Simultaneous Determination of Hydrazine, Methylhydrazine and 1,1-Dimethylhydrazine in Waters by HPLC with Spectrophotometric Detection Using Catalysis to Obtain Derivatives

• Published in: Journal of analytical chemistry (New York, N.Y.) N.Y.), 2021-10, Vol.76 (10), p.1163-1171
• Main Authors: Timchenko, Yu. V., Apenkina, A. V., Smolenkov, A. D., Pirogov, A. V., Shpigun, O. A.
• Format: Article
• Language: English
• Subjects: Analytical Chemistry; Backup software; Benzaldehyde; Catalysis; Chemical tests and reagents; Chemistry; Chemistry and Materials Science; Dimethylhydrazines; High performance liquid chromatography; Methylhydrazine; Reagents; Room temperature; Sodium dodecyl sulfate; Spectrophotometry; Sulfates; Surface active agents
• ISSN: 1061-9348; 1608-3199
• DOI: 10.1134/S1061934821100117

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.