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纯银中的痕量杂质元素多用发射光谱法测定,但由于锑的挥发损失,往往给光谱分析制样带来困难.锑在许多介质中都有极谱波.观察锑在盐酸介质中的示波极谱行为时,发现在+0.15～+0.40伏范围里出现的锑(Ⅲ)的氧化波,波形比之在同一介质中的还原波更好,测定时不必除氧,简化了手续.锑的这一氧化波未见报导,因此我们通过试验确定了测定锑的最佳条件,并用硝酸溶解试样,以铬(Ⅲ)为共沉淀剂,用氨水沉淀分离出锑.利用这一氧化波测定纯银中的痕量锑.
Trace impurity elements in sterling silver are determined by multiple emission spectrometry, but due to the loss of volatility of antimony, it is often difficult to prepare samples for spectroscopic analysis. Antimony has a polarographic wave in many media. It was found that the oxidation wave of antimony (Ⅲ) appeared in the range of +0.15 to +0.40 volts, the waveform was better than the reduction wave in the same medium, and the procedure did not need to be deoxidized, which simplified the procedure. Of the oxidation wave has not been reported, so we determined by testing the best conditions for the determination of antimony, and nitric acid dissolved in the sample, with chromium (Ⅲ) as a coprecipitant precipitated with ammonia precipitation antimony using this oxidation wave Determination of trace silver in sterling silver.