铜阳极泥脱铜渣中金、银、钯含量测定
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摘要
建立了连续测定铜阳极泥脱铜渣中金、银、钯含量的分析方法,并与火试金法进行比较。首先,利用硝酸+乙二胺四乙酸(EDTA)+酒石酸消解铜阳极泥脱铜渣,得到含有银、钯和少量金的消解液,考察了硝酸、EDTA和酒石酸用量对消解效果的影响。结果表明,硝酸、EDTA和酒石酸用量分别为30m L、3m L、1.5g时,消解效果最好。然后,利用王水对残渣进行二次消解,得到含有金和少量银、钯的消解液,考察了王水用量对消解效果的影响。结果表明,王水用量为15m L时即可完成消解。最后采用火焰原子吸收光谱仪测定消解液中的金、银、钯含量。采用本方法测定铜阳极泥脱铜渣,Au、Ag、Pd各元素相对标准偏差均小于1%(n=10),加标回收率在95.57%~98.70%之间,实验结果准确可靠、重现性好,与火试金法测定结果相一致。
The method of continuous determination of gold,silver and palladium in copper anode low grade copper slag was established and compared with the fire test method. First,the copper anode low grade copper slag was digested with nitric acid+EDTA+tartaric acid to obtain a digestion solution containing silver,palladium and a small amount of gold. The effects of nitric acid,EDTA and tartaric acid dosage on digestion were investigated. The results showed that the digestion was the best when the dosage of nitric acid,EDTA and tartaric acid were 30 m L,3 m L and 1.5 g,respectively. Then,the residue was subjected to secondary digestion with aqua regia to obtain a digestion solution containing gold and a small amount of silver and palladium. The effects of aqua regia dosage on digestion were investigated. The results showed that the amount of aqua regia required to complete the digestion was 15 m L. Finally,the contents of gold,silver and palladium in digestion solution were determined by flame atomic absorption spectrometer. The relative standard deviations of Au,Ag and Pd in the copper anode low grade copper slag were less than 1%(n=10),and the recoveries were between 95.57% and 98.70% by this method. The experimental results are accurate,reliable and reproducible,which is consistent with the results of fire test method.
The method of continuous determination of gold,silver and palladium in copper anode low grade copper slag was established and compared with the fire test method. First,the copper anode low grade copper slag was digested with nitric acid+EDTA+tartaric acid to obtain a digestion solution containing silver,palladium and a small amount of gold. The effects of nitric acid,EDTA and tartaric acid dosage on digestion were investigated. The results showed that the digestion was the best when the dosage of nitric acid,EDTA and tartaric acid were 30 m L,3 m L and 1.5 g,respectively. Then,the residue was subjected to secondary digestion with aqua regia to obtain a digestion solution containing gold and a small amount of silver and palladium. The effects of aqua regia dosage on digestion were investigated. The results showed that the amount of aqua regia required to complete the digestion was 15 m L. Finally,the contents of gold,silver and palladium in digestion solution were determined by flame atomic absorption spectrometer. The relative standard deviations of Au,Ag and Pd in the copper anode low grade copper slag were less than 1%(n=10),and the recoveries were between 95.57% and 98.70% by this method. The experimental results are accurate,reliable and reproducible,which is consistent with the results of fire test method.
引文
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[13]曹显庆,廖丽,白群华,等.干灰化-火焰原子吸收分光光度法测定头发中钙铁锌铜[J].应用化工,2014(7):1346-1348.CAO Xianqing,LIAO Li,BAI Qunhua,et al.Determination of Ca,Fe,Zn,Cu in hair by dry-ashing-FAAS[J].Applied Chemical Industry,2014(7):1346-1348.
[2]杨洪英,陈国宝,彭驭风,等.高镍铜阳极泥预处理富集金银的研究[J].东北大学学报(自然科学版),2013,34(3):399-402.YANG Hongying,CHEN Guobao,PENG Yufeng,et al.Pretreatment of copper anode slime with high nickel content for concentrating gold and silver[J].Journal of Northeastern University(Natural Science),2013,34(3):399-402.
[3]胡一平.铜阳极泥处理工艺的选择[J].云南冶金,2015,44(4):34-38.HU Yiping.The selection of copper anode slime treatment technology[J].Yunnan Metallurgy,2015,44(4):34-38.
[4]LIU Weifeng,YANG Tianzu,ZHANG Duchao,et al.Pretreatment of copper anode slime with alkaline pressure oxidative leaching[J].International Journal of Mineral Processing,2014,128(5):48-54.
[5]何梅,胡军凯.电感耦合等离子体原子发射光谱法(ICP-AES)测定铜阳极泥和分银渣中锡、碲的含量[J].中国无机分析化学,2012,2(2):45-48.HE Mei,HU Junkai.Determination of tin and tellurium content in copper anode slime and silver slag by inductively coupled plasma atomic emission spectrometry(ICP-AES)[J].Chinese Journal of Inorganic Analytical Chemistry,2012,2(2):45-48.
[6]全国有色金属标准化技术委员会.铜阳极泥化学分析方法——第2部分:金量和银量的测定火试金重量法:YS/T 745.2—2016[S].北京:中国标准出版社,2016.National Nonferrous Metals Standardization Technical Committee.Methods for chemical analysis of copper anode slime——Part 2:determination of gold content and silver content—Fire assay gravimetric method:YS/T 745.2—2016[S].Beijing:China Standard Press,2016.
[7]全国有色金属标准化技术委员会.铜阳极泥化学分析方法——第3部分:铂量和钯量的测定火试金富集-电感耦合等离子体发射光谱法:YS/T 745.3—2010[S].北京:中国标准出版社,2010.National Nonferrous Metals Standardization Technical Committee.Methods for chemical analysis of copper anode slime——Part 3:Determination of platinum content and palladium content—Fire assay collection-inductively coupled plasma atomic emission spectrometric methods:YS/T 745.3—2010[S].Beijing:China Standard Press,2010.
[8]孙红林,王琳,陈浩凤,等.电感耦合等离子体原子发射光谱法测定地质样品中铂钯金[J].冶金分析,2015,35(11):8-15.SUN Honglin,WANG Lin,CHEN Haofeng,et al.Determination of platinum,palladium and gold in geological samples by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2015,35(11):8-15.
[9]刘益锋,冯俊汉,李展江,等.电感耦合等离子体发射光谱法同时测定粗铜中金和银[J].冶金分析,2012,32(7):52-54.LIU Yifeng,FENG Junhan,LI Zhanjiang,et al.Simultaneous determination of gold and silver in blister copper by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2012,32(7):52-54.
[10]肖红新.湿法分离-火焰原子吸收光谱法测定杂铜中的金[J].贵金属,2013,34(1):67-69.XIAO Hongxin.Determination of gold in composition brass by wet separation-flame atomic absorption spectrometry[J].Precious Metals,2013,34(1):67-69.
[11]韩丽娟,胡军凯,吴一微.降低Ag Cl沉淀对铂和钯吸附的研究[J].湖北师范学院学报(自然科学版),2012,32(4):71-74.HAN Lijuan,HU Junkai,WU Yiwei.Research of reducing the Ag Cl precipitate on the adsorption of platinum and palladium[J].Journal of Hubei Normal University(Natural Science),2012,32(4):71-74.
[12]梁志伟,王立新,杨雪梅.在氨性介质中原子吸收法测定金精矿中的银和铜[J].黄金,2004,25(4):49-50.LIANG Zhiwei,WANG Lixin,YANG Xuemei.Determination of silver and copper in gold concentrate by atomic absorption spectrometry in the present of ammoniacal medium[J].Gold,2004,25(4):49-50.
[13]曹显庆,廖丽,白群华,等.干灰化-火焰原子吸收分光光度法测定头发中钙铁锌铜[J].应用化工,2014(7):1346-1348.CAO Xianqing,LIAO Li,BAI Qunhua,et al.Determination of Ca,Fe,Zn,Cu in hair by dry-ashing-FAAS[J].Applied Chemical Industry,2014(7):1346-1348.