ICP-OES同时测定废铝基催化剂中镍、钼、钒、钴  

Determination of Ni, Mo, V and Co in Spent Aluminum-based Catalyst by ICP-OES

作　　者：黎俏 余淑媛 高欣 许铮 冯均利 唐梦奇 LI Qiao;YU Shu-Yuan;GAO Xin;XU Zheng;FENG Jun-Li;TANG Meng-Qi(Nanning Customs Technology Centre,Nanning 530021;The Testing and Technology Center for Industrial Products,Shenzhen Customs,Shenzhen 518067;Science and Technology Research Center of China Customs,Beijing 100094)

机构地区：[1]南宁海关技术中心,南宁530021 [2]深圳海关工业品检测技术中心,深圳518067 [3]中国海关科学技术研究中心,北京100094

出　　处：《中国口岸科学技术》2021年第11期36-40,共5页China Port Science and Technology

基　　金：国家重点研发计划课题(2019YFC1904802);海关总署科研项目(2019HK013、2020HK256)。

摘　　要：废铝基催化剂中Ni、Co、V、Mo的定量分析,有助于评估其综合回收利用价值。本文采用氢氧化钠焙烧和硫酸浸出相结合的方式,将废铝基催化剂与氢氧化钠按质量比1:1.8混合,900℃焙烧2 h,再以4 mol/L硫酸于80℃条件下浸取1 h,最后用电感耦合等离子体发射光谱法(ICP-OES)同时测定浸取液中Ni、Co、V、Mo的含量,探讨了前处理最佳的消解方法,分析了仪器常用波长之间的差异。结果表明,Ni、Co、V、Mo曲线的相关系数在0.9997~0.9999之间;配制与样品基体一致的溶液进行11次空白测定,其检出限为0.0112~0.128 mg/L;对实际样品进行6次平行测定,其精密度为0.31%~0.50%;对3个水平实际样品加标,回收率为96.5%~102.2%。The quantitative analysis of Ni, Co, V and Mo in spent aluminum catalyst is helpful to evaluate the value of its comprehensive recovery and utilization. In this paper, the method of soda calcination and sulfuric acid leaching is adopted. The spent Al-based catalyst was mixed with soda ash at the mass ratio of 1:1.8, claimed at 900℃ for 2 h, and then leached at 80℃ with 4 mol/L sulfuric acid for 1 h. Finally, the contents of Ni, Co, V and Mo in the leaching solution were determined by inductively coupled plasma emission spectrometry(ICP-OES) simultaneously. In this work, the best digestion method of pretreatment was discussed, and the differences of the wavelengths in common use were analyzed. The experimental results showed that the correlation coefficients of Ni, Co, V and Mo curves range from 0.9997 to 0.9999. The solution consistent with the sample matrix was prepared for 11 blank tests, and the detection limit was between 0.0112 mg/L and 0.128 mg/L. The precision of the actual samples was 0.31%-0.50% after 6 times of parallel determination. Three levels of standard addition tests were carried out on the actual samples, and the recovery was 96.5%-102.2%.

关 键 词：ICP-OES 废催化剂 镍 钼 钒 钴 同时测定 

分 类 号：X833[环境科学与工程—环境工程] O657.31[理学—分析化学]