高锰酸钾氧化-亚铁滴定法测定钒铝合金中的钒量

Determination of Vanadium in Vanadium-Aluminium alloys by KMnO4-Ferrous titration method

摘要:

采用硫酸-磷酸-硝酸混酸溶解试样，高锰酸钾氧化-硫酸亚铁铵滴定法测定钒铝中间合金中的钒量。考察了试样分解方法、钒的氧化条件、高锰酸钾用量、亚硝酸钠用量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。对含钒量不同的6个钒铝合金样品中钒量进行11次测定，测定结果在49.45%～83.33%之间，方法的相对标准偏差（RSD）均为0.2%左右，加标回收率在98.2%～102.5%之间。通过与其他7家实验室间的比对试验，测定结果一致性好、无明显系统偏差。所建立的方法具有操作简便、快速，测定含量范围宽，结果准确等特点。适用于各种钒铝合金中钒量的测定。

Abstract:

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.