电感耦合等离子体原子发射光谱法测定地质样品中镉
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摘要
样品经硝酸-氢氟酸-高氯酸混合酸溶解后,用氯化铵调节酸度,加入缓冲溶液使溶液的pH值保持在10~11,使铁、钴、镍等干扰元素沉淀,选择Cd 228.802nm作为分析线,并设置合适的背景扣除位置,采用电感耦合等离子体原子发射光谱法(ICP-AES)测定地质样品中镉。镉的质量浓度在0.000 176~0.160 mg/L范围内与其发射强度呈线性,相关系数r=0.999 8。镉的检出限为0.06μg/g。实验方法用于测定两个地质标准样品中镉,结果的相对标准偏差(RSD,n=12)分别为2.3%和3.2%。按照实验方法测定地质标准样品中镉,结果与认定值相符。
The geological sample was dissolved with mixed nitric acid-hydrofluoric acid-perchloric acid.The acidity was adjusted with ammonium chloride.The pH of solution was kept in range of 10-11 by adding buffer solution to precipitate interference elements including iron,cobalt and nickel.Cd 228.802 nm was selected as the analytical line.The proper background deduction position was set.The content of cadmium in geological sample was determined by inductively coupled plasma atomic emission spectrometry(ICPAES).The mass concentration of cadmium in range of 0.000 176-0.160mg/L was linear to the emission intensity.The correlation coefficient was r=0.999 8.The detection limit of cadmium was 0.06μg/g.The proposed method was applied to the determination of cadmium in two standard geological samples.The relative standard deviation(RSD,n=12)was 2.3% and 3.2%,respectively.The content of cadmium in standard geological samples was determined according to the experimental method,and the results were consistent with the certified values.
The geological sample was dissolved with mixed nitric acid-hydrofluoric acid-perchloric acid.The acidity was adjusted with ammonium chloride.The pH of solution was kept in range of 10-11 by adding buffer solution to precipitate interference elements including iron,cobalt and nickel.Cd 228.802 nm was selected as the analytical line.The proper background deduction position was set.The content of cadmium in geological sample was determined by inductively coupled plasma atomic emission spectrometry(ICPAES).The mass concentration of cadmium in range of 0.000 176-0.160mg/L was linear to the emission intensity.The correlation coefficient was r=0.999 8.The detection limit of cadmium was 0.06μg/g.The proposed method was applied to the determination of cadmium in two standard geological samples.The relative standard deviation(RSD,n=12)was 2.3% and 3.2%,respectively.The content of cadmium in standard geological samples was determined according to the experimental method,and the results were consistent with the certified values.
引文
[1]地质矿产部科学技术司实验管理处.岩石和矿石分析规程:第1分册[M].西安:陕西科学技术出版社,1993:266-275.
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[3]吕跃明.火焰原子吸收光谱法测定土壤中的镉[J].理化检验:化学分册,2004,40(8):468-469.LYue-ming.FAAS determination of cadmium in soil[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2004,40(8):468-469.
[4]张琪,刘琳娟.高压密闭消解-原子吸收光度法同时测定土壤中的铜、锌、铅、镉、镍、铬[J].化学分析计量,2007,16(5):48-50.ZHANG Qi,LIU Lin-juan.Simultaneous determination of Cu,Zn,Pb,Cd,Ni,Cr in soil by atomic absorption spectrometry with digestion under high pressure in a closed pot[J].Chemical Analysis and Meterage,2007,16(5):48-50.
[5]孙汉文,温晓华,梁淑轩.悬浮体进样-基体改进效应石墨炉原子吸收光谱法直接测定土壤中铅和镉[J].光谱学与光谱分析,2006,26(5):950-954.SUN Han-wen,WEN Xiao-hua,LIANG Shu-xuan.Direct determination of lead and cadmium in soil by graphite furnace atomic absorption spectrometry effect of slurry sampling matrix improvement[J].Spectrocopy and Spectral Analysis,2006,26(5):950-954.
[6]邵文军,张激光,刘晶晶.石墨炉原子吸收光谱法测定岩石和土壤中痕量镉[J].岩矿测试,2008,27(4):310-312.SHAO Wen-jun,ZHANG Ji-guang,LIU Jing-jing.Determination of trace cadmium in rock and soil samples by graphite furnace atomic absorption spectrometry[J].Rock and Mineral Analysis,2008,27(4):310-312.
[7]付冉冉,刘水清,荣德福,等.原子荧光光谱法测定铁矿石中的镉[J].岩矿测试,2009,28(6):595-597.FU Ran-ran,LIU Shui-qing,RONG De-fu,et al.Determination of cadmium in iron ores by atomic fluorescene spectrometry[J].Rock and Mineral Analysis,2009,28(6):595-597.
[8]吴成.氢化物发生-原子荧光光谱法测定土壤中的镉[J].光谱学与光谱分析,2003,23(5):990-992.WU Cheng.Determination of Cd in soil by hydride generation-atomic fluorescence spectrometry[J].Spectrocopy and Spectral Analysis,2003,23(5):990-992.
[9]李中玺,周丽萍.断续流动在线分离富集-蒸气发生原子荧光光谱法测定复杂环境样品中痕量镉[J].岩矿测试,2006,25(3):233-238.LI Zhong-xi,ZHOU Li-ping.Intermittent flow injection on-line pre-concentration and determination of ultra-trace cadmium in environmental samples by vapour generation-non-dispersive atomic fluorescence spectrometry[J].Rock and Mineral Analysis,2006,25(3):233-238.
[10]林光西,徐霞,张静梅.电感耦合等离子体质谱法测定地质样品中的镉[J].现代仪器,2007,22(4):63-64.LIN Guang-xi,XU Xia,ZHANG Jing-mei.Determination of trace Cd in geological samples by ICP-MS[J].Modern Instrument,2007,22(4):63-64.
[11]周丽萍,李中玺.王水提取-电感耦合等离子体质谱法同时测定地质样品中微量银、镉、铋[J].分析试验室,2005,24(9):20-25.ZHOU Li-ping,LI Zhong-xi.Determination of silver,cadmium,bismuth in geochemical samples by inductively coupled plasma mass spectrometry with aqua regia extraction[J].Analytical Laboratory,2005,24(9):20-25.
[12]范凡,温宏利,屈文俊,等.王水溶样-等离子体质谱法同时测定地质样品中砷锑铋银镉铟[J].岩矿测试,2009,28(4):333-336.FAN Fan,WEN Hong-li,QU Wen-jun,et al.Determination of arsenic,antimony,bismuth,silver,cadmium and indium in geological samples by inductively coupled plasma-mass spectrometry with aqua regia sample digestion[J].Rock and Mineral Analysis,2009,28(4):333-336.
[13]范晨子,胡明月,赵令阳,等.激光剥蚀电感耦合等离子体质谱分析石笋样品中多元素比值及45种元素含量[J].岩矿测试,2013,32(3):383-391.FAN Chen-zi,HU Ming-yue,ZHAO Ling-yang,et al.Accurate multi-element content and ratio analysis of stalagmites by laser ablation-inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2013,32(3):383-391.
[14]陈永欣,黎香荣,吕泽娥,等.电感耦合等离子体原子发射光谱法测定锰矿石中铝铜锌铅砷镉[J].冶金分析,2009,29(4):46-49.CHEN Yong-xin,LI Xiang-rong,LZe-e,et al.Determination of aluminium,copper,zinc,lead,arsenic and cadmium in manganese ores by inductively coupled plasma-atomic emission spectrometry[J].Metallurgical Analysis,2009,29(4):46-49.
[15]黎香荣,韦万兴,崔翔,等.电感耦合等离子体发射光谱法测定磷矿石中微量有毒元素铅砷镉[J].岩矿测试,2009,28(4):370-372.LI Xiang-rong,WEI Wan-xing,CUI Xiang,et al.Determination of trace toxic elements of lead,arsenic and cadmium in phosphate ores by inductively coupled plasma-atomic emission spectrometry[J].Rock and Mineral Analysis,2009,28(4):370-372.
[16]李清彩,赵庆令,荀红梅.电感耦合等离子体原子发射光谱法测定多金属矿石中砷镉铟硫锑[J].冶金分析,2015,35(2):61-64.LI Qing-cai,ZHAO Qing-ling,XUN Hong-mei.Determination of arsenic,cadmium,indium,sulfur and antimony in polynetallic ore by inductively coupled plasmaatomic emission spectrometry[J].Metallurgical Analysis,2015,35(2):61-64.
[17]沙艳梅,赵学沛,张歌,等.多向观测电感耦合等离子体发射光谱法同时测定土壤和水系沉积物中常量和微量元素[J].岩矿测试,2008,27(4):291-294.SHA Yan-mei,ZHAO Xue-pei,ZHANG Ge,et al.Simultaneous determination of macro-amount and trace elements in soil and stream sediment samples by inductively coupled plasma-optical emission spectrometry with multi-direction viewing mode[J].Rock and Mineral Analysis,2008,27(4):291-294.
[18]于阗,张连起,陈小迪.电感耦合等离子体发射光谱法和火焰原子吸收光谱法连续测定化探样品中12个元素[J].岩矿测试,2011,30(1):71-74.YU Tian,ZHANG Lian-qi,CHEN Xiao-di.Continuous determination of 12elements in geochemical samples by inductively coupled plasma-atomic emission spectrometry and flame atomic absorption spectrometry[J].Rock and Mineral Analysis,2011,30(1):71-74.
[19]曹晓燕,何颖贤,陈强,等.微波消解样品-电感耦合等离子体原子发射光谱法测定锌精矿中镉、砷和汞[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B:Chemical Analysis),2011(6):731-732,735.
[20]闵国华,张庆建,刘稚,等.电感耦合等离子体原子发射光谱法测定铅矿、锌矿和铅锌矿中杂质元素[J].冶金分析,2014,34(5):51-55.MIN Guo-hua,ZHANG Qing-jian,LIU Zhi,et al.Determination of impurity elements in lead ore,zinc ore and lead-zinc ore by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(5):51-55.
[21]叶家喻,江宝林.区域地球化学勘查样品分析方法[M].北京:地质出版社,2004:226-227.
[22]吕春绪,诸松渊.化验室工作手册[M].江苏:江苏科学技术出版社,1997:197-200.
[2]程志臣,王素兰,杨志杰,等.原子捕集-火焰原子吸收光谱法测定环境土壤中痕量镉[J].石油化工环境保护,2001(1):45-47.CHENG Zhi-chen,WANG Su-lan,YANG Zhi-jie,et al.Determination of trace cadmium in environment soil by atomic trapping-flame atomic absorption spectrometry[J].Environment Protection in Petrochemical Industry,2001(1):45-47.
[3]吕跃明.火焰原子吸收光谱法测定土壤中的镉[J].理化检验:化学分册,2004,40(8):468-469.LYue-ming.FAAS determination of cadmium in soil[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2004,40(8):468-469.
[4]张琪,刘琳娟.高压密闭消解-原子吸收光度法同时测定土壤中的铜、锌、铅、镉、镍、铬[J].化学分析计量,2007,16(5):48-50.ZHANG Qi,LIU Lin-juan.Simultaneous determination of Cu,Zn,Pb,Cd,Ni,Cr in soil by atomic absorption spectrometry with digestion under high pressure in a closed pot[J].Chemical Analysis and Meterage,2007,16(5):48-50.
[5]孙汉文,温晓华,梁淑轩.悬浮体进样-基体改进效应石墨炉原子吸收光谱法直接测定土壤中铅和镉[J].光谱学与光谱分析,2006,26(5):950-954.SUN Han-wen,WEN Xiao-hua,LIANG Shu-xuan.Direct determination of lead and cadmium in soil by graphite furnace atomic absorption spectrometry effect of slurry sampling matrix improvement[J].Spectrocopy and Spectral Analysis,2006,26(5):950-954.
[6]邵文军,张激光,刘晶晶.石墨炉原子吸收光谱法测定岩石和土壤中痕量镉[J].岩矿测试,2008,27(4):310-312.SHAO Wen-jun,ZHANG Ji-guang,LIU Jing-jing.Determination of trace cadmium in rock and soil samples by graphite furnace atomic absorption spectrometry[J].Rock and Mineral Analysis,2008,27(4):310-312.
[7]付冉冉,刘水清,荣德福,等.原子荧光光谱法测定铁矿石中的镉[J].岩矿测试,2009,28(6):595-597.FU Ran-ran,LIU Shui-qing,RONG De-fu,et al.Determination of cadmium in iron ores by atomic fluorescene spectrometry[J].Rock and Mineral Analysis,2009,28(6):595-597.
[8]吴成.氢化物发生-原子荧光光谱法测定土壤中的镉[J].光谱学与光谱分析,2003,23(5):990-992.WU Cheng.Determination of Cd in soil by hydride generation-atomic fluorescence spectrometry[J].Spectrocopy and Spectral Analysis,2003,23(5):990-992.
[9]李中玺,周丽萍.断续流动在线分离富集-蒸气发生原子荧光光谱法测定复杂环境样品中痕量镉[J].岩矿测试,2006,25(3):233-238.LI Zhong-xi,ZHOU Li-ping.Intermittent flow injection on-line pre-concentration and determination of ultra-trace cadmium in environmental samples by vapour generation-non-dispersive atomic fluorescence spectrometry[J].Rock and Mineral Analysis,2006,25(3):233-238.
[10]林光西,徐霞,张静梅.电感耦合等离子体质谱法测定地质样品中的镉[J].现代仪器,2007,22(4):63-64.LIN Guang-xi,XU Xia,ZHANG Jing-mei.Determination of trace Cd in geological samples by ICP-MS[J].Modern Instrument,2007,22(4):63-64.
[11]周丽萍,李中玺.王水提取-电感耦合等离子体质谱法同时测定地质样品中微量银、镉、铋[J].分析试验室,2005,24(9):20-25.ZHOU Li-ping,LI Zhong-xi.Determination of silver,cadmium,bismuth in geochemical samples by inductively coupled plasma mass spectrometry with aqua regia extraction[J].Analytical Laboratory,2005,24(9):20-25.
[12]范凡,温宏利,屈文俊,等.王水溶样-等离子体质谱法同时测定地质样品中砷锑铋银镉铟[J].岩矿测试,2009,28(4):333-336.FAN Fan,WEN Hong-li,QU Wen-jun,et al.Determination of arsenic,antimony,bismuth,silver,cadmium and indium in geological samples by inductively coupled plasma-mass spectrometry with aqua regia sample digestion[J].Rock and Mineral Analysis,2009,28(4):333-336.
[13]范晨子,胡明月,赵令阳,等.激光剥蚀电感耦合等离子体质谱分析石笋样品中多元素比值及45种元素含量[J].岩矿测试,2013,32(3):383-391.FAN Chen-zi,HU Ming-yue,ZHAO Ling-yang,et al.Accurate multi-element content and ratio analysis of stalagmites by laser ablation-inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2013,32(3):383-391.
[14]陈永欣,黎香荣,吕泽娥,等.电感耦合等离子体原子发射光谱法测定锰矿石中铝铜锌铅砷镉[J].冶金分析,2009,29(4):46-49.CHEN Yong-xin,LI Xiang-rong,LZe-e,et al.Determination of aluminium,copper,zinc,lead,arsenic and cadmium in manganese ores by inductively coupled plasma-atomic emission spectrometry[J].Metallurgical Analysis,2009,29(4):46-49.
[15]黎香荣,韦万兴,崔翔,等.电感耦合等离子体发射光谱法测定磷矿石中微量有毒元素铅砷镉[J].岩矿测试,2009,28(4):370-372.LI Xiang-rong,WEI Wan-xing,CUI Xiang,et al.Determination of trace toxic elements of lead,arsenic and cadmium in phosphate ores by inductively coupled plasma-atomic emission spectrometry[J].Rock and Mineral Analysis,2009,28(4):370-372.
[16]李清彩,赵庆令,荀红梅.电感耦合等离子体原子发射光谱法测定多金属矿石中砷镉铟硫锑[J].冶金分析,2015,35(2):61-64.LI Qing-cai,ZHAO Qing-ling,XUN Hong-mei.Determination of arsenic,cadmium,indium,sulfur and antimony in polynetallic ore by inductively coupled plasmaatomic emission spectrometry[J].Metallurgical Analysis,2015,35(2):61-64.
[17]沙艳梅,赵学沛,张歌,等.多向观测电感耦合等离子体发射光谱法同时测定土壤和水系沉积物中常量和微量元素[J].岩矿测试,2008,27(4):291-294.SHA Yan-mei,ZHAO Xue-pei,ZHANG Ge,et al.Simultaneous determination of macro-amount and trace elements in soil and stream sediment samples by inductively coupled plasma-optical emission spectrometry with multi-direction viewing mode[J].Rock and Mineral Analysis,2008,27(4):291-294.
[18]于阗,张连起,陈小迪.电感耦合等离子体发射光谱法和火焰原子吸收光谱法连续测定化探样品中12个元素[J].岩矿测试,2011,30(1):71-74.YU Tian,ZHANG Lian-qi,CHEN Xiao-di.Continuous determination of 12elements in geochemical samples by inductively coupled plasma-atomic emission spectrometry and flame atomic absorption spectrometry[J].Rock and Mineral Analysis,2011,30(1):71-74.
[19]曹晓燕,何颖贤,陈强,等.微波消解样品-电感耦合等离子体原子发射光谱法测定锌精矿中镉、砷和汞[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B:Chemical Analysis),2011(6):731-732,735.
[20]闵国华,张庆建,刘稚,等.电感耦合等离子体原子发射光谱法测定铅矿、锌矿和铅锌矿中杂质元素[J].冶金分析,2014,34(5):51-55.MIN Guo-hua,ZHANG Qing-jian,LIU Zhi,et al.Determination of impurity elements in lead ore,zinc ore and lead-zinc ore by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(5):51-55.
[21]叶家喻,江宝林.区域地球化学勘查样品分析方法[M].北京:地质出版社,2004:226-227.
[22]吕春绪,诸松渊.化验室工作手册[M].江苏:江苏科学技术出版社,1997:197-200.