高纯稀土氧化物中的非稀土杂质的测定流动注射微柱预富集ICP-AES法  

Determination of Trace Non Rare Earth Elements in High Purity Rare Earth Oxides by ICP AES

作　　者：吉红念[1,2] 江祖成[1,2] 

机构地区：[1]无锡轻工大学化工系 [2]武汉大学化工系

出　　处：《无锡轻工大学学报（食品与生物技术）》1999年第1期74-77,共4页Journal of Wuxi University of Light Industry

摘　　要：利用自合成的碳硅凝胶为吸附材料，以铜试剂［二乙基二硫代氨基甲酸钠（ＮａＤＤＴＣ）］为柱前衍生化试剂。在优化的实验条件下，于ｐＨ４．６的缓冲介质中在线预富集Ａｌ（Ⅲ），Ｃｒ（Ⅵ），Ｃｕ（Ⅱ），Ｆｅ（Ⅲ），Ｐｂ（Ⅱ），Ｖ（Ⅴ）和Ｚｎ（Ⅱ）．采用停流技术洗脱，富集倍数可达８．１～１２．６倍，检出限为ｎｇ／ｍＬ级。对高纯氧化铕（Ｅｕ２Ｏ３）中的非稀土杂质进行测定，可避免大量稀土基体对测定的干扰。A new method for the determination of trace non rare earth elements in high purity rare earth oxides by ICP AES with preconcentration on an active carbon silica gel microcolumn in a flow injection system is described in this paper. Experimental parameters such as pH,flow rate, reagent concentration,length of reaction coil,eluent acidity,etc.were optimized.In the buffer solution at pH 4.6,Al,Cr,Cu,Fe,Pb,V and Zn can be preconcentrated and then eluted with 4.5 mol/L nitric acid utilizing stop flow technique.The enrichment factors were in range of 8.1￣12.6 with detection limits of μg/mL level,and the RSD with metals at μg/g level were 2.3￣5.0% (n=7). The method proposed can reduce the matrix interference effectively,and has been applied satisfactory to the determination of non rare earth metals at μg/g level in high purity Eu 2O 3 .

关 键 词：高纯氧化铕 非稀土杂质 测定 杂质 氧化铕 

分 类 号：TQ133.3[化学工程—无机化工]