电感耦合等离子体原子发射光谱法测定钨产品中痕量杂质元素

Determination of trace elements in tungsten products by inductively coupled plasma atomic emission spectrometry

采用在密闭塑料瓶中硝酸、氢氟酸常温常压分解样品，系统分析了样品中痕量杂质元素V、Ti、Mo、Fe、Sb、Pb、As、Co、Mg、Ca、Mn、Al、Sn、Na、K、Ni、Cr、Cd、Si、Cu、P、Bi的光谱干扰情况及钨酸沉淀分离基体后各元素的回收率情况，最终确立了电感耦合等离子体原子发射光谱（ICP—AES）法测定钨产品中痕量元素的方法。V、Ti由于基本不受基体干扰，钨酸沉淀分离基体后回收率较低，采用在校准曲线中补加基体的方法对其进行测定，其中V的测定下限为5．2μg／g，Ti的测定下限1．3μg／g；Co、Mg、Ca、Mn、Al、Na、K、Ni、Cr、Cd、Si、Cu、Pb、Sn、As、Sb、Bi等元素，受钨基体干扰比较严重，采用钨酸沉淀分离基体后，回收率均在90．0％以上，故采用沉淀分离基体，水标直接测定，各元素的测定下限均在0．10～6．7μg／g之间；而对于受钨基体严重干扰，而且钨酸沉淀分离基体后回收率较低的Fe、Mo、P3元素，目前没有很好的解决方案。此方法为解决钨产品中痕量杂质元素测定提供了一种有效可行的方法。

After the sample was dissolved with nitric acid and hydrofluoric acid in sealed plastic bottle at ambient temperature and pressure, the spectral interference of trace elements in samples, including V, Ti, Mo, Fe, Sb, Pb, As, Co, Mg, Ca, Mn, A1, Sn, Na, K, Ni, Cr, Cd, Si, Cu, Co, P and Bi, and the recoveries of elements after matrix separation by tungstic acid precipitation method was inves- tigated. Consequently, a method for determination of trace elements in tungsten products was estab- lished by inductively coupled plasma atomic emission spectrometry（ICP-AES）. For V and Ti, since there was no matrix interference and the recoveries was a little low after matrix separation by tungstic acid precipitation method, they were determined by adding matrix in the calibration curve. The low limits of determination for V and Ti were 5.2 and 1.3 ~g/g. For other elements, including Sb, Pb, As, Co, Mg, Ca, Mn, A1, Sn, Na, K, Ni, Cr, Cd, Si, Cu, Co, P and Bi, since there were serious interference from tungsten matrix, and the recoveries were over 90.0% after matrix separation by tungstic acid precipitation method, they were determined after matrix separation by tungstic acid pre- cipitation method. The low limits of determination for them were between 0. 10 and 6.7 μg/g. For Fe, Mo and P, there were no good solution because of serious interference from tungsten matrix, low recoveries after matrix separation by tungstic acid precipitation method. This method provides a feasi- ble way for determination of trace elements in tungsten products.