色层分离－端视电感耦合等离子体发射光谱法测定高纯氧化铕中稀土杂质元素

Determination of 14 Rare Earth Impurities in High Purity Europium Oxide by Axis-view ICP-AES with Chromatographic Separation

对Ｐ５０７萃淋树脂分离稀土元素的条件进行了实验，拟定了以Ｐ５０７萃淋树脂为固定相，ＨＣｌ为流动相分离４Ｎ级荧光材料Ｅｕ＿２Ｏ＿３中１４种稀土杂质元素的流程，使被测杂质与基体Ｅｕ＿２Ｏ＿３达到了较好的分离；再用阳离子交换树脂分离被测液中非稀土杂质元素。选择了端视ＩＣＰ－ＡＥＳ测量稀土杂质元素的最佳条件。称样量５０ｍｇ时各杂质组分的测定下限（ｕｇ／ｇ）为：ＣｅＯ＿２、Ｐｒ＿６Ｏ＿（１１）、Ｎｄ＿２Ｏ＿３、Ｓｍ＿２Ｏ＿３、Ｔｂ＿４Ｏ＿７、Ｈｏ＿２Ｏ＿３、Ｅｒ＿２Ｏ＿３，Ｔｍ＿２Ｏ＿３、Ｌｕ＿２Ｏ＿３０．４，Ｌａ＿２Ｏ＿３、Ｇｄ＿２Ｏ＿３、０．２，Ｄｙ＿２Ｏ＿３、Ｙ＿２Ｏ＿３０．０４，Ｙｂ＿２Ｏ＿３０．０２。６次取样分析，各杂质组分加入量为１０ｕｇ／ｇ（ＣｅＯ＿２为２ｕｇ／ｇ），加入回收率在８４％～１１２％；ＲＳＤ＜１３％。方法可用于纯度在９９．９９％～９９．９９９５％Ｅｕ＿２Ｏ＿３中１４种稀土杂质元素的测定。

n axis-view ICp-AES with chromato graphic separation procedure for determination of 14rare earth impurities in high purity(> 99.99%)europium oxide has been developed.In thisprocedure,two separation steps are employed:the first one, P507 extraction-elution resin wasused as the fixed phase and diluted HCl as effluents,14 RE elements were separated from Europ-ium oxide and the second one,non-rare earth elements,which came from sample as well aschemicals, were removed by cation exchanger.ARF generator with independent drive oscillatorand PGS-2 grating spectrometer were used.The detection limits of 14 RE elements are listed below(ug/g):CeO_2,Pr_6O_(11),Nd_2O_3.Sm_2O_3.Tb_4O_7,Ho_2O_3,Er_2O_3,Tm_2O_3,Lu_2O_3 0.4;La_2O_3,Gd_2O_3 0.2; Dy_2O_3,Y_2O_3 0.04;Yb_2O_3 0.02.Based on six experiznents, the recoveries of 14 REelements(CeO_22ug/g,other 10ug/g)through this procedure are between 84%and 112%,Therelative standard deviation(RSD)is within 13%,This procedure can meet the requirement ofhigh technology.