石油炼制与化工 ›› 2024, Vol. 55 ›› Issue (6): 164-171.

• 分析与评定 • 上一篇    下一篇

单一酸密闭消解-电感耦合等离子体法测定催化剂中Pt、Pd含量

李明哲,周勇,杨彦鹏,王子健,王涛,聂骥,赖婷婷,谢莉,王杰广   

  1. 中石化石油化工科学研究院有限公司
  • 收稿日期:2023-07-11 修回日期:2024-03-01 出版日期:2024-06-12 发布日期:2024-05-28
  • 通讯作者: 谢莉 E-mail:xieli@ripp-sinopec.com
  • 基金资助:
    氧化铝的规模化制备技术及工业示范应用

DETERMINATION OF PLATINUM AND PALLADIUM CONTENT IN CATALYST BY ICP-OES


  • Received:2023-07-11 Revised:2024-03-01 Online:2024-06-12 Published:2024-05-28

摘要: 建立了单一酸密闭消解-电感耦合等离子体发射光谱(ICP-OES)分析方法,测定催化重整(简称重整)生成油脱烯烃催化剂中的Pt、Pd含量。研究了前处理和消解条件对催化剂消解的影响,对比了单一酸消解法和常规混合酸消解法的消解效果,系统讨论了Pt和Pd分析谱线选择依据、Al基体对测定元素影响的原因、杂质元素和Pt、Pd元素间干扰对测定结果的影响。确定了单一酸消解的前处理和消解条件为:在空气气氛下,将催化剂样品于550 ℃灼烧4 h后研磨至粒径120 μm以下;称取样品0.2g,加3 mL浓盐酸,在密闭消解罐内于180℃消解6 h。所建立的方法与常规混合酸消解法相比,简便快捷,结果准确,同时还具有用酸量少、对实验人员和环境友好的优点,可应用于重整生成油脱烯烃催化剂中Pt质量浓度为2.08~12500μg/g、Pd质量浓度为2.67~12500 μg/g范围内Pt、Pd含量的精准测定。

关键词: 电感耦合等离子体发射光谱, 脱烯烃, 催化剂, 单一酸, 铂,

Abstract: A novel method was developed to determine platinum and palladium content in industrial reforming oil decolefin catalyst under single acid closed digestion condition by ICP-OES. The effects of pretreatment and digestion conditions on the digestion of catalyst were investigated, and the digestion effects of the single acid digestion and conventional mixed acid digestion were compared. Additionally, this study systematically discussed the selection basis for spectral lines used in platinum and palladium analysis, as the influence of aluminum matrix on measured elements, impact of impurity elements, and interference between Pt and Pd elements results. The pre-treatment and digestion conditions for single acid were determined as follows: the catalyst samplewas burned at 550 ℃ for 4 h in air atmosphere and ground to a particle size of less than 120 μm; 0.2 g samples and 3 mL concentrated hydrochloric acid were added and digested in an airtight digestion tank at 180 ℃ for 6 h. Compared with the conventional mixed acid digestion method, the established method is simple, rapid and accurate, and has the advantages of less acid consumption,being friendly to laboratory personnel and environment. The method can be applied to the accurate determination of Pt and Pd in the range of 2.08-12 500 μg/g Pt and 2.67-12 500 μg/g Pd in the catalysts utilized in industrial reforming.

Key words: ICP-OES, deolefin, catalyst, simple acid, platinum, palladium