后处理工艺中叠氮酸测定的离子色谱法

本工作研究肼及其衍生物与偏钒酸铵反应所生成的叠氮酸的单柱离子色谱测定法。首先用氢氧化钠中和样品中多余的酸，再采用VydacIC302柱、以1mmol/L邻苯二甲酸作淋洗液进行色谱分离，然后由电导检测器进行测定。该方法对N^-₃的检测下限为5μg/mL，N^-₃线性范围为5~201μg/mL，线性相关系数为0.9994。待测实际样品需稀释10倍，叠氮酸的检测下限随之升至51μg/mL。

Single-Column Ion Chromatography With Determination of Hydrazoic Acid Produced in Spent Nuclear Fuel Reprocessing

The reaction of hydrazine and its derivative with ammonium metavanadate may produce hydrazoic acid(HN₃). A single column ion chromatography is used for the determination of HN₃ after neutralizing the rest acid in the sample with sodium hydroxide. Chromatography separation of HN₃ is carried out on a 25 cm×0.46 cm (inside diameter) stainless steel column packed with Vydac IC302 ion Chromatography packing. The eluent is 1 mmol/L o-phthatic acid, and the ion is detected by conductivity detector. The detection limit in the presence chromatography is 5 μg/mL, the linear range is from 5 to 201 μg/mL, the linear correlation coefficient is 0.999 4, respectively. The analysis accuracy is 2% for standard sample, and the detection limit is 51 μg/mL for HN₃ in the real sample.