特号镍,按我国产品规定,含镍不少于99.985％,铅量不大于0.0003％。在如此大量基体元素镍中,定量测定其中痕量铅有国外的经典方法和我国冶金部部颁化学分析法,但试样用量大(如10克),前者需用大量剧毒试剂氰化钾,而后者用双硫腙显色灵敏度虽高,但选择性差。方法中测铅所需试剂均要求纯度高或须高度净化达到双硫腙检验合格后方可使用,这给分析工作带来困难和不便,此外相对增加了分析费用。看来上述方法均有其缺点。 本文改用萃取催化示波导数极谱法,避免使用双硫腙和氰化钾,以期提供另一测定途径。 据文献,我们以碘化钾-盐酸羟胺的 Special Nickel, according to our product regulations, not less than 99.985% nickel, lead content of not more than 0.0003%. In such a large amount of matrix nickel, quantitative determination of trace amounts of lead there are foreign classical methods and China’s Ministry of Metallurgy Ministry of Chemical Analysis, but the sample dosage (such as 10 grams), the former need to use a large number of highly toxic reagents, potassium cyanide , While the latter with dithizone color sensitivity is high, but the selectivity is poor. The required reagents for measuring lead in the method all require high purity or high purity to be used after being qualified by dithizone test, which brings difficulties and inconveniences to the analysis work and additionally increases the analysis cost. It seems that the above methods have their drawbacks. In this paper, the extraction catalytic oscillographic derivative polarography was used to avoid the use of dithizone and potassium cyanide in order to provide another route of determination. According to the literature, we take potassium iodide - hydroxylamine hydrochloride