量元素。选定了各元素的分析谱线和光谱级次,采用离峰背景校正法消除背景干扰,干扰元素校正系数法消除元素间的谱线重叠干扰。方法检出限为1.43~18.8 μg/g,加标回收率为90%~110%。经钨矿石和钼矿石标准物质分析验证,测定结果与标准值基本吻合,方法精密度(RSD,n=10)小于8%。该方法克服了碱熔引入大量碱金属元素以及可能引入杂质的缺陷,又不用处理钨酸和钼酸沉淀,能快速测定钨矿石和钼矿石中微量共生或伴生元素。

     

    Abstract: Tungsten and molybdenum ores have abundant paragenesis or associated elements. Detection of these elements is beneficial to the comprehensive utilization of mineral resources. At present, the contents of these elements are detected respectively by the national standard method of tungsten ore and molybdenum ore, which has a low efficiency. A method for the determination of trace elements in tungsten ore and molybdenum ore by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) is proposed. Tungsten ore and molybdenum ore samples were dissolved by HCl-HNO3-HF-HClO4 at normal pressure and extracted by hydrochloric acid (7% of HCl). The 10 trace elements of Bi, Co, Cu, Li, Ni, P, Pb, Sr, V and Zn were simultaneously measured by ICP-AES. Analytical wavelength and spectral level of elements were selected. The background interferences were eliminated with an off-peak background correction method,and the spectral overlapping interferences between elements were eliminated using an interference elements correction coefficients method.The detection limits were 1.43-18.8 μg/g and the recovery rates were 90%-110%. This method has been applied to the determination of tungsten ore and molybdenum ore national certified reference materials, and the results were in good agreement with the certified values with RSD (n=10) 1ess than 8%. The method avoided the influence of adding a large amount of alkali metal elements and probably foreign matter with alkali fusion, without precipitation processing of tungstic acid and molybdic acid. It can be used to rapidly determine paragenesis or associated elements in tungsten ore and molybdenum ore.

     

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