The use of glyoxal and glyoxylic acid to determine N- and N,N-alkyl-substituted hydrazines by liquid chromatographyстатья

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Дата последнего поиска статьи во внешних источниках: 4 февраля 2014 г.

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[1] The use of glyoxal and glyoxylic acid to determine n- and n,n-alkyl-substituted hydrazines by liquid chromatography / R. S. Smirnov, A. D. Smolenkov, T. A. Bolotnik, O. A. Shpigun // Moscow University Chemistry Bulletin. — 2013. — Vol. 68, no. 1. — P. 17–22. Using chromatography and spectrophotometry for investigation of reaction of 1,1-dimethylhydrazine (UDMH), methylhydrazine (MH) and 2-hydroxyethylhydrazine (HEH) with excess of glyoxal (Gl) and glyoxylic acid (GlA) in aqueous solutions it was shown that corresponding monohydrazone was produced as the single derivatization product. The derivatization reaction is quantitative within 20 min at pH 3.5 and at 25 or 40 oC temperature for Gl and GlA respectively. Electronic absorption spectra of derivatives have maxima in the range of 275–305 nm. The conditions for simultaneous determination of hydrazines in water samples by RP–HPLC with UV-detection with preliminary derivatization were proposed. The derivatives were separated on a Zorbax SB-C18 (150×4.6 mm) column with a mobile phase of 20 mM phosphate buffer solution (pH 3.5) – (2–5)% acetonitrile. The limits of detection were 0.25–0.5 or 0.4–0.7 μg/L for derivative of Gl and GlA respectively. [ DOI ]

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