CAJ | 학술논문

采用离子色谱作为检测仪器,建立了简便、灵敏的测定草酸钚沉淀母液中残留草酸根的新方法。样品稀释后,首先用羟基脲(HU)还原破坏MnO-4,再过H柱去除阳离子,然后采用5L/min氮吹55℃蒸发的方法去除硝酸干扰,离子色谱仪进行检测。标准曲线在0.01~50mg/L范围内线性良好,相关系数r2=0.996,草酸根的检出限为5.3μg/L。采用建立的方法对模拟样品进行重加回收实验,草酸根回收率在88%~92%之间,0.5mg/L草酸根6次测定的sr=4.0%。该方法操作简单、灵敏度高,为草酸钚沉淀母液中残留草酸根的检测提供了可行的分析方法。
채용리자색보작위검측의기,건립료간편、령민적측정초산비침정모액중잔류초산근적신방법。양품희석후,수선용간기뇨(HU)환원파배MnO-4,재과H주거제양리자,연후채용5L/min담취55℃증발적방법거제초산간우,리자색보의진행검측。표준곡선재0.01~50mg/L범위내선성량호,상관계수r2=0.996,초산근적검출한위5.3μg/L。채용건립적방법대모의양품진행중가회수실험,초산근회수솔재88%~92%지간,0.5mg/L초산근6차측정적sr=4.0%。해방법조작간단、령민도고,위초산비침정모액중잔류초산근적검측제공료가행적분석방법。
A simple and sensitive method for the measurement of residual oxalate in plutoni-um(Ⅳ)oxalate precipitation mother liquor was established by using ion chromatography. After the sample was diluted,at first,hydroxyurea (HU)was used to deoxidize MnO-4 , then the sample flowed through H column to remove of cations,and was followed by the evaporation at 55 ℃-5 L/min nitrogen purge to eliminate the interference of HNO3 .Finally, the disposed sample was determined by ion chromatography.The standard curves of oxalate show good linearity with r 2 =0.996 in the range of 0.01-50 mg/L,and the detection limits of oxalate is 5.3 μg/L.The proposed method was utilized to detect the trace oxalate in simula-tive plutonium(Ⅳ)oxalate precipitation mother liquor,and the result shows that the recov-ery of 0.5 mg/L oxalate is 88%-92%,s r is 4.0%(n=6).This method is simple,accurate and highly sensitive.Therefore,it provides a viable method for determining the residual oxalate in plutonium(Ⅳ)oxalate precipitation mother liquor.