硫酸亚铁铵滴定法连续测定铝钒锡铬合金中钒和铬

发布时间：2018-04-30 23:42

本文选题：硫酸亚铁铵 + 铝钒锡铬合金　；参考：《冶金分析》2015年06期

【摘要】：铝钒锡铬合金是冶炼钛合金的一种中间合金,为了准确、快速测定该合金中钒和铬,对硫酸亚铁铵滴定法连续测定该合金中高含量钒和高含量铬的条件进行研究并建立了测定方法。试样以硫酸-磷酸-硝酸的混酸分解后,在常温下,以高锰酸钾氧化钒,亚硝酸钠还原过量的高锰酸钾,同时用尿素分解多余的亚硝酸钠,用硫酸亚铁铵标准滴定液滴定钒,根据消耗的硫酸亚铁铵标准滴定液体积,求得钒含量;在加热情况下,将滴定钒后的溶液在硝酸银的催化作用下,用过硫酸铵溶液将钒和铬同时氧化至高价,再用硫酸亚铁铵标准滴定液滴定钒和铬的合量,两次滴定所消耗滴定液的体积之差即为滴定铬所需滴定液的体积,据此求得铬的含量。方法用于铝钒锡铬合金样品中钒和铬的测定,测定结果的相对标准偏差(RSD,n=10)分别为0.22%和0.75%,加标回收率分别在101%~105%和96%~101%之间。
[Abstract]:Aluminum vanadium tin chromium alloy is a master alloy for smelting titanium alloy. In order to determine vanadium and chromium in the alloy quickly, The conditions for the continuous determination of vanadium and chromium in the alloy by ammonium ferrous sulfate titration were studied and the determination method was established. The sample was decomposed with a mixture of sulfuric acid, phosphoric acid and nitric acid, vanadium was oxidized with potassium permanganate at room temperature, excess potassium permanganate was reduced by sodium nitrite, excess sodium nitrite was decomposed with urea, vanadium was titrated with standard titration solution of ammonium ferrous sulfate, The vanadium content is obtained according to the volume of standard titration solution of ammonium ferrous sulfate consumed. Under the condition of heating, the vanadium and chromium after titration are oxidized to high value with ammonium persulfate solution under the catalysis of silver nitrate. After titrating vanadium and chromium with standard ammonium ferrous sulfate titration solution, the difference between the volume of the titrate consumed by the two titrations is the volume of the titrate required for the titration of chromium, and the content of chromium is obtained. The method has been applied to the determination of vanadium and chromium in aluminum, vanadium, tin and chromium alloys. The relative standard deviations of the determination results are 0.22% and 0.75%, respectively. The recoveries are between 101% and 96%.
【作者单位】：西部金属材料股份有限公司理化检验中心;
【分类号】：TG115.3

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