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作 者:廖奕鸥 单红飞[1] 赵素云[1] 倪雪梅[1] LIAO Yi-ou;SHAN Hong-fei;ZHAO Su-yun;NI Xue-mei(Shenyang Sanju Kaite Catalyst Co.,Ltd., Liaoning Shenyangll0144, China)
机构地区:[1]沈阳三聚凯特催化剂有限公司,辽宁沈阳110144
出 处:《当代化工》2019年第3期652-655,共4页Contemporary Chemical Industry
摘 要:选择使用微波消解仪法消解选择性加氢催化剂样品,结合电感耦合等离子体収射光谱仪(ICP-OES)测定选择性加氢催化剂中的Pt、Pd元素含量。系统考察了微波消解法消解样品条件,优化了电感耦合等离子体収射光谱仪(ICP-OES)的工作条件,采用内标校正标准工作曲线法,建立了ICP-OES法测定选择性催化剂中Pt、Pd元素含量的分析方法。结果表明,以8 mL硝酸和2 mL氢氟酸体系混合酸体系,微波消解法能够充分消解选择性加氢催化剂样品;测定选择性加氢催化剂中Pt含量:6.489~6.703 mg/L、Pd含量:14.85~15.31mg/L;相对标准偏差(RSD)分别为铂:1.216%、钯:1.217%;样品加标回收率分别为Pt:99.25%~101.26%、Pd:99.58%~102.24%。ICP-OES测定方法用于可以应用于选择性加氢催化剂中Pt、Pd元素含量的测定,分析快速,结果准确,已应用于生产分析中。The sample of selective hydrogenation catalyst was digested by microwave digestion, and the content of Pt and Pd in the selective hydrogenation catalyst was measured by inductively coupled plasma emission spectrometry(ICP-OES). The microwave digestion conditions of the sample was investigated, and the working conditions of the inductively coupled plasma emission spectrometer(ICP-OES) were optimized. The internal standard method was used to calibrate the standard working curve, an analytical method for the determination of Pt and Pd elements in selective catalysts by ICP-OES was established. The results showed that the microwave digestion method fully digested the selective hydrogenation catalyst sample by the mixed acid system of 8 mL nitric acid and 2 mL hydrofluoric acid;The determination result of Pt content was 6.489~6.703 mg/L, that of Pd content was 14.85~15.31 mg/L;The relative standard deviation(RSDs) were 1.216% for Pt,1.217% for Pd;recoveries of samples were 99.25%~101.26% for Pt,99.58~102.24% for Pd, respectively. ICP-OES method for determination of Pt and Pd in the selective hydrogenation catalyst is rapid, easy to master, so it can be used in production analysis.
关 键 词:铂、钯 电感耦合等离子体发射光谱仪 选择性加氢催化剂
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