硫酸氧钒的制备及硫酸氧钒中钒的测定

以五氧化二钒为原料，研究了制备硫酸氧钒的方法，并研究了硫酸氧钒中钒含量的测定方法．五氧化二钒经浓硫酸溶解活化后，经草酸还原等系列实验过程制备高纯度的硫酸氧钒蓝色晶体．考察了反应温度对反应的影响，结果显示在90~C条件下，硫酸氧钒产率为92．13％．将制得的硫酸氧钒试样经高锰酸钾氧化，用亚硝酸钠、尿素除去干扰物，以邻苯氨基苯甲酸作指示剂，在pH=0的酸性条件下，用硫酸亚铁氨溶液进行滴定，测得钒的含量约为29．56％，表明所制备的样品纯度较高．

Vanadyl Sulfate Preparation and Determination of Its Vanadium

In this paper, it was studied for the preparation of vanadyl sulfate using vanadium pentoxide as raw ma- terials and the method for determination of vanadium content in vanadyl sulfate was established. The pure vanadyl sul- fate in blue crystal form was obtained from vanadium pentoxide by process for activation of sulfuric acid and reduction of oxalic acid in turn. The effect of temperature on the resultant product was investigated, and the yield of vanadyl sul- fate reach 92. 13% at the optimal reaction temperature of 90 ℃. The determination of V in vanadyl sulfate was carried out by volumetric analysis. The samples of vanadyl sulfate were treated by potassium permanganate with sodium nitrite, urea to remove interfering substances, then the solutions obtained were titrated by ammonium ferrous sulfate using n - phenylanthranilic acid as indicator under pH of 0. It was found that average V content in the resultant products is 29. 56% which indicated the purity of vanadyl sulfate prepared by this method is high.