Abstract：There were some problems during determination of vanadium in titanium-aluminum-vanadium alloy by ammonium ferrous sulfate titrimetry. For example, the sample was hardly dissolved. Moreover, the high-content titanium in sample was easily hydrolyzed, which would interfere with the judgment of color at titration endpoint. After the sample was dissolved in nitric acid-hydrofluoric acid-sulfuric acid system, sodium hydroxide was added to react with matrix titanium to form sodium trititanate precipitate, realizing the separation of titanium and vanadium. In mixed sulfuric acid-phosphoric acid medium, vanadium in filtrate was fully oxidized to pentavalent vanadium with potassium permanganate. The excessive potassium permanganate was reduced with sodium nitrite, and then the excessive sodium nitrite was decomposed with urea. The content of vanadium was titrated with ammonium ferrous sulfate standard solution with N-phenylanthranilic acid as indicator. Consequently, a determination method of vanadium in titanium-aluminum-vanadium alloy was established by ammonium ferrous sulfate titrametry. The interference tests of coexisting elements indicated that the coexisting elements in the sample did not interfere with the determination. The content of vanadium with mass fraction in range of 3%-6% in two titanium-aluminum-vanadium alloy samples was determined according to the experimental method. The relative standard deviation (RSD, n=6) was 0.20% and 0.25%, respectively. The proposed method was applied for determination of vanadium in six titanium-aluminum-vanadium alloy samples, and the results were consistent with those obtained by flame atomic absorption spectrometry (FAAS).
阚文斌,林均品.增材制造技术制备钛铝合金的研究进展[J].中国材料进展,2015(2):15-23.KAN Wen-bin,LIN Jun-pin.Research progress on fabrication of aluminide fabricated by additive manufacturing[J].Materials China,2015(2):15-23.
[2]
刘素琴,桑玉,李林德,等.电位滴定法测定钒电池电解液中不同价态的钒[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B:Chemical Analysis),2007,43(12):90-93.
[3]
付二红,蒙玉林,汪磊.可视滴定法测定铝钒中间合金中的钒时称样量和滴定液浓度的优化[J].化学分析计量,2013,22(2):97-101.FU Er-hong,MENG Yu-lin,WANG Lei.Optimization of the sampling and titration concentration of vanadium in the determination of vanadium in aluminium-vanadium master alloy by visual titration[J].Chemical Analysis and Meterage,2013,22(2):97-101.
[4]
刘兴沂,魏燕,金玉清,等.硫酸亚铁铵滴定法快速测定钒氮铁合金中的钒[J].山东冶金,2009,31(1):48-49.LIU Xing-yi,WEI Yan,JIN Yu-qing,et al.The determination of vanadium in vanadium ferroalloys was quickly determined by ammonium ferrous sulfate titration[J].Shandong Metallurgy,2009,31(1):48-49.
[5]
陈自斌,杨新能,李小青,等.硫酸亚铁铵滴定法测定铁矿石中钒含量国家标准研究[J].冶金标准化与质量,2012,50(1):6-9.CHEN Zi-bin,YANG Xin-neng,LI Xiao-qing,et al.Study on national tandard for the determination of vanadium in iron ore by ammonium ferrous sulfate titrimetric method[J].Metallurgical Standardization and Quality,2012,50(1):6-9.
[6]
唐华.PAR光度法测定钒[J].高师理科学刊,2000,20(2): 35-37.TANG Hua.Assay vanadium by par absorbance analysis[J].Journal of Science of Teachers,2000,20(2): 35-37.
[7]
韦筱香,余莉莉.钽试剂萃取光度法测定合金钢中微量钒含量[J].化学过程与装备,2010(3):148-149,109.WEI Xiao-xiang,YU Li-li.Determination of trace amount of vanadium in alloy steel by tantalum reagent extraction photometric method[J].Chemical Engineering & Equipment,2010(3):148-149,109.
[8]
邱林友,赵尔燕.分光光度法测定铸铁中钒[J].现代铸铁,1991(3):35-37.QIU Lin-you,ZHAO Er-yan.Determination vanadium in cast iron by the spectrophotometry[J].Modern Cast Iron,1991(3):35-37.
