光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2010年
2期
523-527
,共5页
龚琦%陈杰%吉日文%潘雪珍%伍娟
龔琦%陳傑%吉日文%潘雪珍%伍娟
공기%진걸%길일문%반설진%오연
高纯氧化镱%强酸型离子交换纤维%分离%稀土杂质%ICP-AES
高純氧化鐿%彊痠型離子交換纖維%分離%稀土雜質%ICP-AES
고순양화의%강산형리자교환섬유%분리%희토잡질%ICP-AES
High purity ytterbium oxide%Strong acid ion exchange fiber%Separation%Rare earth impurities%ICP-AES
以强酸型离子交换纤维柱分离寓集高纯Yb_2O_3中La,Nd,Eu和Gd等痕量杂质元素,并用Optima5300 DV ICP-AES测定分离寓集后的这4种元素.供试纤维对Yb的动态吸附容量为134 mg·g~(-1),4.0 g纤维柱的分离条件为:pH 3.00的试液以1.0 mL·min~(-1)流速上柱后,分离柱先以流速为1.5 mL·min~(-1)的pH 3.00 HNO_3溶液80 mL预淋洗,再以同样流速pH 5.00的0.01 mol·L~(-1) EDTA铵溶液淋洗.结果表明:10 mg Yb与各为0.100 μg的La,Nd,Eu和Gd能达到基线分离;分离含100 mg Yb的试液后,在杂质富集液中Yb的残留浓度仅为0.017 1 μg·mL~(-1).研究显示,当待测试液中Yb_2O_3的浓度小于100 μg·mL~(-1)(如Yb 87.8 μg·mL~(-1))时,它对测定La,Nd,Eu和Gd等杂质元素的基体干扰可以忽略不计.富集倍数分别为La_2O_3 3.68×10~5,Nd_2O_3 4.20×10~5,Eu_2O_3 3.82×10~5,Gd_2O_3 4.01×10~5.方法检出限分别为La_2O_3 0.005 0 pg·mL~(-1),Nd_2O_3 0.014 pg·mL~(-1),Eu_2O_3 0.001 8 pg·mL~(-1),Gd_2O_3 0.008 2 pg·mL~(-1).本方法已用于99.99%Yb_2O_3样品中4种稀土杂质的测定,标准加入的平均回收率分别为La_2O_3 94.2%,Nd_2O_3 107%,Eu_2O_3 97.8%,Gd_2O_3 102%,RSD(%,n=5)分别为La_2O_3 6.2,Nd_2O_3 5.9,Eu_2O_3 7.3,Gd_2O_3 2.5,校正曲线不需进行Yb的基体匹配,分析周期为4 h.
以彊痠型離子交換纖維柱分離寓集高純Yb_2O_3中La,Nd,Eu和Gd等痕量雜質元素,併用Optima5300 DV ICP-AES測定分離寓集後的這4種元素.供試纖維對Yb的動態吸附容量為134 mg·g~(-1),4.0 g纖維柱的分離條件為:pH 3.00的試液以1.0 mL·min~(-1)流速上柱後,分離柱先以流速為1.5 mL·min~(-1)的pH 3.00 HNO_3溶液80 mL預淋洗,再以同樣流速pH 5.00的0.01 mol·L~(-1) EDTA銨溶液淋洗.結果錶明:10 mg Yb與各為0.100 μg的La,Nd,Eu和Gd能達到基線分離;分離含100 mg Yb的試液後,在雜質富集液中Yb的殘留濃度僅為0.017 1 μg·mL~(-1).研究顯示,噹待測試液中Yb_2O_3的濃度小于100 μg·mL~(-1)(如Yb 87.8 μg·mL~(-1))時,它對測定La,Nd,Eu和Gd等雜質元素的基體榦擾可以忽略不計.富集倍數分彆為La_2O_3 3.68×10~5,Nd_2O_3 4.20×10~5,Eu_2O_3 3.82×10~5,Gd_2O_3 4.01×10~5.方法檢齣限分彆為La_2O_3 0.005 0 pg·mL~(-1),Nd_2O_3 0.014 pg·mL~(-1),Eu_2O_3 0.001 8 pg·mL~(-1),Gd_2O_3 0.008 2 pg·mL~(-1).本方法已用于99.99%Yb_2O_3樣品中4種稀土雜質的測定,標準加入的平均迴收率分彆為La_2O_3 94.2%,Nd_2O_3 107%,Eu_2O_3 97.8%,Gd_2O_3 102%,RSD(%,n=5)分彆為La_2O_3 6.2,Nd_2O_3 5.9,Eu_2O_3 7.3,Gd_2O_3 2.5,校正麯線不需進行Yb的基體匹配,分析週期為4 h.
이강산형리자교환섬유주분리우집고순Yb_2O_3중La,Nd,Eu화Gd등흔량잡질원소,병용Optima5300 DV ICP-AES측정분리우집후적저4충원소.공시섬유대Yb적동태흡부용량위134 mg·g~(-1),4.0 g섬유주적분리조건위:pH 3.00적시액이1.0 mL·min~(-1)류속상주후,분리주선이류속위1.5 mL·min~(-1)적pH 3.00 HNO_3용액80 mL예림세,재이동양류속pH 5.00적0.01 mol·L~(-1) EDTA안용액림세.결과표명:10 mg Yb여각위0.100 μg적La,Nd,Eu화Gd능체도기선분리;분리함100 mg Yb적시액후,재잡질부집액중Yb적잔류농도부위0.017 1 μg·mL~(-1).연구현시,당대측시액중Yb_2O_3적농도소우100 μg·mL~(-1)(여Yb 87.8 μg·mL~(-1))시,타대측정La,Nd,Eu화Gd등잡질원소적기체간우가이홀략불계.부집배수분별위La_2O_3 3.68×10~5,Nd_2O_3 4.20×10~5,Eu_2O_3 3.82×10~5,Gd_2O_3 4.01×10~5.방법검출한분별위La_2O_3 0.005 0 pg·mL~(-1),Nd_2O_3 0.014 pg·mL~(-1),Eu_2O_3 0.001 8 pg·mL~(-1),Gd_2O_3 0.008 2 pg·mL~(-1).본방법이용우99.99%Yb_2O_3양품중4충희토잡질적측정,표준가입적평균회수솔분별위La_2O_3 94.2%,Nd_2O_3 107%,Eu_2O_3 97.8%,Gd_2O_3 102%,RSD(%,n=5)분별위La_2O_3 6.2,Nd_2O_3 5.9,Eu_2O_3 7.3,Gd_2O_3 2.5,교정곡선불수진행Yb적기체필배,분석주기위4 h.
In the present paper,trace La,Nd,Eu and Gd were separated and enriched with strong acid ion exchange fiber column from high purity Yb_2O_3,and then determined by Optima 5 300 DV ICP-AES.The ion exchange fiber's breakthrough capacity for Yb was 134 mg·g~(-1).The separation condition using 4.0 g fiber column was that after the test solution(ph=3.0)was fed into the ion exchange fiber column at 1.0 mL·min~(-1),the column was pre-leached by dilute nitric acid(Ph=3.00)of 80 mL at 1.5 mL·min~(-1) at first,and then was eluted by 0.01 mol·L~(-1) ammonium EDTA(Ph=5.00)at the same flow rate.The results showed that 10 mg Yb could reach the baseline separation with 0.100 μg of the four rare earth impurities,and after 100 mg Yb in feed solution had been separated,only 0.017 1 μg·mL~(-1) Yb remained in the impurities enriched effluent.When the concentration of Yb_2O_3 is less than 100 μg·mL~(-1)(87.8 μg·mL~(-1) Yb),the matrix interference from Yb on withdetermination of La,Nd,Eu and Gd can be neglected.The enrichment factors were 3.68×10~5 for La_2O_3,4.20×10~5 for Nd_2O_3,3.82×10~5 for Eu_2O_3,and 4.01×10~5 for Gd_2O_3,and the detection limits of the method were 0.005 0,0.014,0.001 8 and 0.008 2 pg ·mL~(-1) for La_2O_3,Nd_2O_3,Eu_2O_3 and Gd_2O_3 respectively.The proposed method was applied to the analysis of 99.99% Yb_2O_3 with RSD(%,n=5)of 6.2,5.9,7.3 and 2.5 for La_2O_3,Nd_2O_3,Eu_2O_3 and Gd_2O_3 respectively,and the average recoveries of standard addition were 94.2%,107%,97.8% and 102% for La_2O_3,Nd_2O_3,Eu_2O_3 and Gd_2O_3 respectively.The calibration curve did not need matrix matching with Yb,and the analysis period was within 4 hour.
