Gas chromatographic determination of 1,1-dimethylhydrazine in water samples by solid-phase microextraction with derivatization

  • Madi Abilev al-Farabi Kazakh National University
  • Bulat Kenessov al-Farabi Kazakh National University http://orcid.org/0000-0001-8541-0903
  • Svetlana Batyrbekova al-Farabi Kazakh National University
Keywords: 1, 1-dimethylhydrazine, acetone, acetone dimethylhydrazone, derivatization, solid phase microextraction, gas chromatography, mass-spectrometry, water, analysis

Abstract

1,1-Dimethylhydrazine (1,1-DMH) used as a rocket fuel component is highly reactive and unstable compound. It greatly complicates its accurate and express determination in environmental samples. Goal of this work was to develop a method for its express determination in water samples based on solid-phase microextraction with preliminary derivatization. Acetone was selected as reagent for derivatization because during its reaction with 1,1-DMH, volatile and hydrophobic acetone dimethylhydrazone (ADMH) was formed. It was established that fiber based on 100-micron polydimethylsiloxane provides the most efficient extraction of ADMH from water at extraction time 2 min. Optimal concentration of acetone was 30 mg/mL. The minimum time for reaction of 1,1-DMH with acetone is 10 minutes. Addition of acids and alkali reduced ADMH response that may be caused by degradation of 1,1-DMH and reduction of derivatization rate. Addition of salt allowed to increase the response of ADMH however made impossible the quantitative determination of 1,1-DMH. Dependence of ADMH response on the concentration of 1,1-DMH at optimized parameters is linear in the concentrations range of 0.1-100 mg/L and can be used for quantitative determination of 1,1-DMH in water. Detection limit of the developed method is 0.02 mg/L. Reproducibility index of the method in the whole range of concentrations did not exceed 7%, accuracy index - 15%. Developed method is simple, inexpensive, accurate, automated and can be recommended for implementation in laboratories conducting environmental monitoring in areas of rocket-carriers fall.

Author Biographies

Madi Abilev, al-Farabi Kazakh National University
Center of Physical Chemical Methods of Research and Analysis, Ph.D. student
Bulat Kenessov, al-Farabi Kazakh National University
Center of Physical Chemical Methods of Research and Analysis, Vice-Director on International Relations, Ph.D., Associate Professor
Svetlana Batyrbekova, al-Farabi Kazakh National University
Center of Physical Chemical Methods of Research and Analysis, Chief Scientist

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Published
2014-10-31
How to Cite
Abilev, M., Kenessov, B., & Batyrbekova, S. (2014). Gas chromatographic determination of 1,1-dimethylhydrazine in water samples by solid-phase microextraction with derivatization. Chemical Bulletin of Kazakh National University, (3), 91-102. https://doi.org/https://doi.org/10.15328/chemb_2014_391-102
Section
Analytical Chemistry