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
束玉珍,邓惟勤,谈树苹,吴继宗,陶苗苗
中国原子能科学研究院,北京 102413
Determination of hydrazoic acid in simulated nuclear fuel reprocessing liquid by liquid-liquid extraction-ion chromatography
束玉珍,邓惟勤,谈树苹,吴继宗,陶苗苗
China Institute of Atomic Energy, Beijing 102413, China
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2 mmol/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0.04~12 μg/mL范围内与色谱峰面积呈良好的线性关系,线性相关系数(r2)为0.9994,对原始料液的检出限为0.27 μg/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。
Abstract: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 0.04-12 μg/mL. The linear correlation coefficient (r2) was 0.9994. The detection limit of raw liquid was 0.27 μg/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
Keywords:ion chromatography; extraction; hydrazoic acid; simulated nuclear fuel reprocessing liquid
本文引用格式:
束玉珍,邓惟勤,谈树苹,等.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.[J].化学分析计量,2018,27(6):60-63.
SHU Y H,DENG W Q,TAN S P,etal. Determination of hydrazoic acid in nuclear fuel reprocessing liquid by liquid-liquid extraction-ion chromatography[J]. Chemical analysis and meterage,2018,27(6):60-63.
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