液液萃取–离子色谱法测定乏燃料后处理模拟料液中的叠氮酸  

Determination of hydrazoic acid in simulated nuclear fuel reprocessing liquid by liquid–liquid extraction–ion chromatography

作　　者：束玉珍 邓惟勤[1] 谈树苹[1] 吴继宗[1] 陶苗苗[1] SHU Yuzhen;DENG Weiqin;TAN Shuping;WU Jizong;TAO Miaomiao(China Institute of Atomic Energy,Beijing 102413,China)

机构地区：[1]中国原子能科学研究院,北京102413

出　　处：《化学分析计量》2018年第6期60-63,共4页Chemical Analysis And Meterage

摘　　要：建立乏燃料后处理模拟料液中叠氮酸的液液萃取–离子色谱测定方法。在相比1∶1的情况下,以30%TBP–煤油对1 g/L的叠氮酸进行萃取,将目标料液稀释10倍以上体积即硝酸浓度在0.3 mol/L以下,以提高叠氮酸根萃取率,同时降低硝酸、铀及其它金属离子的干扰;用浓度不低于2mmol/L的KOH溶液对叠氮酸根进行反萃取;用Dionex-AS11HC大容量阴离子色谱柱进行分离。叠氮酸的质量浓度在0.04～12μg/mL范围内与色谱峰面积呈良好的线性关系,线性相关系数(r^2)为0.999 4,对原始料液的检出限为0.27μg/mL。测定结果的相对标准偏差为2.17%(n=10),加标回收率为89.5%～109.0%。该方法灵敏度高,重复性好,抗杂质离子干扰,可用于乏燃料后处理料液中叠氮酸的测定。A liquid–liquid extraction–ion chromatography method for the determination of hydragoic acid in the simulated nuclear fuel reprocessing liquid was established.The experiment results showed that 30%TBP–kerosene was sufficient to extract 1 g/L azide with phase ratio of 1∶1.The target liquid was diluted more than 10 times,that is,the concentration of nitric acid was less than 0.3 mol/L.At this condition,the azide extraction rate was improved,while the interference of nitric acid,uranium and other metal ions was reduced.Azide could be stripped completely by KOH solution with concentration not less than 2 mmol/L.Dionex-AS11HC large-capacity anion column was used.The mass concentration of hydrazoic acid was linear with the chromatographic peak area in the range of 0.04–12μg/mL.The linear correlation coefficient(r2)was 0.999 4.The detection limit of raw liquid was 0.27μg/mL.The relative standard deviation of detection results was 2.17%(n=10),and the standard addition recovery was 89.5%–109.0%.The method has high sensitivity,good repeatability and resistance to impurity ion interference,it can be used for the analysis of hydrazoic acid in the nuclear fuel reprocessing liquid.

关 键 词：离子色谱法 萃取 叠氮酸 乏燃料后处理模拟料液 

分 类 号：O657.7[理学—分析化学]