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微波消解-容量法测定钒铝合金中的钒
引用本文:张玉平,;高树峰,;张海岩,;李彦辉,;郭玉聪.微波消解-容量法测定钒铝合金中的钒[J].承德石油高等专科学校学报,2014(2):30-32.
作者姓名:张玉平  ;高树峰  ;张海岩  ;李彦辉  ;郭玉聪
作者单位:[1]承德石油高等专科学校石油工程系,河北承德067000; [2]河北钢铁集团承钢公司河北省钒钛工程技术研究中心,河北承德067102; [3]河北钢铁集团承钢公司钒制品厂,河北承德067102
基金项目:河北省科技支撑项目(氮化钒铁与铝钒合金的检测方法的开发与应用):12214903.
摘    要:分别用微波消解技术与传统的酸解方法分解样品后,以稀硫酸为反应介质,利用高锰酸钾把钒铝合金中低价态钒氧化至五价;然后在滴加尿素的条件下,以亚硝酸钠还原过量的高锰酸钾,以N-苯代邻氨基苯甲酸为指示剂,用硫酸亚铁铵标准溶液滴定,并通过在钒标液中添加不同体积的铝标液来研究样品中铝元素对钒的质量分数测定结果的影响。该方法用于测定钒的质量分数,相对标准偏差为0.119 0%~0.270 7%,具有良好的精密度,可作为钒铝合金钒成分快速检测的可行新方法。

关 键 词:钒铝合金    容量法  微波消解

Volumetric Method Determination of Vanadium Content in Vananum with Microwave Assisted Sample Digestion
Affiliation:ZHANG Yu-ping, GAO Shu-feng ,ZHANG Hai-yan, LI Yan-hui, GUO Yu-cong ( 1. Department of Petroleum Engineering, Chengde Petroleum College, Chengde 067000, Hebei, China; 2. Hebei Province Vanadium Titanium Engineering Technology Research Center, Chengde Iron and Steel Company, Hebei Iron and Steel Group, Chengde 067102, Hebei, China; 3. Vanadium Products Factory, Chengde Iron and Steel Company, Hebei Iron and Steel Group, Chengde 067102,Hebei, China)
Abstract:The sample was decomposed with microwave digestion technique, with dilute sulfuric acid as reaction medium, using potassium permanganate to vanadium aluminum alloy with low valence vanadium oxidized to high valence vanadium; and then dropping urea, using sodium nitrite reduction of excess potassium permanganate and N-benzene substituted O-Aminbenzoic acid as indicator, titration with ferrous ammonium sulfate standard solution. By adding different content of aluminum standard solution into vanadium standard solution, we tested how much aluminum effect on the measured results. Method for determination of sample, the relative standard deviation is 0. 1190% - 0. 2707%. The results of application showed that this method had good precision in determining vanadium in vanadium aluminum alloy, and can be used as a new method of feasible detection of vanadium in vanadium aluminum alloy smelting production.
Keywords:vananum  vanadium  volumetry  microwave digestion
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