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作 者:付建丽[1] 邓惟勤[1] 谈树苹[1] 吴继宗[1] 赵立飞[1]
机构地区:[1]中国原子能科学研究院放射化学研究所,北京102413
出 处:《核化学与放射化学》2015年第1期24-30,共7页Journal of Nuclear and Radiochemistry
摘 要: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MnO4^-,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。A simple and sensitive method for the measurement of residual oxalate in plutonium(Ⅳ) oxalate precipitation mother liquor was established by using ion chromatography. After the sample was diluted, at first, hydroxyurea(HU) was used to deoxidize MnO4^-, 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 5.3μg/L. The proposed method was utilized to detect the trace oxalate in simulative plutonium(Ⅳ) oxalate precipitation mother liquor, and the result shows that the recovery of 0.5mg/L oxalate is 88%-92%,sr 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.
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