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中国无机分析化学:2022,12(4):131-135
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碱熔-电感耦合等离子体原子发射光谱法测定废弃加氢脱硫(HDS)催化剂中的钒
张 琳, 韩 晓, 李华昌
(北矿检测技术有限公司)
Determination of vanadium in waste hydrodesulfurization (HDS) catalyst by Inductively coupled plasma atomic emission
ZHANG Lin, HAN Xiao, LI Huachang
(BGRIMM MTC Technology Co.,ltd.)
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投稿时间:2022-02-24    修订日期:2022-03-17
中文摘要: 本文建立了碱熔-电感耦合等离子体原子发射光谱法(ICP-OES)测定废弃加氢脱硫(HDS)催化剂中钒的方法,来协助加氢脱硫(HDS)催化剂回收实验的进行。试验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%,并选择钒292.401 nm为分析谱线。试验结果表明,为了消除基体效应的影响,需要使试液中钠元素、盐酸的含量和标准溶液中的钠元素、盐酸的含量相同。钒质量浓度在1.00-20.00 μg/mL时与发射强度呈线性关系,相关系数均为1。按照上述方法测定了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%-101%。该方法有效解决了废弃加氢脱硫(HDS)催化剂中钒测定的难题,可用于测定钒质量分数为0.50%-10.00%的HDS催化剂,同时对其他产品中钒的测定提供一种新思路。
Abstract: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. Sodium peroxide was used to melt the sample, 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 in order to eliminate the influence of matrix effect, it is necessary to make the content of sodium and hydrochloric acid in the test solution the same as that in the standard solution. The mass concentration of vanadium is 1.00-20.00 μ At g / ml, it has a linear relationship with the emission intensity, and the correlation coefficients are all 1. 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 recovery rate of standard addition is 99% - 101%. This method effectively solves the problem of vanadium determination in waste hydrodesulfurization (HDS) catalyst, and can be used to determine HDS catalyst with vanadium content of 0.50% - 10.00%. At the same time, it provides a new idea for the determination of vanadium in other products.
文章编号:     中图分类号:O657.31    文献标志码:
基金项目:十四五”国家重点研发计划国家质量基础设施体系专项(2021YFF0602602)
引用文本:
张 琳,韩 晓,李华昌.碱熔-电感耦合等离子体原子发射光谱法测定废弃加氢脱硫(HDS)催化剂中的钒[J].中国无机分析化学,2022,12(4):131-135.
ZHANG Lin,HAN Xiao,LI Huachang.Determination of vanadium in waste hydrodesulfurization (HDS) catalyst by Inductively coupled plasma atomic emission[J].Chinese Journal of Inorganic Analytical Chemistry,2022,12(4):131-135.

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