Abstract:The accurate determination of precious metal palladium in waste motors is of great significance to the comprehensive recycling of waste motors. The content of palladium in the waste motor is relatively low, and it also contains a large amount of copper. If the content of palladium is directly determined after acid dissolution, the matrix interference will be serious. In experiments, the lead fire assaying method was used for the separation and enrichment of palladium in waste motor samples. The method for determination of palladium in waste motors by flame atomic absorption spectrometry (FAAS) was established using air-acetylene flame. The determination wavelength was 247.6 nm.The amount of lead oxide, the cupellation temperature, and the measurement medium were optimized: the amount of lead oxide was 200 g, the cupellation temperature was 900 ℃, and the measurement medium was 10% (volume fraction) hydrochloric acid. The interference tests showed that the single presence or coexistence of lead, bismuth, tellurium and silver in sample will not affect the determination of palladium. The linear range of calibration curve was 1.00-4.00 μg/mL, and the correlation coefficient was 0.999 92. The limit of detection was 0.051 8 μg/mL, and the limit of quantification was 0.173 μg/mL. The content of palladium in waste motor was determined according to the experimental method, and the found results were basically consistent with those obtained by inductively coupled plasma atomic emission spectroscopy (ICP-AES). The relative standard deviations (RSD, n=7) were between 2.2% and 3.1%, and the recoveries were between 98% and 102%.
刘秋波, 王皓莹, 康羽. 铅试金-火焰原子吸收光谱法测定废旧电机中钯[J]. 冶金分析, 2022, 42(7): 26-31.
LIU Qiubo, WANG Haoying, KANG Yu. Determination of palladium in waste motor by flame atomic absorption spectrometry with lead fire assay. , 2022, 42(7): 26-31.
[1] 陆雪祥.废旧电器拆解新工艺的应用及成效分析[J].再生资源与循环经济,2014,7(8):37-39. LU Xuexiang.Analysis on the application and effects of scrambling technology of waste electronic appliances[J].Recyclable Resources and Circular Economy,2014,7(8):37-39. [2] 袁鹏程.火试金富集ICP-AES测定铜冶炼烟灰中铂和钯量[J].有色冶金设计与研究,2017,38(3):21-23. YUAN Pengcheng.Determination of platinum and palladium in the copper smelting soot by fire assay enrichment-ICP-AES[J].Nonferrous Metals Engineering & Research,2017,38(3):21-23. [3] 汤淑芳.电感耦合等离子体原子发射光谱法(ICP-AES)测定黑铜中铂、钯含量[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2013,3(suppl.1):86-88. [4] 北京矿冶研究总院分析室编委会.矿石及有色金属分析手册[M].北京:冶金工业出版社,1990:197-201. [5] 侯君钊,张圣欢,闫爽,等.钯含量分析方法研究进展[J].化学计量分析,2021,30(12):89-94. HOU Junzhao,ZHANG Shenghuan,YAN Shuang,et al.A research progress of analysis methods for contents of palladium[J].Chemical Analysis and Meterage,2021,30(12):89-94. [6] 邵坤,范建雄,李刚,等.铅试金-电感耦合等离子体原子发射光谱法测定高镍锍中金铂钯[J].冶金分析,2021,41(10):49-56. SHAO Kun,FAN Jianxiong,LI Gang,et al.Determination of gold,platinum and palladium in high nickel matte by inductively coupled plasma atomic emission spectrometry with lead fire assay[J].Metallurgical Analysis,2021,41(10):49-56. [7] 陈丽梅,陈兰,罗正波,等.火试金-电感耦合等离子体原子发射光谱法测定提钯螯合剂中残余钯[J].冶金分析,2018,38(8):58-62. CHEN Limei,CHEN Lan,LUO Zhengbo,et al.Determination of residual palladium in palladium chelating agent by inductively coupled plasma atomic emission spectrometry after fire assaying[J].Metallurgical Analysis,2018,38(8):58-62. [8] 史博洋,王皓莹,谢大伟.火试金富集-电感耦合等离子体发射光谱(ICP-OES)法测定分银渣中的铂、钯[J].中国无机分析化学,2018,8(1):53-56. SHI Boyang,WANG Haoying,XIE Dawei.Determination of platinum and palladium content in sub-silver by ICP-OES with fire assay preconcentration[J].Chinese Journal of Inorganic Analytical Chemistry,2018,8(1):53-56. [9] 赵伟,尤雅婷,徐松,等.火试金富集-电感耦合等离子体质谱法测定铜精矿中金钯铂[J].冶金分析,2011,31(10):41-45. ZHAO Wei,YOU Yating,XU Song,et al.Determination of gold,palladium and platinum in copper concentrates by inductively coupled plasma mass spectrometry combined with fire assay preconcentration[J].Metallurgical Analysis,2011,31(10):41-45. [10] 胡秋芬,郭红,黄齐林,等.固相萃取-火焰原子吸收光谱法测定金[J].理化检验(化学分册),2009,45(5):561-563. HU Qiufen,GUO Hong,HUANG Qilin,et al.Determination of gold by flame atomic absorption spectrometry with solid phase extraction[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2009,45(5):561-563. [11] 程晓娟.石墨炉原子吸收光谱法测定铁矿石中痕量铅[J].冶金分析,2016,36(12):50-54. CHENG Xiaojuan.Determination of trace lead in iron ore by graphite furnace atomic absorption spectrometry[J].Metallurgical Analysis,2016,36(12):50-54. [12] 姚明星,毛香菊,孙启亮,等.铅试金-石墨炉原子吸收光谱法测定铂钯矿浸出液中铂和钯[J].冶金分析,2021,41(9):34-40. YAO Mingxing,MAO Xiangju,SUN Qiliang,et al.Determination of platinum and palladium in leaching solution of platinum-palladium ore by graphite furnace atomic absorption spectrometry after the preconcentration with lead fire assay[J].Metallurgical Analysis,2021,41(9):34-40. [13] 魏巍.铅试金重量法结合原子吸收光谱法测定银钯精矿中银[J].冶金分析,2018,38(1):64-69. WEI Wei.Determination of silver in silver-palladium concentrate by lead fire assaying gravimetry combined with atomic absorption spectrometry[J].Metallurgical Analysis,2018,38(1):64-69. [14] 杨新周,杨子仙,胡秋芬,等.钯分离富集方法研究进展[J].云南化工,2013,40(1):30-35. YANG Xinzhou,YANG Zixian,HU Qiufen,et al.The latest advance in methods of separation and enrichment of palladium[J].Yunnan Chemical Technology,2013,40(1):30-35. [15] 林海山.火试金法测定粗铜中金和钯[J].冶金分析,2002,22(1):53-56. LIN Haishan.Determination of gold and palladium in crude copper by fire-assaying method[J].Metallurgical Analysis,2002,22(1):53-56. [16] 夏珍珠.火试金重量法测定载金炭中银[J].冶金分析,2017,37(2):54-58. XIA Zhenzhu.Determination of silver in gold-loaded carbon by fire assay gravimetric method[J].Metallurgical Analysis,2017,37(2):54-58. [17] 王豪,蹇瑞红,刘维桥,等.铜阳极泥脱铜渣中金、银、钯含量测定[J].化工进展,2018,37(7):2854-2859. WANG Hao,JIAN Ruihong,LIU Weiqiao,et al.Determination of gold,silver and palladium in copper anode low grade copper slag[J].Chemical Industry and Engineering Progress,2018,37(7):2854-2859.