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阴离子交换树脂分离甲苯萃取ICP-AES测定铋系超导粉中的痕量镍
引用本文:Fan LX,Li JQ,Fan HL,Sun JL,Zhang X,Bao R,Lu Q,Wang J. 阴离子交换树脂分离甲苯萃取ICP-AES测定铋系超导粉中的痕量镍[J]. 光谱学与光谱分析, 2011, 31(12): 3375-3378. DOI: 10.3964/j.issn.1000-0593(2011)12-3375-04
作者姓名:Fan LX  Li JQ  Fan HL  Sun JL  Zhang X  Bao R  Lu Q  Wang J
作者单位:1. 北京科技大学化学系,北京,100083
2. 北京英纳超导技术有限公司,北京,100176
基金项目:国家(863计划)项目(2006AA03Z236)资助
摘    要:
建立了ICP-AES测定超导粉中痕量镍的新方法。优化了仪器工作参数,对超导前驱粉中痕量镍测定时的基体干扰及干扰消除方法进行了系统研究,结果表明:大量存在的基体元素产生严重基体效应,导致测定重现性及准确度变差,实验采用分离富集方法以提高测定结果的准确度和精密度。实验中首先用阴离子交换树脂,除去Bi3+及部分Pb2+,Sr2+,Ca2+,Cu2+等基体元素;在碱性条件下再通过甲苯萃取镍与丁二酮肟的络合物、稀盐酸反萃取富集镍;对分离富集条件进行了优化。对模拟标准样品进行测定,分析结果与理论值一致,相对标准偏差为1.9%,方法检出限为0.19μg.g-1。该方法已用于超导前驱粉样品中痕量镍的分析,结果令人满意。

关 键 词:  ICP-AES  超导粉  甲苯萃取  阴离子交换树脂  

Determination of trace nickel in bi-based superconductor powder by inductively coupled plasma atomic emission spectroscopy after separation with anion exchange resin and extraction with methylbenzene
Fan Li-xin,Li Jian-qiang,Fan Hui-li,Sun Jian-ling,Zhang Xia,Bao Rui,Lu Qing,Wang Jie. Determination of trace nickel in bi-based superconductor powder by inductively coupled plasma atomic emission spectroscopy after separation with anion exchange resin and extraction with methylbenzene[J]. Spectroscopy and Spectral Analysis, 2011, 31(12): 3375-3378. DOI: 10.3964/j.issn.1000-0593(2011)12-3375-04
Authors:Fan Li-xin  Li Jian-qiang  Fan Hui-li  Sun Jian-ling  Zhang Xia  Bao Rui  Lu Qing  Wang Jie
Affiliation:FAN Li-xin1,LI Jian-qiang1,FAN Hui-li1,SUN Jian-ling1,ZHANG Xia1,BAO Rui2,LU Qing1,WANG Jie1 1.Department of Chemistry,University of Science and Technology Beijing,Beiji ng 100083,China 2.Innova Superconductor Technology Co.Ltd.,Beijing 100176,China
Abstract:
A new method for the determination of trace nickel in superconductor powder by ICP-AES was proposed.The instru-ment parameters were optimized,and the matrix effects as well as the method of eliminating interferences were also studied sys-temically.The results showed that matrix interference in the superconductor powder was serious when the amount of matrix in-creased,and the repeatability as well as the accuracy was poor,so it was necessary to used separation and preconcentration toimprove the accuracy and ...
Keywords:Nickel  ICP-AES  Superconductor powder  Extr action with methylbenzene  Anion exchange resin  
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