高锰酸钾氧化-亚铁滴定法测定钒铝合金钒含量

Determination of Vanadium in Vanadium-Aluminium Alloys by KMnO_4-Ferrous Titration Method

介绍了硫酸-磷酸-硝酸混酸溶解试样,钒铝中间合金中钒量的高锰酸钾氧化-硫酸亚铁铵滴定法。考察了试样分解方法、钒的氧化条件、尿素用量、亚硝酸钠用量、溶液酸度的影响及共存离子干扰等一系列条件对钒测定结果的影响,确定了最佳实验条件。运用此法对含钒量不同的6个钒铝合金样品中钒量进行11次测定,含钒量从50%到85%,相对标准偏差（RSD）均不大于0.2%,加标回收率在98.2%～102.5%。通过与其他7家实验室间的比对试验,证实该法测定结果无明显系统偏差,适于推广应用。

A method for the determination of Vanadium in Vanadium-Aluminium master alloys by KMnO4 -Ferrous titration method is presented .The sample was digested by H2SO4-H3PO4-HNO3. The influence of the method for sample digestion; the amount of KMnO4 and NaNO2; the interference of co-existence elements were discussed so as to confirm the best condition. The proposed method was applied to determine the Vanadium contents in six Vanadium-Aluminium master alloy samples whose Vanadium content was different from 49.45% to 83.33%. The results showed that the relative standard deviations（n=11） were all about 0.2%, and the recoveries were in the range of 98.2%～102.5%.Compared with 7 different laboratories , the results were consistent without significant deviation. This method has the advantages of fast,accurate and a wide analytical range. It is suitable for determination Vanadium in Vanadium-Aluminium master alloys.