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Determination of 1,1-Dimethylhydrazine in Water with High Pressure Liquid Chromatography and Spectrophotometric Detection Using Micellar Catalysisстатья
Дата последнего поиска статьи во внешних источниках: 8 апреля 2022 г.
- Авторы: Timchenko Yu V., Belikova I.V., Smolenkov A.D., Pirogov A.V., Shpigun O.A.
- Журнал: Inorganic Materials
- Том: 57
- Номер: 14
- Год издания: 2021
- Издательство: Maik Nauka/Interperiodica Publishing
- Местоположение издательства: Russian Federation
- Первая страница: 47
- Последняя страница: 55
- DOI: 10.1134/S0020168521140119
- Аннотация: The possibility of improving the detection of 1,1-dimethylhydrazine (unsymmetrical dimethylhydrazine, UDMH) by HPLC-SP under preliminary derivatization with 2-nitrobenzaldehyde (2NBA) and4-nitrobenzaldehyde (4NBA) in water with micellar catalysis is studied. The conditions for the derivatizationof UDMH (pH, concentrations of reagent and surfactant, temperature, and reaction time) are optimized.The derivatization reactions proceed completely at pH 9 in the presence of 87 mM sodium dodecyl sulfate(SDDS) solution and an excess of reagents at room temperature for 45 and 30 min for 2NBA and 4NBA,respectively. Quantitative yield of the reaction products, which is found by the absence of UDMH in the reaction mixture with ion chromatography, is achieved under these conditions. The micellar catalysis allows derivatization under milder conditions and provides the completeness of the reaction under low UDMH concentrations, which expands the linear range of the concentrations determined. A ZORBAX Eclipse Plus C18chromatographic column (150 × 3.0 mm × 3.5 μm) was used for HPLC-SP detection of UDMH, and a mixture of acetonitrile and 10 mM ammonia buffer solution at pH 7 (50/50, vol %) at a flow rate of 0.7 mL/minin isocratic mode was used as a mobile phase. The 2NBA and 4NBA dimethylhydrazones were detected atthe wavelengths of 308 and 394 nm, respectively. The detection limits for UDMH (S/N = 3) were 3 and1.5 μg/L for 2NBA and 4NBA, respectively. The chromatographic analysis time was 15 min. The methoddeveloped for water analysis provides a simple, sensitive, and reproducible detection of UDMH in the concentration range of 5–1000 μg/L by the HPLC-SP method without additional concentration.
- Добавил в систему: Тимченко Юрий Валерьевич
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