铋试金富集检测废汽车尾气催化剂中的钯

引用本文: 张福元, 张广安, 徐娟, 赵卓, 徐亮. 铋试金富集检测废汽车尾气催化剂中的钯[J]. 分析化学, 2020, 48(11): 1590-1596. doi: 10.19756/j.issn.0253-3820.191520 shu

Citation: ZHANG Fu-Yuan, ZHANG Guang-An, XU Juan, ZHAO Zhuo, XU Liang. Determination of Palladium in Spent Automobile Exhaust Catalysts by Bismuth Fire Assay Preconcentration[J]. Chinese Journal of Analytical Chemistry, 2020, 48(11): 1590-1596. doi: 10.19756/j.issn.0253-3820.191520 shu

铋试金富集检测废汽车尾气催化剂中的钯

安徽工业大学冶金工程学院, 马鞍山 243032

通讯作者: 张福元,sanzhfy@163.com

基金项目:
本文系国家自然科学基金项目（Nos.U1703130，51904003）和安徽省重点实验室开发基金项目（No.SKF18-01）资助

摘要: 建立了金属铋作为捕集剂的试金方法，用于废汽车尾气催化剂中铂族金属钯的检测。分析了铋试金选择性造渣的过程，讨论了铋捕集贵金属的热力学机理，分析了铋试金过程金属氧化物的还原顺序，考察了影响铋试金结果的主要因素。贵金属氧化物均优先于Bi₂O₃被还原，Bi₂O₃优先于TeO₂、Cu₂O、As₂O₃、PbO、NiO等杂质被还原，Bi₂O₃具有较强排除Te、Cu、As、Ni等多种杂质的能力，贵金属单质分散在金属铋相，较分散在熔渣相更能降低体系自由能。配料为48.00 g Bi₂O₃、25.00 g无水Na₂CO₃、5.5 g面粉、硅硼质量比为1：1、控制熔渣硅酸度为1.1，20 min内马弗炉温度由900℃升至1080℃，并保温25 min，金属铋质量为40 g，钯的测定结果均值为2852 g/t，极差值为17 g/t，RSD仅为0.2%。建立的铋试金方法与国标中的分光光度法相比，结果准确，精密度高，误差小于国标要求的误差范围。

关键词:

English

Determination of Palladium in Spent Automobile Exhaust Catalysts by Bismuth Fire Assay Preconcentration

School of Metallurgical Engineering, Anhui University of Technology, Ma'anshan 243032, China

Corresponding author: ZHANG Fu-Yuan, sanzhfy@163.com

Received Date: 26 August 2019
Revised Date: 28 August 2020
Fund Project:
This work was supported by the National Natural Science Foundation of China (Nos. U1703130, 51904003) and the Anhui Province Key Laboratory of Metallurgy Engineering & Resources Recycling (No. SKF18-01).

Abstract: A new method for accurate detection of platium group metals in spent automobile exhaust catalysts samples by inductively coupled plasma spectrometry (ICP-OES) combined with fire assay enrichment through green metal bismuth was established. In this work, the ability of selective slag forming in bismuth fire assay was analyzed, the thermodynamic mechanism from the micro level of bismuth concentrate precious metals was revealed, the order of metal reduced in bismuth fire assay was discussed, and the main factors affecting the results of bismuth fire assay were investigated. The result showed that precious metal oxides were reduced prior to Bi₂O₃, Bi₂O₃ was reduced prior to TeO₂, Cu₂O, As₂O₃, PbO, NiO and other impurities, and Bi₂O₃ had a stronger ability to remove impurities such as Te, Cu, As and Ni. Precious metal elements dissolved in metallic bismuth phase could reduce the free energy of the system more than dissolved in slag phase. Each of the samples or above-mentioned powder were mixed with flux and collectors proportionately, such as 48.00 g of bismuth trioxide, 25.00 g of sodium carbonate anhydrous, 5.5 g of wheat flour, slag silicate degree of 1.1, and 1:1 mass ratio of silicon to boron. The mixture was transferred into fire-clay crucibles and fused at the temperature range from 900℃ to 1080℃ in 20 min, and maintained at 1080℃ for 25 min. The quality of bismuth button was 40 g. The average detection value of palladium was 2852 g/t, the extreme difference was 17 g/t with relative standard deviation of 0.21%. The bismuth fire assay for detection of platinum group metals had higher precision and recovery, and the detection error was less than the error range of national standard.

Key words:

1. [1]
  Chaudhari N K, Joo J, Kwon H, Kim B, Kim H Y, Joo S H, Lee K. Nano Res.,2018,11(12):6111-6140
2. [2]
  Binder A J, Toops T J, Parks J E. ChemcatChem,2018,10(6):1263-1266
3. [3]
  LI Peng-Yuan, ZHOU Ping, QI Ya-Bin, TANG Jin-Rong, ZHANG Shou-Ting. Geol. Bull. China,2017,36(4):676-683 李鹏远, 周平, 齐亚彬, 唐金荣, 张寿庭.地质通报,2017,36(4):676-684
4. [4]
  Kuchekar1 S R, Bhumkar S D, Aher H R. J. Mater. Environ. Sci.,2019,10(4):316-327
5. [5]
  GB/T 23277-2009, Chemical Analysis Methods of Catalysts Containing Precious Metals-Determination of Platinum, Palladium and Rhodium in Automobile Exhaust-Purifying Catalysts-Spectrophotometry. National Standards of the People's Republic of China贵金属催化剂化学分析方法汽车尾气净化催化剂中铂、钯、铑量的测定分光光度法.中华人民共和国国家标准. GB/T 23277-2009
6. [6]
  Volzhenin A V, Petrova N I, Medvedev N S, Saprykin A I. Microchem. J.,2018,138:390-394
7. [7]
  Yildiz Y, Kotb M, Hussein A, Sayedahmed M, Rachid M, Cheem M. Am. J. Anal. Chem,2019,10:127-136
8. [8]
  GUAN You-Xiang, XU Guang, WANG Ying-Jin, WU Xiao-Feng, LIU Xia, ZHU Li-Ya, LIU Yun-Jie, MA Yuan, AN Zhong-Qing, GAN Jian-Zhuang. Precious Metals,2011,32(2):67-71 管有祥, 徐光, 王应进, 吴晓峰, 刘霞, 朱利亚, 刘云杰, 马媛, 安中庆, 甘建壮.贵金属,2011,32(2):67-71
9. [9]
  ZHAO Jia-Chun, CUI Hao, BAO Si-Min, TONG Wei-Feng, DONG Hai-Gang. Precious Metals,2018,39(1):56-59 赵家春, 崔浩, 保思敏, 童伟锋, 董海刚.贵金属,2018,39(1):56-59
10. [10]
  XU Kai-Hua, ZHOU Ji-Feng. China Patent, 201611069175.3,2016 许开华, 周继峰.中国专利, 201611069175.3,2016
11. [11]
  LI Ke-Ji, LIU Shu-Jun, SHAO Kun.Chinese J. Anal. Chem.,2014,42(6):909-912 李可及, 刘淑君, 邵坤.分析化学,2014,42(6):909-912
12. [12]
  Ni W S, Mao X J, Zhang H L. Anal. Lett.,2019,52(11):1699-1710
13. [13]
  Ni W S, Zhang H L, Mao X J, Liu L, Xiao F. Microchem. J.,2019,150:104187
14. [14]
  ZHAO Ling-Hao, ZHAN Xiu-Chun, HU Ming-Yue, SUN Dong-Yang, FAN Chen-Zi, YUAN Ji-Hai, KUAI Li-Jun, QU Wen-Jun. Rock Min. Anal.,2013,32(5):694-701 赵令浩, 詹秀春, 胡明月, 孙冬阳, 范晨子, 袁继海, 蒯丽君, 屈文俊.岩矿测试,2013,32(5):694-701
15. [15]
  XIA Bing-Wei. Chinese J. Inorg. Anal. chem.,2015,5(1):49-52 夏兵伟.中国无机分析化学,2015,5(1):49-52
16. [16]
  LI Ke-Ji, ZHAO Chao-Hui, FAN Jian-Xiong. Metall. Anal.,2013,33(8):19-23 李可及, 赵朝辉, 范建雄.冶金分析,2013,33(8):19-23
17. [17]
  CHEN Jing. Eng. Sci.,2007,9(5):11-16 陈景.中国工程科学,2007,9(5):11-16

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

铋试金富集检测废汽车尾气催化剂中的钯

通讯作者: 张福元,sanzhfy@163.com

English

Determination of Palladium in Spent Automobile Exhaust Catalysts by Bismuth Fire Assay Preconcentration

Corresponding author: ZHANG Fu-Yuan, sanzhfy@163.com

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

铋试金富集检测废汽车尾气催化剂中的钯

通讯作者: 张福元,sanzhfy@163.com

English

Determination of Palladium in Spent Automobile Exhaust Catalysts by Bismuth Fire Assay Preconcentration

Corresponding author: ZHANG Fu-Yuan, sanzhfy@163.com

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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