Abstract

A simple, rapid, and sensitive method is developed for the simultaneous determination of hydrazine, methylhydrazine, and 1,1-dimethylhydrazine in waters based on precolumn derivatization with benzaldehyde and the determination of the resulting products by reversed-phase HPLC with spectrophotometric detection at 300, 282, and 298 nm, respectively. The effect of imine and micellar catalysis is applied for the first time to obtain hydrazine derivatives on their simultaneous presence. The conditions of derivatization are chosen: the type, pH and concentration of the buffer system; the concentration of the reagent and the surfactant; and the temperature and duration of the reaction. It is found that the derivatization reaction proceeds completely at pH 9.4 in the presence of a catalytic system based on 0.6 M ammonium and 87 mM sodium dodecyl sulfate, and also 3.5 mM reagent at room temperature for 5 min. The quantitative yield of the derivatization products is confirmed by ion chromatography. The limits of detection (S/N = 3) without additional preconcentration are 0.3, 2.3, and 1.3 μg/L, and the linearity range is 1–500, 7–1000, and 5–1000 μg/L for hydrazine, methylhydrazine, and 1,1-dimethylhydrazine, respectively.

中文翻译：

---

HPLC 与分光光度法检测同时测定水中的肼、甲基肼和 1,1-二甲基肼，使用催化获得衍生物

摘要

建立了一种简单、快速、灵敏的方法，以苯甲醛柱前衍生化为基础，同时测定水中的肼、甲基肼和 1,1-二甲基肼，并通过反相 HPLC 测定所得产物，在 300 分光光度法检测分别为 、282 和 298 nm。首次应用亚胺和胶束催化作用获得肼衍生物同时存在。选择衍生条件：缓冲系统的类型、pH值和浓度；试剂和表面活性剂的浓度；以及反应的温度和持续时间。发现在基于 0.6 M 铵和 87 mM 十二烷基硫酸钠的催化体系存在下，衍生反应在 pH 9.4 下完全进行，以及 3.5 mM 试剂在室温下放置 5 分钟。衍生产物的定量产率通过离子色谱法确认。没有额外预浓缩的检测限 (S/N = 3) 为 0.3、2.3 和 1.3 µg/L，肼、甲基肼、甲肼的线性范围为 1–500、7–1000 和 5–1000 µg/L。和 1,1-二甲基肼，分别。