萃取色层分离-水平式ICP/AES法测定U_3O_8中Hf,Zr,Sc,Th,Ag

DETERMINATION OF TRACE Hf, Zr, Sc, Th AND Ag IN U_3O_8, BY HORIZONTAL ICP/AES AFTER SEPARATION WITH TBP LEVEXTREL RESIN CHROMATOGRAPHY

摘要: 本章叙述了用萃取色层分离-水平式ICP/AES法测定U_3O_8中Hf,Zr,Sc,Th,Ag等杂质元素。U_3O_8样品用HNO_3-HF混合酸溶解,并用HCl转化成氯化铀酰后,通过以CL-TBP萃淋树脂为固定相,5mol/l HCl为流动相的萃取色层柱,将杂质元素与铀分离后,以水平式ICP为激发光源,在W-100型平面光栅摄谱仪上进行光谱测定。取样0.3g时,测定下限Hf,Zr,Th为0.23×10~(-6),Sc为0.023×10~(-6),Ag为0.04×10~(-6),重加回收率在84％～114％范围内,相对标准偏差低于10％。

Abstract: A method for the determination of trace Hf, Zr, Sc, Th and Ag in U_3O_8 isreported. The sample is dissolved in HNO_3--HF mixture and converted to UO_2Cl_2with HCl. The uranium is separated by TBP levextrel resin chromatography.The impurity elements in aqueous phase are determined by horizontal ICP/AES.With a sample of 0.3g, the determination limit of Hf, Zr, Th is 0.23×10~(-6), Sc is0.023×10~(-6), Ag is 0.24×10~(-6), the recovery for all the 5 elements is in the rangeof 84%--114%, the relative standard deviation (RSD) is less than 10%. Thismethod is simple, rapid, the determination limit is low and it may be useful forthe determination of impurity elements in the other uranium compounds too.