碱熔-电感耦合等离子体原子发射光谱(ICP-AES)法测定废弃加氢脱硫(HDS)催化剂中的钒

Determination of Vanadium in Waste Hydrodesulfurization(HDS)Catalyst by Inductively Coupled Plasma Atomic Emission Spectrometry

为对加氢脱硫(HDS)催化剂中重金属元素进行回收,建立了碱熔-电感耦合等离子体原子发射光谱(ICP-AES)法测定废弃加氢脱硫(HDS)催化剂中钒的方法。采用过氧化钠熔解试样,用盐酸浸取后定容,稀释试液后控制盐酸酸度为10%,使用基体匹配法并选择钒292.401 nm为分析谱线进行测定。结果表明,钒质量浓度在1.00~20.00μg/mL时与发射强度呈线性关系,相关系数为1.0。测定了5个废弃加氢脱硫(HDS)催化剂样品中的钒,并采用格拉布斯检验方法检验11次,测定结果无异常值,加标回收率为99.0%~101%。方法可用于测定钒质量分数为0.50%~10.0%的HDS催化剂,同时对其他产品中钒的测定提供一种新思路。

A method for the determination of vanadium in waste hydrodesulfurization(HDS)catalyst by alkali fusion inductively coupled plasma atomic emission spectrometry(ICP-OES)was established to assist in the recovery experiment of HDS catalyst.Samples were digested by sodium peroxide,the volume was fixed after leaching with hydrochloric acid,the acidity of hydrochloric acid was controlled to 10%after diluting the test solution,and vanadium 292.401 nm was selected as the analytical spectral line.The test results show that,it is necessary to make the content of sodium and hydrochloric acid in the test solution the same as that in the standard solution for eliminating the influence of matrix effect.Correlation coefficient of vanadium is 1.0 when the linearity range of vanadium is in the range of 1.00-20.00μg/mL.Vanadium in five waste HDS catalyst samples was determined according to the above method,and tested 11 times by grubs test method.The determination results have no abnormal value,and the recoveries of vanadium in sample are 99.0%-101%.This method effectively solves the problem of vanadium determination in waste hydrodesulfurization(HDS)catalyst,and can be used to determine HDS catalyst with the content of vanadium from 0.50%to 10.0%.At the same time,it provides a new idea for the determination of vanadium in other products.