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Determination of 1,1-Dimethylhydrazine in Water with High Pressure Liquid Chromatography and Spectrophotometric Detection Using Micellar Catalysis

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Abstract

The possibility of improving the detection of 1,1-dimethylhydrazine (unsymmetrical dimethylhydrazine, UDMH) by HPLC-SPD under preliminary derivatization with 2-nitrobenzaldehyde (2NBA) and 4‑nitrobenzaldehyde (4NBA) in water with micellar catalysis is studied. The conditions for the derivatization of 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 (SDS) 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 C18 chromatographic column (150 × 3.0 mm × 3.5 μm) was used for HPLC-SPD 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/min in isocratic mode was used as a mobile phase. The 2NBA and 4NBA dimethylhydrazones were detected at the wavelengths of 308 and 394 nm, respectively. The detection limits for UDMH (S/N = 3) were 3 and 1.5 μg/L for 2NBA and 4NBA, respectively. The chromatographic analysis time was 15 min. The method developed for water analysis provides a simple, sensitive, and reproducible detection of UDMH in the concentration range of 5–1000 μg/L by the HPLC-SPD method without additional concentration.

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Funding

This work was financially supported by the Russian Foundation for Basic Research (project 19-33-90120).

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Authors and Affiliations

  1. Moscow State University, Moscow, Russia

    Yu. V. Timchenko, I. V. Belikova, A. D. Smolenkov, A. V. Pirogov & O. A. Shpigun

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  1. Yu. V. Timchenko
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  2. I. V. Belikova
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  3. A. D. Smolenkov
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  4. A. V. Pirogov
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  5. O. A. Shpigun
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Correspondence to Yu. V. Timchenko.

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Translated by A. Tulyabaev

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Timchenko, Y.V., Belikova, I.V., Smolenkov, A.D. et al. Determination of 1,1-Dimethylhydrazine in Water with High Pressure Liquid Chromatography and Spectrophotometric Detection Using Micellar Catalysis. Inorg Mater 57, 1413–1421 (2021). https://doi.org/10.1134/S0020168521140119

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