电感耦合等离子体发射光谱（ICP-OES）法测定废钒触媒中钒的含量
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摘要
建立了用盐酸、硝酸、氢氟酸和高氯酸混合酸溶解样品,采用电感耦合等离子体发射光谱(ICPOES)法测定废钒触媒中钒含量的分析方法。确定了最佳溶样方法和仪器的最佳条件。在选定的操作条件下,钒的检出限0.006μg/mL,相对标准偏差(RSD,n=11)<1%,加标回收率在98.9%～101%,用来测定废钒触媒中钒的含量,流程短、易操作,结果令人满意。
A method for the determination of vanadium in waste vanadium catalyst by inductively coupled plasma optical emission spectrometry(ICP-OES)was developed.The sample was dissolved with mixed acid of hydrochloric acid nitric acid hydrofluoric acid and perchloric acid and the content of vanadium in waste vanadium catalyst was determined by ICP-OES.The optimum sample dissolution method and the optimum conditions of the instrument were determined by this method.Under the selected operating conditions,the detection limit of vanadium is 0.006μg/mL.The relative standard deviation(RSD,n=11)less than 1%and the recovery rate is 98.9%—101%.This method can be used to determine the content of vanadium in waste vanadium catalyst.The process is short and easy to operate with satisfactory results.
A method for the determination of vanadium in waste vanadium catalyst by inductively coupled plasma optical emission spectrometry(ICP-OES)was developed.The sample was dissolved with mixed acid of hydrochloric acid nitric acid hydrofluoric acid and perchloric acid and the content of vanadium in waste vanadium catalyst was determined by ICP-OES.The optimum sample dissolution method and the optimum conditions of the instrument were determined by this method.Under the selected operating conditions,the detection limit of vanadium is 0.006μg/mL.The relative standard deviation(RSD,n=11)less than 1%and the recovery rate is 98.9%—101%.This method can be used to determine the content of vanadium in waste vanadium catalyst.The process is short and easy to operate with satisfactory results.
引文
[1]刘彬，于少明，张颍，等．废钒催化剂综合回收利用技术的研究[J]．无机盐工业，2012,44(11):157-59.LIU Bin,YU Shaoming,ZHANG Ying,et al.Study on comprehensive recovery and utilization technology of waste vanadium catalyst[J]. Inorganic Chemicals Industry,2012,44(11):157-59.
[2]郝喜才，高敏杰，李洁．废钒催化剂回收技术研究进展[J]．开封大学学报，2017,31(2):74-78.HAO Xicai,GAO Minjie,LI Jie.Recycling technology of waste vanadium catalyst[J].Journal of Kaifeng University,2017,31(2):74-78.
[3]刘波，童庆云，李国良．氧化焙烧法回收废钒触媒中的钒[J]．四川大学学报（工程科学版），2002,34(2):112-115.LIU Bo,TONG Qingyun,LI Guoliang.Recovery of vanadium from waste vanadium catalyst by oxidation roasting[J].Journal of Sichuan University(Engineering Sicence Edition),2002,34(2):112-115.
[4]邵延海，冯其明，欧乐明，等．从废催化剂氨浸渣中综合回收钒和钼的研究[J]．稀有金属，2009,33(4):606-610.SHAO Yanhai,FENG Qiming,OU Leming,et al.Comprehensive recovery of vanadium and molybdenum from waste catalyst ammonia leaching residue[J].Chinese Journal of Rare Metals,2009,33(4):606-610.
[5]梅毅．电感耦合等离子体原子发射光谱测定钒钛高炉渣中钪镓铬镍钴[J]．中国无机分析化学，2018,8(6):58-63.MEI Yi. Determination of scandium, gallium,chromium,nickel and cobalt in vanadium-titanium blast furnace slag by inductively coupled plasma atomic emission spectrometry[J].Chinese Journal of Inorganic Analytical chemistry,2018,8(6):58-63.
[6]陈国成，黎应芬．火花直读光谱法测定铝及铝合金中的钒含量[J]．中国无机分析化学，2017,7(3):59-61.CHEN Guocheng, LI Yingfen. Determination of vandium content in aluminum and aluminum alloys by direct spark reading spectroscopy[J].Chinese Journal of Inorganic Analytical chemistry 2017,7(3):59-61.
[2]郝喜才，高敏杰，李洁．废钒催化剂回收技术研究进展[J]．开封大学学报，2017,31(2):74-78.HAO Xicai,GAO Minjie,LI Jie.Recycling technology of waste vanadium catalyst[J].Journal of Kaifeng University,2017,31(2):74-78.
[3]刘波，童庆云，李国良．氧化焙烧法回收废钒触媒中的钒[J]．四川大学学报（工程科学版），2002,34(2):112-115.LIU Bo,TONG Qingyun,LI Guoliang.Recovery of vanadium from waste vanadium catalyst by oxidation roasting[J].Journal of Sichuan University(Engineering Sicence Edition),2002,34(2):112-115.
[4]邵延海，冯其明，欧乐明，等．从废催化剂氨浸渣中综合回收钒和钼的研究[J]．稀有金属，2009,33(4):606-610.SHAO Yanhai,FENG Qiming,OU Leming,et al.Comprehensive recovery of vanadium and molybdenum from waste catalyst ammonia leaching residue[J].Chinese Journal of Rare Metals,2009,33(4):606-610.
[5]梅毅．电感耦合等离子体原子发射光谱测定钒钛高炉渣中钪镓铬镍钴[J]．中国无机分析化学，2018,8(6):58-63.MEI Yi. Determination of scandium, gallium,chromium,nickel and cobalt in vanadium-titanium blast furnace slag by inductively coupled plasma atomic emission spectrometry[J].Chinese Journal of Inorganic Analytical chemistry,2018,8(6):58-63.
[6]陈国成，黎应芬．火花直读光谱法测定铝及铝合金中的钒含量[J]．中国无机分析化学，2017,7(3):59-61.CHEN Guocheng, LI Yingfen. Determination of vandium content in aluminum and aluminum alloys by direct spark reading spectroscopy[J].Chinese Journal of Inorganic Analytical chemistry 2017,7(3):59-61.