核化学与放射化学
覈化學與放射化學
핵화학여방사화학
HE HUAXUE YU FANGSHE HUAXUE
2014年
z1期
27-34
,共8页
白雪%李定明%常志远%谈树苹%张倩慈
白雪%李定明%常誌遠%談樹蘋%張倩慈
백설%리정명%상지원%담수평%장천자
拉曼光谱%U(Ⅵ)定量%水相体系%有机相体系
拉曼光譜%U(Ⅵ)定量%水相體繫%有機相體繫
랍만광보%U(Ⅵ)정량%수상체계%유궤상체계
Raman spectra%the quantitatively detection of U(Ⅵ)%aqueous phase%organic phase
建立了Purex后处理工艺水相和有机相料液中 U(Ⅵ)的拉曼光谱分析方法。对于水相体系,870 cm-1处 UO2+2的拉曼谱峰强度与 U(Ⅵ)质量浓度在5.0~450.0 g/L范围内呈现良好的线性关系,r2=0.9999,检出限为1.2 g/L。增加仪器的积分时间可以使U(Ⅵ)的检出限降至0.2 g/L。硝酸、其他锕系元素与裂片元素的存在对 U(Ⅵ)的检测无影响。对于含0.5~4.0 mol/L硝酸的70.0 g/L U(Ⅵ)溶液,6次检测的相对标准偏差均不高于1.4%。进行含有裂片元素的重加回收实验,重加回收率在98.3%~101.6%之间。在有机相体系,拉曼信号强度与 U(Ⅵ)质量浓度在5.0~107.0 g/L 范围内呈现线性关系,r2=0.9990,检出限为0.7 g/L。该方法具有测定简便、无需考虑干扰、绿色无损等优点,可实现现场的快速检测,适用于水相和有机相中常量U(Ⅵ)的定量检测。
建立瞭Purex後處理工藝水相和有機相料液中 U(Ⅵ)的拉曼光譜分析方法。對于水相體繫,870 cm-1處 UO2+2的拉曼譜峰彊度與 U(Ⅵ)質量濃度在5.0~450.0 g/L範圍內呈現良好的線性關繫,r2=0.9999,檢齣限為1.2 g/L。增加儀器的積分時間可以使U(Ⅵ)的檢齣限降至0.2 g/L。硝痠、其他錒繫元素與裂片元素的存在對 U(Ⅵ)的檢測無影響。對于含0.5~4.0 mol/L硝痠的70.0 g/L U(Ⅵ)溶液,6次檢測的相對標準偏差均不高于1.4%。進行含有裂片元素的重加迴收實驗,重加迴收率在98.3%~101.6%之間。在有機相體繫,拉曼信號彊度與 U(Ⅵ)質量濃度在5.0~107.0 g/L 範圍內呈現線性關繫,r2=0.9990,檢齣限為0.7 g/L。該方法具有測定簡便、無需攷慮榦擾、綠色無損等優點,可實現現場的快速檢測,適用于水相和有機相中常量U(Ⅵ)的定量檢測。
건립료Purex후처리공예수상화유궤상료액중 U(Ⅵ)적랍만광보분석방법。대우수상체계,870 cm-1처 UO2+2적랍만보봉강도여 U(Ⅵ)질량농도재5.0~450.0 g/L범위내정현량호적선성관계,r2=0.9999,검출한위1.2 g/L。증가의기적적분시간가이사U(Ⅵ)적검출한강지0.2 g/L。초산、기타아계원소여렬편원소적존재대 U(Ⅵ)적검측무영향。대우함0.5~4.0 mol/L초산적70.0 g/L U(Ⅵ)용액,6차검측적상대표준편차균불고우1.4%。진행함유렬편원소적중가회수실험,중가회수솔재98.3%~101.6%지간。재유궤상체계,랍만신호강도여 U(Ⅵ)질량농도재5.0~107.0 g/L 범위내정현선성관계,r2=0.9990,검출한위0.7 g/L。해방법구유측정간편、무수고필간우、록색무손등우점,가실현현장적쾌속검측,괄용우수상화유궤상중상량U(Ⅵ)적정량검측。
A new method via Raman spectroscopy for determination of U(Ⅵ)in aqueous and organic solutions was developed.The concentration of U(Ⅵ)can be quantified by the Raman band of UO2+2 ,which is 870 cm-1 in aqueous solutions and 860 cm-1 in organic solutions.In the aqueous phase,a good linear relationship is obtained between the Raman signal and con-centration of U(Ⅵ)in the range of 5.0-450.0 g/L,with the r2= 0.999 9.The detection limit is 1.2 g/L.The detection limit can be reduced to 0.2 g/L by increasing the integration time.The existence of nitric acid and fission products has no effect on the detection of U(Ⅵ).The sr is no more than 1.4%(n=6)for detection of 70.0 g/L U(Ⅵ),with 0.5-4.0 mol/L HNO3 .The recoveries are in the range of 98.3%-101.6%.In organic solutions, the linearity is observed in the range of 5.0-107.0 g/L with r2=0.999 0 and a limit of detec-tion of 0.7 g/L.With the advantage of simple,rapid,green and no interference of internal substance,the method is applicable for in situ detection of U (Ⅵ)in aqueous and organic solutions.