电感耦合等离子体质谱法测定镧镁合金中稀土杂质
张立锋1, 2 , 张秀艳1, 2 , 张翼明1, 2 , 李立刚1, 2
1.包头稀土研究院, 内蒙古包头 014030; 2. 稀土冶金及功能材料国家工程研究中心, 内蒙古包头 014030
Determination of rare earth impurities in lanthanum-magnesium alloy by inductively coupled plasma mass spectrometry
ZHANG Li-feng1, 2 , ZHANG Xiu-yan1, 2 , ZHANG Yi-ming1, 2 , LI Li-gang1, 2
1.Baotou Research Institute of Rare Earths, Baotou 014030, China; 2.National Engineering Research Centre of Rare Earth Metallurgy and Funcional Materials, Baotou 014030, China
摘要 采用硝酸溶解样品, 建立了电感耦合等离子体质谱法(ICP-MS)测定镧镁合金中稀土杂质的含量。选择合适的测定同位素以及选用干扰元素校正方程克服了质谱干扰。对仪器工作条件进行了优化, 确定功率为1 100 W, 载气流量为0.80 L/min。讨论了测定条件对结果的影响, 确定测定介质为1%硝酸, 内标元素为Cs, 基体浓度小于0.3 mg/mL。方法测定下限为0.006 9~0.046 ng/mL。采用方法对实际样品进行测定, 回收率为98%~102%。与电感耦合等离子体发射光谱法(ICP-AES)进行方法对照, 两种方法测定结果基本一致, 相对标准偏差(RSD, n =6)在1.7%~4.5%之间。
关键词 :
电感耦合等离子体质谱法(ICP-MS) ,
镧镁合金 ,
稀土杂质
Abstract :After the sample was dissolved by nitric acid, a method for determination of rare earth impurities in lanthanum-magnesium alloy was established by inductively coupled plasma mass spectrometry. Appropriate isotopes and interfering elements correction equation were chosen to overcome spectral interferences. The instrument working conditions were optimized with power of 1 100 W and carrier gas flow rate of 0.80 L/min. A discussion of the impact of testing conditions on the result was conducted. The testing conditions were confirmed as follows: 1% nitric acid as medium, Cs as internal standard element and substrate concentration less than 0.3 mg/mL. The low limit of determination of the method was 0.006 9-0.046 ng/mL. This method was employed to determine actual sample with recoveries of 98%-102%. Compared with inductively coupled plasma atomic emission spectrometry (ICP-AES), the results of both methods were basically consistent with each other, and relative standard deviation (RSD, n =6) were in the range of 1.7%-4.5%.
Key words :
inductively coupled plasma mass spectrometry (ICP-MS)
lanthanum-magnesium alloy
rare earth impurity
收稿日期: 2013-08-09
作者简介 : 张立锋(1981-)男, 工程师, 本科, 从事冶金分析研究;
引用本文:
张立锋, 张秀艳, 张翼明, 李立刚. 电感耦合等离子体质谱法测定镧镁合金中稀土杂质[J]. 冶金分析, 2014, 34(6): 33-37.
ZHANG Li-feng, ZHANG Xiu-yan, ZHANG Yi-ming, LI Li-gang. Determination of rare earth impurities in lanthanum-magnesium alloy by inductively coupled plasma mass spectrometry. , 2014, 34(6): 33-37.
链接本文:
http://47.93.29.245/Jweb_yjfx/CN/10.13228/j.issn.1000-7571.2014.06.007 或 http://47.93.29.245/Jweb_yjfx/CN/Y2014/V34/I6/33
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