电感耦合等离子体质谱法测定稀土系贮氢合金中镉和铅
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摘要
采用硝酸低温溶解试样,以2%(V/V)硝酸为测定介质,建立了电感耦合等离子体质谱法(ICP-MS)测定稀土系贮氢合金中镉和铅的方法。以~(111) Cd和~(208)Pb作为测定同位素,消除了同量异位素和多原子离子的质谱干扰;以10.0ng/mL的~(133) Cs为内标校正了基体效应和仪器信号漂移。镉和铅元素的校准曲线相关系数均大于0.999 8,线性关系良好,方法检出限分别为0.03ng/mL和0.04ng/mL,方法测定下限分别为0.10ng/mL和0.13ng/mL。采用在稀土系贮氢合金试样中加入镉和铅标准溶液的方法配制稀土系贮氢合金合成试样,按实验方法进行处理并测定,测得结果与电感耦合等离子体原子发射光谱法(ICP-AES)测定结果基本一致。采用实验方法对稀土系贮氢合金中铅进行测定,相对标准偏差(n=11)为4.2%,镉和铅的加标回收率分别为96%~104%和95%~102%。
Afer the sample was dissolved with nitric acid at low temperature,a determination method of cadmium and lead in rare earth based hydrogen storage alloy was established by inductively coupled plasma mass spectrometry(ICP-MS)with 2%(V/V)nitric acid as determination medium.111 Cd and 208 Pb were selected as determination isotopes to eliminate the mass spectrometry interference of isobars and polyatomic ions.The matrix effect and instrumental signal drift were corrected with 10.0ng/mL 133 Cs as internal standard.The correlation coefficients of calibration curves for cadmium and lead were higher than 0.999 8,indicating the good linear relationship.The detection limit of method was 0.03ng/mL and 0.04ng/mL,respectively.While the lower limit of determination was 0.10ng/mL and 0.13ng/mL,respectively.The synthetic samples of rare earth based hydrogen storage alloy were prepared by adding standard solution of cadmium and lead into rare earth based hydrogen storage alloy samples,and then treated and determined according to the experimental method.The results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry(ICP-AES).The proposed method was applied for the determination of lead in rare earth based hydrogen storage alloy.The relative standard deviation(RSD,n=11)was 4.2%.The recoveries for cadmium and lead were 96%-104% and 95%-102%,respectively.
Afer the sample was dissolved with nitric acid at low temperature,a determination method of cadmium and lead in rare earth based hydrogen storage alloy was established by inductively coupled plasma mass spectrometry(ICP-MS)with 2%(V/V)nitric acid as determination medium.111 Cd and 208 Pb were selected as determination isotopes to eliminate the mass spectrometry interference of isobars and polyatomic ions.The matrix effect and instrumental signal drift were corrected with 10.0ng/mL 133 Cs as internal standard.The correlation coefficients of calibration curves for cadmium and lead were higher than 0.999 8,indicating the good linear relationship.The detection limit of method was 0.03ng/mL and 0.04ng/mL,respectively.While the lower limit of determination was 0.10ng/mL and 0.13ng/mL,respectively.The synthetic samples of rare earth based hydrogen storage alloy were prepared by adding standard solution of cadmium and lead into rare earth based hydrogen storage alloy samples,and then treated and determined according to the experimental method.The results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry(ICP-AES).The proposed method was applied for the determination of lead in rare earth based hydrogen storage alloy.The relative standard deviation(RSD,n=11)was 4.2%.The recoveries for cadmium and lead were 96%-104% and 95%-102%,respectively.
引文
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[2]MALGORZATA KARWOWSKA,TOMASZ JARON,KAROL J FIJALKOWSKI,et al.Influence of electrolyte composition on behavior of AB5hydrogen storage alloy used as negative electrode in Ni/MH batteries[J].Journal of Power Sources,2014,263(5):304-309.
[3]曹慧,柳召刚,徐津,等.热处理对La0.53Ce0.47Ni3.4Co0.6-Mn0.3Cu0.1合金相结构和储氢性能的影响[J].有色金属:冶炼部分,2016(6):58-61.CAO Hui,LIU Zhao-gang,XU Jin,et al.Effect of heat treatment on structure and hydrogen storage property of La0.53Ce0.47Ni3.4Co0.6Mn0.3Cu0.1 alloy[J].Nonferrous Metals:Extractive Metallurgy,2016(6):58-61.
[4]唐仁衡,周顺,肖方明,等.热处理温度对La0.8Ce0.2-(NiCoMnAl)5储氢合金结构与性能的影响[J].材料导报,2014,28(7):114-120.TANG Ren-heng,ZHOU Shun,XIAO Fang-ming,et al.Influence of heat treatment on the structure and properties of La0.8Ce0.2(NiCoMnAl)5hydrogen storage of alloy[J].Materials Review,2014,28(7):114-120.
[5]袁华堂,王一菁,闫超,等.新型稀土高性能储氢合金研究进展[J].化工进展,2012,31(2):253-258.YUAN Hua-tang,WANG Yi-jing,YAN Chao,et al.Analysis of influencing factors on properties of rare-earth hydrogen storage alloys[J].Chemical Industry and Engineering Progress,2012,31(2):253-258.
[6]刘丽静,刘晓杰,许涛,等.电感耦合等离子体光谱法测定La15Fe77B8型储氢合金中镧、铁、硼、铝、镍、锰的含量[J].稀土,2015,36(3):100-104.LIU Li-jing,LIU Xiao-jie,XU Tao,et al.Determination of La,Fe,B,Al,Ni,Mn in La15Fe77B8type of hydrogen storage alloys by inductively coupled plasma atomic emission spectrometry[J].Rare Earth,2015,36(3):100-104.
[7]靳兰兰,王秀季,李会来,等.电感耦合等离子体质谱技术进展及其在冶金分析中的应用[J].冶金分析,2016,36(7):1-14.JIN Lan-lan,WANG Xiu-ji,LI Hui-lai,et al.Progress in inductively coupled plasma mass spectrometry technology and its application in metallurgical analysis[J].Metallurgical Analysis,2016,36(7):1-14.
[8]黄楚楚,李青,张国霞,等.上海市区大气颗粒物(PM2.5)中铅、镉的分析测定和污染特征研究[J].分析化学,2016,44(7):1047-1052.HUANG Chu-chu,LI Qing,ZHANG Guo-xia,et al.Analysis of pollution characteristics of cadmium and lead in atmospheric particulates(PM2.5)of shanghai downtown[J].Chinese Journal of Analytical Chemistry,2016,44(7):1047-1052.
[9]葛晶晶,刘洁.电感耦合等离子体质谱法测定高纯锌中7种痕量元素[J].冶金分析,2016,36(9):37-41.GE Jing-jing,LIU Jie.Determination of seven trace elements in high purity zinc by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2016,36(9):37-41.
[10]田衎,孙自杰,周裕敏,等.电感耦合等离子体质谱法分析高纯金属银中痕量杂质元素[J].冶金分析,2016,36(7):51-55.TIAN Kan,SUN Zi-jie,ZHOU Yu-min,et al.Determination of trace impurity elements in high purity metal silver by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2016,36(7):51-55.
[11]郝原芳,刘新,宋丽华,等.电感耦合等离子体质谱法测定铅合金中的微量杂质元素镉和锡[J].岩矿测试,2016,35(4):378-383.HAO Yuan-fang,LIU Xin,SONG Li-hua,et al.Determination of trace cadmium and tin in lead alloys by inductively coupled plasma mass spectrometry[J].Rock and Mineral Analysis,2016,35(4):378-383.