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Rao等曾采用硫酸肼还原、钒酸盐滴定的方法测定纯溶液中的钼。但该文末提及杂质的干扰问题。所拟条件也常使钼的还原率偏低。本工作在以硫酸肼还原高价钼时,添加8-羟基喹啉,以使还原反应达到完全;添加草酸以防止形成钼蓝,并改进了有关滴定条件,从而改善了方法的准确度。本法快速,简便,特效性高,适于含钼在5％以上的钼矿及钼铁的分析。准确度不低于钼酸铅重量法。 (一)主要试剂钼标准溶液:称光谱纯MoO_36.0014克,以1％NaOH溶液溶解,并准确稀释至
Rao et al. Used hydrazine sulfate reduction and vanadate titration to determine molybdenum in pure solution. However, at the end of the article, the problem of interference with impurities is mentioned. The proposed conditions often make molybdenum reduction rate is low. In this work, when hydrazine sulfate is used to reduce high-valent molybdenum, 8-hydroxyquinoline is added to complete the reduction reaction; oxalic acid is added to prevent the formation of molybdenum blue and the titration conditions are improved, thus improving the accuracy of the method. This method is fast, simple and effective, suitable for the analysis of molybdenum ore and ferromolybdenum with more than 5% molybdenum. Accuracy of not less than the lead molybdate weight method. (A) The main reagent molybdenum standard solution: The spectrum of pure MoO_36.0014 grams, dissolved in 1% NaOH solution and accurately diluted to