Abstract:In order to improve the control efficiency of vanadium hydrometallurgy process, a method for the determination of vanadium content by hydrogen peroxide spectrophotometry based on the coloring characteristics of peroxide-vanadium ion [VO(O2)+] was proposed, realizing the rapid determination of vanadium content in sample on site. Firstly, the pH of sample solution was adjusted to 9-10 by adding appropriate amount of sodium hydroxide solution. Hydrogen peroxide was added to fully oxidize the low-valence vanadium to vanadium (V). Then sulfuric acid was added to adjust the solution to be acid. Vanadium (V) could react with hydrogen peroxide at room temperature to form a stable red-brown peroxide-vanadium ion [VO(O2)+]. The absorbance was measured at 450 nm. The Bill's law was obeyed between the absorbance and mass concentration of vanadium in range of 2.0-400 mg/L. The contents of vanadium in three vanadium extraction liquid samples of hydrometallurgy (including vanadium leaching solution, solution after vanadium precipitation, and wastewater) were determined according to the experimental method. The relative standard deviation (RSD, n = 10) of determination results was 0.38%, 3.5% and 7.6%, respectively. The found results were consistent with those obtained by potassium permanganate oxidization-ammonium ferrous sulfate titration method.
[1] 陈家镛.湿法冶金手册[M].北京:冶金工业出版社,2005:935-984. [2] 贾秀敏,李培佑,黄永,等.陕西某钒矿石钙化焙烧-酸浸工艺研究湿法冶金[J].湿法冶金,2015,34(3):182-185,196. JIA Xiumin,LI Peiyou,HUANG Yong,et al.Leaching of tungsten and molybdenum from molybdenum slag[J].Hydrometallurgy of China,2015,34(3):182-185,196. [3] 匡敬忠,李成,贾帅,等.从含钒磁铁矿精矿中浸出钒的试验研究[J].湿法冶金,2013,32 (3):143-146. KUANG Jingzhong,LI Cheng,JIA Shuai,et al.Study on leaching of vanadium from magnetite concentrate containing vanadium[J].Hydrometallurgy of China,2013,32(3):143-146. [4] 耿立唐,李兰杰,赵备备,等.钒化工流程高效提取钒元素[J].过程工程学报,2017,17(4):744-750. GENG Litang,LI Lanjie,ZHAO Beibei,et al.High efficiency leaching of vanadium in vanadium chemical process[J].The Chinese Journal of Process Engineering,2017,17(4):744-750. [5] 龚明明,孙浩波,宫增艳,等.石煤钠化焙烧物中不同价态钒的测定[J].湿法冶金,2012,31(4):260-263. GONG Mingming,SUN Haobo,GONG Zengyan,et al.Determination of vanadium in stone coaled with sodium codium chloride[J].Hydrometallurgy of China,2012,31(4):260-263. [6] 曾繁武,宋明明,陈彦博,等.不同基准物质及标准滴定溶液标定亚铁时对测定钒含量的影响[J].冶金分析,2013,33(10):69-72. ZENG Fanwu,SONG Mingming,CHEN Yanbo,et al. Effect of various reference materials and standard titration solution on the determination of vanadium content during the calibration of ferrous[J].Metallurgical Analysis,2013,33(10):69-72. [7] 曾繁武,宋明明,王姝婷.电位滴定法测定钒储能介质中钒(Ⅲ)和全钒[J].理化检验(化学分册),2018,54(5):563-565. ZENG Fanwu,SONG Mingming,WANG Shuting,et al. Potentiometric titration for the synchronous analysis of trivalent vanadium and total vanadium in the electrolyte[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2018,54(5):563-565. [8] 黎涛,冯自平,陈金发,等.电感耦合等离子体原子发射光谱法测定偏钒酸铵中钒含量[J].理化检验(化学分册),2011,47(9):1086-1087. LI Tao,FENG Ziping,CHEN Jinfa,et al.ICP-AES determination of vanadium in ammonium metavanadate[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2011,47(9):1086-1087. [9] 李桂艳,周之荣,陈安银,等.钒的痕量分析方法与应用的研究进展[J].光谱实验室,2009,26(2):269-277. LI Guiyan,ZHOU Zhirong,CHEN Anyin,et al. Progress in research and application of trace analysis methods for vanadium[J].Chinese Journal of Spectroscopy Laboratory,2009,26(2):269-277. [10] 季彦鋆,唐姚瑶,沈沁怡,等.石墨炉原子吸收法测定地表水中钒的方法探讨[J].环境科学与管理,2013,38 (5):157-159. JI Yanyun,TANG Yaoyao,SHEN Qinyi,et al.Determination of vanadium in water by graphite furnace atomic absorption spectrometry method[J].Environmental Science and Management,2013,38(5):157-159. [11] 魏清清,杨金燕.分光光度法测定水中钒全量的改进[J].工业安全与环保, 2015,41(5):61-63. WEI Qingqing,YANG Jinyan.Determination of vanadium concentration in water by improved spectrophotometry[J].Industrial Safety and Environmental Protection,2015,41(5):61-63. [12] 翟庆洲,胡伟华,袁克英,等.钒光度分析研究的进展[J].理化检验(化学分册),2004,40(3):182-186. ZHAI Qingzhou,HU Weihua,YUAN Keying,et al.Progress of the research on photometry of vanadium[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2004,40(3):182-186. [13] George Telep, D F Boltz.Ultraviolet spectrophotometric determination of vanadium[J].Analytical Chemistry,1951,23(6):901-903. [14] Mato Orhanovic,Ralph G Wilkins. Kinetic Studies of the reactions of peroxy compounds of chromium(VI), vanadium(V), and titanium(IV) in acid media[J]. Journal of the American Chemical Society,1967,89(2):278-282. [15] G A Dean. Studies on the pervanadium complex[J].Can. J. Chem.,1961,39:1174-1183. [16] Alison Butler,Melissa J Clague,Gretchen E Meister.Vanadium peroxide complexes[J].Chem. Rev.,1994,94:625-638.