Application of modified chemical sequential extraction-inductively coupled plasma mass spectrometry to determination of chemical speciation of copper,lead,zinc,cadinum and nickel in lead and zinc tailings
SHI Yi-hua,YANG Zhao-hong,XU hua,GU Xing-qian,QIU Li,TANG Bi-yu
Testing Center,China Nonferrous MetalGuilin Geology and Amining Co.,Ltd.,Guilin 541004,China
Four chemical forms (i.e., exchangeable form(F1), reducible form(F2), oxidable form(F3) and residual form(F4)) of heavy metal elements including copper, lead, zinc, cadmium and nickel in lead-zinc tailings were extracted by modified chemical sequential extraction (BCR) method. Then, the total amount and the content of each speciation of copper, lead, zinc, cadmium and nickel in lead-zinc tailings were determined by inductively coupled plasma mass spectrometry (ICP-MS). The results showed that the detection limits of method for each speciation of these four elements were between 0.012 mg/kg and 0.85 mg/kg, and the corresponding relative standard deviations (RSD, n=5) were between 2.1% and 9.9%. The ratios of the content sum of all speciations to the total measured value for each element were between 88.1%-101.2%. It indicated that the proposed method was applicable for the speciation analysis of copper, lead, zinc, cadmium and nickel in lead-zinc tailings. Three lead-zinc tailings samples were determined according to the experimental method. The results showed that the content of residual form of copper, lead, zinc, cadmium and nickel accounted for the maximum proportion with not less than 30% of total content. The content distribution sequence from high to low for lead and zinc was F4, F2, F1, F3. For copper and zinc, the sequence was F4,F3,F2,F1, while it was F4,F1,F3,F2 for cadmium. This proposed method provided important reference information for the comprehensive utilization of heavy metal elements in lead-zinc tailings region, the environmental impact assessment and the environmental governance.
施意华,阳兆鸿,徐 华,古行乾,邱 丽,唐碧玉. 改进化学顺序提取-电感耦合等离子体质谱法应用于铅锌尾矿中铜铅锌镉镍的化学形态分析[J]. 冶金分析, 2016, 36(7): 83-88.
SHI Yi-hua,YANG Zhao-hong,XU hua,GU Xing-qian,QIU Li,TANG Bi-yu. Application of modified chemical sequential extraction-inductively coupled plasma mass spectrometry to determination of chemical speciation of copper,lead,zinc,cadinum and nickel in lead and zinc tailings. , 2016, 36(7): 83-88.
王钦建,石琳,黄颖.国内铅锌尾矿综合利用概况[J].中国资源综合利用,2012,30(8):33-37.WANG Qin-jian,SHI Lin,HUANG Ying.Comprehensive utilization situation of tailing ore of lead and zinc in China[J].China Resources Comprehensive Utilization,2012,30(8):33-37.
[2]
郭建平,吴甫成,谢淑容,等.湖南临湘铅锌矿尾矿库环境状况及开发利用研究[J].土壤通报,2007,38(3):553-557.GUO Jian-ping,WU Fu-cheng,XIE Shu-rong,et al.Environmental conditions and exploitation of lead-zinc tailings in Linxiang county,Hunan Province[J].Chinese Joumal of Soil Science,2007,38(3):553-557.
[3]
刘新,陈卫中,贾皓,等.火焰原子吸收光谱法测定铅锌矿尾矿矿渣中镉和铬[J].冶金分析,2012,32(9):30-35.LIU Xin,CHEN Wei-zhong,JIA Hao,et al.Determination of cadmium and chromium in lead-zinc ore tailings slag by flame atomic absorption spectrometry[J].Metallurgical Analysis,2012,32(9):30-35.
[4]
王书民,樊雪梅,张晓晶,等.催化动力学光度法测定锌尾矿中痕量铅[J].冶金分析,2013,33(6):42-46.WANG Shu-min,FAN Xue-mei,ZHANG Xiao-jing,et al.Catalytic kinetic spectrophotometric determination of trace lead in zinc mine tailings[J].Metallurgical Analysis,2013,33(6):42-46.
[5]
邱丽,唐碧玉,古行乾,等.电感耦合等离子体质谱法测定铅锌矿尾矿渣中铜、铅、锌和镉[J].理化检验:化学分册,2015,51(7):943-946.QIU Li,TANG Bi-yu,GU Xing-qian,et al.Determination of Cu,Pb,Zn and Cd in lead-zinc tailings slag by ICP-MS[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2015,51(7):943-946.
[6]
王媛,魏忠义,张卫,等.柴河铅锌尾矿中重金属铅、锌、镉的迁移特征[J].环境污染与防治,2015,37(10):58-62.WANG Yuan,WEI Zhong-yi,ZHANG Wei,et al.Migration characteristics of the heavy metals lead,zinc and cadmium from Chaihe lead-zinc tailings[J].Environmental Pollution & Control,2015,37(10):58-62.
[7]
Tessier A,Campbell P G C,Bisson M.Sequential extraction procedure for the speciation of particulate trace metals[J].Anal.Chem.,1979,51(7):844-850.
[8]
刘文长,马玲,刘洪青,等.生态地球化学土壤样品元素形态分析方法研究[J].岩矿测试,2005,24(3):181-188.LIU Wen-zhang,MA Ling,LIU Hong-qing,et al.Research on speciation analysis of chemical elements in soil samples for ecosystem geochemistry study[J].Rock and Mineral Analysis,2005,24(3):181-188.
[9]
黄光明,周康民,汤志云,等.土壤和沉积物中重金属形态分析[J].土壤,2009,41(2):201-205.HUANG Guang-ming,ZHOU Kang-min,TANG Zhi-yun,et al.Analytical method of heavy metal fractions in soil and sediment[J].Soils,2009,41(2):201-205.
[10]
关天霞,何红波,张旭东,等.土壤中重金属元素形态分析方法及形态分布的影响因素[J].土壤通报,2011,42(2):503-512.GUAN Tian-xia,HE Hong-bo,ZHANG Xu-dong,et al.The methodology of fractionation analysis and the factors affecting the species of heavy metals in soil[J].Chinese Journal of Soil Science,2011,42(2):503-512.
[11]
徐亚岩,柏育材,王云龙,等.东海近海沉积物自然粒度中镉和铅的赋存特性及潜在生态风险[J].生态环境学报,2015,24(4):650-657.XU Ya-yan,BAI Yu-cai,WANG Yun-long,et al.Variation characteristics and potential ecological risk assessment of Cd and Pb in the sediments of the East China Sea[J].Ecology and Environmental Sciences,2015,24(4):650-657.
[12]
Quevauviller P,Rauet G,Griepink B.Single and sequential extraction in sediments and soils[J].International Journal of Environmental Analytical Chemistry,1993,51(1-4):231-235.
[13]
胡德新,武素茹,刘跃勇,等.改进BCR法-电感耦合等离子体发射光谱法测定矿产品堆场土壤中镉砷铅的化学形态[J].岩矿测试,2014,33(3):369-373.HU De-xin,WU Su-ru,LIU Yue-yong,et al.Determination of chemical species of cadmium,arsenic and leadin mineral yard soil by modified BCR and ICP-AES method[J].Rock and Mineral Analysis,2014,33(3):369-373.
[14]
任萍,汪明启.改进 BCR 法在分析水系沉积物样品铅形态中的应用[J].物探与化探,2004,28(3):222-223,221.REN Ping,WANG Ming-qi.The modified BCR sequential extraction method for lead spaciation in sediments[J].Geophysical & Geochemical Exploration,2004,28(3):222-223,221.
[15]
张朝阳,彭平安,宋建中,等.改进BCR法分析国家土壤标准物质中重金属化学形态[J].生态环境学报,2012,21(11):1881-1884.ZHANG Chao-yang,PENG Ping-an,SONG Jian-zhong,et al.Utilization of modified BCR procedure for the chemical speciation of heavy metals in Chinese soil reference material[J].Ecology and Environmental Sciences,2012,21(11):1881-1884.
[16]
王琳,来新泽,唐志中,等.改进 BCR 法测定公路两旁表层土壤中铂钯铑的化学形态[J].岩矿测试,2012,31(6):954-960.WANG Lin,LAI Xin-ze,TANG Zhi-Zhong,et al.Determination of chemical species of platinum,palladium and rhodium in roadside surface soil with a modified BCR method[J].Rock and Mineral Analysis,2012,31(6):954-960.
[17]
Oan Muhammad Sahito,Hassan Imran Afridi,Tasneem Gul Kazi,et al.Evaluation of heavy metal bioavailability in soil amended with poultry manure using single and BCR sequential extractions[J].International Journal of Environmental Analytical Chemistry,2015,95(11):1066-1079.
[18]
Roberta Ferria,Dana Hashim,Donald R Smith,et al.Metal contamination of home garden soils and cultivated vegetables in the province of Brescia,Italy Implications for human exposure[J].Science of the Total Environment,2015(518-519) :507-517.
[19]
Elena Ciceri,Barbara Giussani,Andrea Pozzi,et al.Problems in the application of the three-step BCR sequential extraction to low amounts of sediments:An alternative validated route[J].Talanta,2008,76 (3) :621-626.
[20]
Xin Hu,Yun Zhang,Jun Luo,et al.Total concentrations and fractionation of heavy metals in road-deposited sediments collected from different land use zones in a large city (Nanjing),China[J].Chemical Speciation and Bioavailability,2011,23(1):46-52.
[21]
Xiaoping Li,Lin-na Feng.Geostatistical analyses and fractionation of heavy metals in urban soil from industrial district in Weinan,NW China[J].Environmental Earth Sciences,2012,67(7):2129-2140.
[22]
王小如.电感耦合等离子体质谱应用实例[M].北京:化学工业出版社,2005,86-87.
[23]
张亚峰,冯俊,唐杰,等.基于五酸溶样体系-ICP-MS同时测定地质样品中稀土等46种元素[J].质谱学报,2016,37(2):186-192.ZHANG Ya-feng,FENG Jun,TANG Jie,et al.Simultaneous determination of 46 species of micro,trace and rare earth elements by ICP-MS based on the system of five-acids dissolution of sample[J].Journal of Chinese Mass Spectrometry Society,2016,37(2):186-192.