摘要
利用铜粉作为导电介质，与氧化镧粉末混合均匀，压片，采用直流辉光放电质谱法（dc—GDMS）测定了高纯氧化镧粉末中的部分杂质元素含量。考察了辉光放电条件，如放电电流、放电气体流量、离子源温度以及压片条件，如两种粉末的混合比例、压片机压力等因素对放电稳定性以及灵敏度的影响，优化了实验条件；尝试了将镧，氧和铜的总信号归一化进行计算的方法，用差减法计算了高纯氧化镧粉末中的杂质元素含量。将铜粉作为试剂空白，连续测定11次，统计各待测元素检出限为0．005～0．34μg／g；对高纯氧化镧粉末样品独立测定6次，测定结果与电感耦合等离子体质谱法基本吻合，相对标准偏差在20％以内。
Copper powder, as the conductive medium, was mixed evenly with lanthanum oxide powder and tableted. Then the contents of some impurity elements in high purity lanthanum oxide powder were determined by direct current glow discharge mass spectrometry （dc-GDMS）. The glow dischargeconditions like the discharge current, the discharge gas flow rate and the ion source temperature as well as the tableting conditions including the mixing ratio of the two powders and the tableting ma- chine pressure were investigated in terms of their impact on the discharge stability and the sensitivity in order to optimize the experimental conditions. Meanwhile, the total signal of La, O and Cu was normalized and then the content of impurity elements in high purity lanthanum oxide powder were ob- tained by subtraction. Copper powder was considered a reagent blank, and determined for eleven times to obtain the detection limit for analyte elements in the range of 0. 005-0.34 μg/g. The high pu- rity lanthanum oxide powder sample was determined independently for six times. The results were consistent with those obtained by inductively coupled plasma mass spectrometry, and the relative standard deviations （RSD,n=6） were less than 20%.
出处
《冶金分析》
CAS
CSCD
北大核心
2014年第3期24-29,共6页
Metallurgical Analysis
关键词
直流辉光放电质谱法
高纯氧化镧
杂质元素
direct current glow discharge mass spectrometry~ high purity lanthanum oxide
impurity elements
