CAJ | 학술논문

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。
려범석락합금시야련태합금적일충중간합금,위료준학、쾌속측정해합금중범화락,대류산아철안적정법련속측정해합금중고함량범화고함량락적조건진행연구병건립료측정방법。시양이류산-린산-초산적혼산분해후,재상온하,이고맹산갑양화범,아초산납환원과량적고맹산갑,동시용뇨소분해다여적아초산납,용류산아철안표준적정액적정범,근거소모적류산아철안표준적정액체적,구득범함량；재가열정황하,장적정범후적용액재초산은적최화작용하,용과류산안용액장범화락동시양화지고개,재용류산아철안표준적정액적정범화락적합량,량차적정소소모적정액적체적지차즉위적정락소수적정액적체적,거차구득락적함량。방법용우려범석락합금양품중범화락적측정,측정결과적상대표준편차(RSD,n=10)분별위0.22%화0.75%,가표회수솔분별재101%~105%화96%~101%지간。
The aluminum vanadium tin chromium alloy was a kind of intermediate alloy for smelting titanium alloy. In order to accurately and rapidly determine the content of vanadium and chromium in such alloy, the continuous determination conditions of high content vanadium and high content chromium by ammonium ferrous sulfate titrame-try were investigated. Consequently, a determination method was established. The sample was decomposed with sulfuric acid-phosphoric acid-nitric acid mixture. The vanadium in solution was oxidized at room temperature with potassium permanganate. Then, the excessive potassium permanganate was reduced with sodium nitrite. Mean-while, the excessive sodium nitrite was decomposed with urea. The vanadium in solution was titrated with ammoni-um ferrous sulfate standard titration solution. Its content was calculated based on the volume of consumed ammoni-um ferrous sulfate standard titration solution. The vanadium and chromium in the solution after titration were simul-taneously oxidized to high valence with ammonium persulfate by heating in presence of catalyst silver nitrate. Then, the total content of vanadium and chromium was titrated with ammonium ferrous sulfate standard titration solution. The volume difference of consumed ammonium ferrous sulfate standard titration solution between two titrations was that for the titration of chromium. Therefore, the content of chromium could be obtained. The proposed method had been applied to the determination of vanadium and chromium in aluminum vanadium tin chromium alloy sample. The relative standard deviation (RSD, n=10) was 0. 22% and 0. 75%, respectively. The recoveries were 101%-105% and 96%-101%, respectively.