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测定高纯三氧化钨中的痕量杂质元素,通常采用光谱分析法。其方法又可分为载体分馏法,化学光谱法和蒸发法等。后两种方法分析灵敏度较高,但对试剂要求较严,设备亦较复杂。载体法较简便,但进行多元素同时测定,要同时得到较好的分馏效应却十分困难;常因操作上的因素引起分馏效应不佳,从而得到较差的重复性。本工作按照文献中提出的载体成分,下电极采用罩帽杯形电极,上电极用带有孔穴的锥形电极,内装满含有10%NaCl的碳粉,分二次曝光,用0.05%的锗和镱为内标。测定了三氧化钨中的铝、铋、钙、镉、钴、铬、铜、铁、镍、镁、锰、钼、铅、锑、硅、锡、铁、钒等十八种杂质元素。其测定下限达0.3～10ppm,
Determination of trace impurities in high purity tungsten trioxide, usually by spectroscopic analysis. The method can be divided into carrier fractionation, chemical spectroscopy and evaporation. The latter two methods have higher sensitivity but require more stringent reagents and the equipment is more complex. Carrier method is relatively simple, but the simultaneous determination of multiple elements, to get a good fractionation effect is very difficult at the same time; often due to operational factors caused by poor fractionation effect, resulting in poor repeatability. In this work, according to the carrier composition proposed in the literature, the lower electrode adopts a cap cup electrode, the upper electrode is a conical electrode with a hole filled with a carbon powder containing 10% NaCl, and is exposed twice with 0.05% Germanium and ytterbium are internal standards. Eightteen kinds of impurity elements such as aluminum, bismuth, calcium, cadmium, cobalt, chromium, copper, iron, nickel, magnesium, manganese, molybdenum, lead, antimony, silicon, tin, iron and vanadium in tungsten trioxide were determined. The lower limit of determination of 0.3 ~ 10ppm,