直流辉光放电质谱法测定高纯氧化铕中72种杂质元素  

Determination of 72 impurity elements in high purity europium oxide by direct current glow discharge mass spectrometry

作　　者：贾晓琪 张秀艳[1] 陈彪 李欣欣 王振江[1] 任旭东[1] JIA Xiaoqi;ZHANG Xiuyan;CHEN Biao;LI Xinxin;WANG Zhenjiang;REN Xudong(Baotou Rare Earth Research Institute,National Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization,Baotou 014030,China)

机构地区：[1]包头稀土研究院,白云鄂博稀土资源研究与综合利用全国重点实验室,内蒙古包头014030

出　　处：《冶金分析》2023年第11期22-29,共8页Metallurgical Analysis

基　　金：内蒙古自然科学基金分析测试专项(2023FX01);中国北方稀土(集团)高科技股份有限公司科技项目(2022H2386);战略性矿产选冶关键分析检测技术和标准体系研究(2021YFC2903101)。

摘　　要：高纯氧化铕广泛应用于荧光材料,杂质含量直接影响其使用性能,高效、准确测定其杂质元素的含量至关重要。以高纯铟为导电介质,将氧化铕粉末压到铟片上制成样片,利用高纯氧化铕质控样品对其中34种元素的相对灵敏度因子进行校正,通过选择合适的同位素和分辨率克服质谱干扰,建立了直流辉光放电质谱法(dc-GDMS)测定高纯氧化铕中S、Cl、Si、Na等72种杂质元素的方法。优化后的实验条件如下:放电电流为2.0 mA,放电气体流量为0.30 mL/min,预溅射时间为30 min,样品薄层直径为3~5 mm,K元素在高分辨率(R=5689)下测定,其他元素均在中分辨率(R=4000)下测定。实验表明,72种元素的检出限为0.003~50.01μg/g,定量限为0.01~166.7μg/g。按照实验方法测定4N级(纯度为99.99%)高纯氧化铕粉末样品中72种杂质元素,结果表明:样品中杂质元素含量大于1μg/g时,相对标准偏差(RSD,n=6)在10%以内;杂质元素含量在0.1~1μg/g范围内,RSD(n=6)在20%以内;杂质元素含量低于0.1μg/g时,RSD(n=6)在30%以内。采用电感耦合等离子体质谱法(ICP-MS)对该样品中部分含量相对较高的杂质元素进行测定,结果表明,两种方法测定结果基本一致。High purity europium oxide is widely used in fluorescent materials.The content of impurities in high purity europium oxide directly affects its performance.Therefore,it is important to determine the content of impurity elements efficiently and accurately.In this study,the high purity indium was used as conductive medium.The europium oxide powder was pressed onto indium sheet to prepare the sample sheet.The relative sensitivity factors of 34 elements were corrected using the high purity europium oxide quality control sample.The mass spectrum interference was overcome by selecting appropriate isotopes and resolution.A method for the determination of 72 impurity elements such as S,Cl,Si and Na in high purity europium oxide by direct current glow discharge mass spectrometry(dc-GDMS)was established.The optimized experimental conditions were obtained as follows:the discharge current was 2.0 mA,the discharge gas flow was 0.30 mL/min,the pre-sputtering time was set to 30 min,and the thin layer diameter of the sample was about 3-5 mm.Potassium was determined at high resolution(R=5689),and other elements were determined at medium resolution(R=4000).The results showed that the limits of detection of 72 elements ranged from 0.003 to 50.01μg/g,and the limits of quantification ranged from 0.01 to 166.7μg/g.The contents of 72 impurity elements in 4N-grade high purity europium oxide powder sample(the purity was 99.99%)according to the experimental method.The results showed that the relative standard deviations(RSD,n=6)were within 10%when the content of impurities in the sample was greater than 1μg/g.As the content of impurity elements was in the range of 0.1-1μg/g,the RSD(n=6)was less than 20%.When the content of impurity elements was less than 0.1μg/g,the RSD(n=6)was within 30%.The impurity elements with relatively high content in the sample were determined by inductively coupled plasma mass spectrometry(ICP-MS).The results showed that the measurement values of two methods were basically consistent.

关 键 词：直流辉光放电质谱法(dc-GDMS) 高纯氧化铕 相对灵敏度因子(RSF) 杂质元素 

分 类 号：O657.63[理学—分析化学] TF03[理学—化学]