Abstract:The content of gold in electronic wastes is high. The operation procedures in traditional analysis methods are complicated and time-consuming. Moreover, these methods usually require high technical skills. In experiments, certain amount of gold-containing electronic wastes was dissolved with aqua regia. The solution was transferred into 100mL volumetric flask and then diluted to the mark. According to the content of gold, certain volume of sample solution was transferred into beaker. The acidity was maintained in range of 5%-30%. And 1.5g of activated carbon was added for static adsorption. Then the activated carbon was mixed uniformly with microcrystalline cellulose in mass ratio of 1∶1. The content of gold was determined by X-ray fluorescence spectrometry (XRF) with pressed powder pellet. The activated carbon adsorption realized the separation of gold from a large amount of matrix materials in electronic wastes. The specimen matrix for analysis was mainly composed of activated carbon and microcrystalline cellulose. In other words, the composition of specimen matrix for analysis prepared from different samples was basically same. The matrix effect was further corrected using spectral background of gold as internal standard. The spectral interference was eliminated by selecting Au-Lα line, Ge crystal and proper PHA range. The detection limit was 5μg. The precision tests were conducted using three electronic waste samples with different gold contents. The relative standard deviations (RSD, n=12) of determination results were between 1.3% and 2.0%. The analysis results of electronic waste samples were basically consistent with those obtained by hydroquinone titration method. The complicated manual operations such as high-temperature ashing and titration in wet chemical method were avoided in experiments. The proposed method was applicable for the determination of gold in electronic wastes with content in range of 0.x-xx.x g/kg.
陈永红,孟宪伟,苏广东,等.2013—2014年中国金分析测定的进展[J].黄金,2016,37(1):79-84.CHEN Yong-hong,MENG Xian-wei,SU Guang-dong,et al.Progress of gold determination and analysis technology in China,2013 and 2014[J].Gold,2016,37(1):79-84.
[2]
殷保稳,秦士跃,张亦飞,等.从电子废弃物中回收贵金属的方法概述[J].现代化工,2014,34(6):5-9.YIN Bao-wen,QIN Shi-yue,ZHANG Yi-fei,et al.Overview on recovery of precious metals from electronic waste[J].Modern Chemical Industry,2014,34(6):5-9.
[3]
魏金秀,汪永辉,李登新.国内外电子废弃物现状及其资源化技术[J].东华大学学报:自然科学版,2005,31(3):133-138.WEI Jin-xiu,WANG Yong-hui,LI Deng-xin.The current status of the electronic waste and it′s recycling technique home and abroad[J].Journal of Donghua University:Natural Science,2005,31(3):133-138.
[4]
王永乐.电子废弃物中复杂体系贵金属的分析方法研究[D].上海:东华大学,2016.
[5]
Luis A Diaz,Tedd E Lister,Jacob A Parkman,et al.Comprehensive process for the recovery of value and critical materials from electronic waste[J].Journal of Cleaner Production,2016,125(1):236-244.
[6]
李跃光,陈为亮.贵金属元素分析中的分离富集技术应用进展[J].贵金属,2012,33(4):71-74.LI Yue-guang,CHEN Wei-liang.Comments on technical progress of separation and concentration for precious metals elemental analysis[J].Precious Metals,2012,33(4):71-74.
[7]
张志刚,刘凯,陈泓,等.酒石酸络合掩蔽锑-氢醌容量法测定锑矿石样品中的常量金[J].岩矿测试,2015,34(4):454-458.ZHANG Zhi-gang,LIU Kai,CHEN Hong,et al.Determination of gold in antimony ores by hydroquinone volumetric method with antimony tartrate as complexing and masking agent[J].Rock and Mineral Analysis,2015,34(4):454-458.
[8]
班俊生,郑晓钟,任金鑫,等.磷酸三丁酯醋酸纤维富集氢醌滴定法测定氰化液中的金[J].黄金,2008,29(6):59-60.BAN Jun-sheng,ZHENG Xiao-zhong,REN Jin-xin,et al.Determination of Au in cyanide solution by the hydrogen quinone after enriched with tribubyl phosphate-acetic cellulose[J].Gold,2008,29(6):59-60.
[9]
付文慧,艾兆春,葛艳梅,等.火焰原子吸收光谱法测定高品位金矿石中的金[J].岩矿测试,2013,32(3):427-430.FU Wen-hui,AI Zhao-chun,GE Yan-mei,et al.Determination of Au in high grade gold deposits by flame atomic absorption spectrometry[J].Rock and Mineral Analysis,2013,32(3):427-430.
[10]
葛艳梅.王水溶样-火焰原子吸收光谱法直接测定高品位金矿石的金量[J].岩矿测试,2014,33(4):491-496.GE Yan-mei.Direct determination of high grade gold in ore by flame atomic absorption spectrometry with aqua regia sampling preparation[J].Rock and Mineral Analysis,2014,33(4):491-496.
[11]
何小辉,白金峰,陈卫明,等.流动注射-火焰原子吸收光谱法测定地质样品中的常量金[J].岩矿测试,2011,30(1):79-82.HE Xiao-hui,BAI Jin-feng,CHEN Wei-ming,et al.Determination of gold in geological samples by flow injection-flame atomic absorption spectrometry[J].Rock and Mineral Analysis,2011,30(1):79-82.
[12]
夏珍珠.火焰原子吸收光谱法测定载金炭中金[J].黄金,2012,33(4):52-54.XIA Zhen-zhu.Determination of gold in gold-loaded carbon by flame atomic absorption spectrometry[J].Gold,2012,33(4):52-54.
[13]
何炼,肖刚.火试金富集-重量法测定冰铜中金[J].冶金分析,2013,33(3):69-72.HE Lian,XIAO Gang.Determination of gold in matte by fire assaying enrichment-gravimetric method[J].Metallurgical Analysis,2013,33(3):69-72.
[14]
马丽军,陈永红,腾飞,等.火试金重量法测定载金炭中的金量[J].黄金,2013,34(11):69-71.MA Li-jun,CHEN Yong-hong,TENG Fei,et al.Determination of gold in matte by fire assaying enrichment-gravimetric method[J].Gold,2013,34(11):69-71.
[15]
王芳,陈小兰.印刷线路板中金的检测[J].黄金,2014,35(7):80-82.WANG Fang,CHEN Xiao-lan.Determination of gold in printed circuit board scraps[J].Gold,2014,35(7):80-82.
[16]
尹明,李家熙.岩石矿物分析:第3分册[M].北京:地质出版社,2011:614-637.
[17]
罗立强,詹秀春,李国会.X射线荧光光谱分析[M].北京:化学工业出版社,2015.
[18]
陈静,高志军,陈冲科,等.X射线荧光光谱法分析地质样品的应用技巧[J].岩矿测试,2015,34(1):91-98.CHEN Jing,GAO Zhi-jun,CHEN Chong-ke,et al.Application skills on determination of geological sample by X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,2015,34(1):91-98.
[19]
于波,严志远,杨乐山,等.X射线荧光光谱法测定土壤和水系沉积物中碳和氮等36个主次痕量元素[J].岩矿测试,2006,25(1):74-78.YU Bo,YAN Zhi-yuan,YANG Le-shan,et al.Determination of 36 major,minor and trace elements in soil and stream sediment samples by X-ray fluorescence spectrometry[J]. Rock and Mineral Analysis,2006,25(1):74-78.