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首页> 中文期刊> 《冶金分析》 >电感耦合等离子体原子发射光谱法测定铂铼废催化剂中铼

电感耦合等离子体原子发射光谱法测定铂铼废催化剂中铼

         
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摘要

The carbon,sulfur and organic matters in platinum rhenium spent catalyst could be removed by high temperature ignition.However,the volatilization loss of rhenium was also serious.According to the principle that the carbon,sulfur and organic matters could be removed by perchloric acid fuming w hile the rhenium was not volatilized when the temperature was less than 300 ℃,the sample was digested by nitric acid and perchloric acid in this study.The determination method of rhenium in platinum rhenium spent cat-alyst by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.The follow-ing experimental conditions were obtained:the amount of sample was 0.15g;2.0mL of nitric acid and 1.0 mL of perchloric acid were added followed by fuming at 260-290 ℃;then 2.0 mL of nitric acid was add-ed and the solution was heated until fume just appeared;the operation was repeated for twice until the sample solution was clear;10.0 mL of hydrochloric acid was added;the solution was transferred into 100 mL volumetric flask and diluted to the mark;the content of rhenium was determined by ICP-AES using Re 221.426 nm as the analytical line.The coexisting ions including aluminum(III),platinum(IV)and iron(III)had no interference with the determination.The proposed method was applied for the determina-tion of rhenium(639.4-5854.8 g/t)in one test sample and four actual samples of platinum rhenium spent catalyst.The determination value of test sample was basically consistent with the recommended value.The relative standard deviations(RSD,n=11)of determination results were between 0.17% and 0.63%,and the spiked recoveries were between 98.8% and 100.3%.%采用高温灼烧可除去铂铼废催化剂中碳、硫和有机物,但铼挥发损失严重.根据小于300 ℃时,高氯酸冒烟可除去碳、硫和有机物且铼基本不挥发损失这一原理,建立了采用硝酸-高氯酸消解样品,电感耦合等离子体原子发射光谱法(ICP-AES)测定铂铼废催化剂中铼的方法.确定的实验条件为:样品量为0.15 g,加入2.0 m L 硝酸、1.0 m L高氯酸,260~290 ℃加热至刚冒烟;再加入2.0 mL硝酸,加热至刚冒烟;重复2次至试液清亮;加入10.0 mL盐酸,转入100 mL容量瓶中,定容摇匀,于分析线Re 221.426 nm处,ICP-AES测定铼.铝(Ⅲ)、铂(Ⅳ)、铁(Ⅲ)等共存离子不干扰测定.将实验方法用于1个铂铼废催化剂试验样品、4个铂铼废催化剂实际样品中铼(639.4~5854.8 g/t)的测定,试验样品的测定值与推荐值基本一致,结果的相对标准偏差(n=11)为0.17% ~0.63%,加标回收率为98.8% ~100.3%.

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  • 来源
    《冶金分析》 |2018年第2期|47-52|共6页
  • 作者

    马王蕊; 刘文; 张选冬; 罗仙; 崇彪; 韩守礼;

  • 作者单位

    贵研资源(易门)有限公司,贵研铂业股份有限公司稀贵金属综合利用新技术国家重点实验室,云南昆明650106;

    贵研资源(易门)有限公司,贵研铂业股份有限公司稀贵金属综合利用新技术国家重点实验室,云南昆明650106;

    贵研资源(易门)有限公司,贵研铂业股份有限公司稀贵金属综合利用新技术国家重点实验室,云南昆明650106;

    贵研资源(易门)有限公司,贵研铂业股份有限公司稀贵金属综合利用新技术国家重点实验室,云南昆明650106;

    贵研资源(易门)有限公司,贵研铂业股份有限公司稀贵金属综合利用新技术国家重点实验室,云南昆明650106;

    贵研资源(易门)有限公司,贵研铂业股份有限公司稀贵金属综合利用新技术国家重点实验室,云南昆明650106;

  • 原文格式 PDF
  • 正文语种 chi
  • 中图分类
  • 关键词

    铂铼废催化剂; 铼; 电感耦合等离子体原子发射光谱法(ICP-AES);

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