电感耦合等离子体原子发射光谱法测定废钒催化剂中的钒  

Determination of Vanadium in Spent Vanadium Catalyst by Inductively Coupled Plasma Atomic Emission Spectrometry

作　　者：王艳红 WANG Yan-hong(Shenyang Research Institute of Nonferrous Mentals Co.,Ltd.,Shenyang 110141,China)

机构地区：[1]沈阳有色金属研究院有限公司,辽宁沈阳110141

出　　处：《有色矿冶》2020年第3期51-53,共3页Non-Ferrous Mining and Metallurgy

摘　　要：研究了用电感耦合等离子体原子发射光谱法(ICP-AES)测定废钒催化剂中的钒元素的条件,并建立了测定方法。采用盐酸、硝硫混酸(体积比7∶3)溶解样品,在冒三氧化硫白烟时滴加硝硫混酸使碳化物完全溶解,废钒催化剂的载体也溶解完全。选择V311.071nm波长的光谱线作为钒的分析线,在选择最佳条件下测定,废钒催化剂中铝、钛、钾、铁等共存元素对测定无干扰。钒的质量分数在0.1%~10%范围内元素质量分数与对应的发射强度呈线性,其校准曲线线性相关系数均不小于0.999 7,方法中钒元素检出限为0.0008%(质量分数)。本法用于实际样品的分析,结果的相对标准偏差(RSD,n=6)在0.66%~3.03%之间,结果与硫酸亚铁铵滴定法测定的结果基本一致。The determination condition of vanadium in spent vanadium catalyst by inductively coupled plasma atomic emissin spectrometry(ICP-AES)was studied,and accordingly,a determination method was established.The sample was dissolved by hydrochloric acid,nitro-sulfur mixed acid(volume ration 7∶3).In the white smoke of sulfur trioxide,nitro-sulfur mixed acid was added to completely dissolve the carbide,and the suppor of the spent vanadium catalyst was also completely dissolved.V311.07 nm was selected as analytical line.Under the optimum conditions,the co-existing elements sucu as aluminum,titanium,potassium and iron in the spent vanadium catalyst had no interference to the determination.When the mass fraction of vanadium was in range of 0.1%~10%,the mass concentration showed good linearty to the corresponding emission intensity.The linear correlation coefficients of colibration curves were higer than 0.9997.The detection limit of vanadium in this method was 0.0008%(mass fraction).The proposed method was applied to the analysis of actual samples,and the found results were consistent with those obtained by titration with ammonium ferrous sulfate.The relative standard deviations(RSD,n=6)of determination results were between 0.66%and 3.03%.

关 键 词：电感耦合等离子体原子发射光谱法(ICP-AES) 废钒催化剂 钒 硝硫混酸 

分 类 号：O657.31[理学—分析化学]