Chromatographia

, Volume 80, Issue 6, pp 931–940 | Cite as

Quantification of Transformation Products of Unsymmetrical Dimethylhydrazine in Water Using SPME and GC-MS

  • Nadezhda V. Bakaikina
  • Bulat Kenessov
  • Nikolay V. Ul’yanovskii
  • Dmitry S. Kosyakov
  • Sergey A. Pokryshkin
  • Miras Derbissalin
  • Zhailaubay K. Zhubatov
Original

Abstract

Quantification of trace concentrations of transformation products of rocket fuel unsymmetrical dimethylhydrazine (UDMH) in water requires complex analytical instrumentation and tedious sample preparation. The goal of this research was to develop a simple and automated method for sensitive quantification of UDMH transformation products in water using headspace (HS) solid-phase microextraction (SPME) in combination with GC-MS and GC-MS/MS. HS SPME is based on extraction of analytes from a gas phase above samples by a micro polymer coating followed by a thermal desorption of analytes in a GC inlet. Extraction by 85 µm Carboxen/polydimethylsiloxane fiber at 50 °C during 60 min provides the best combination of sensitivity and precision. Tandem mass spectrometric detection with positive chemical ionization improves method accuracy and selectivity. Detection limits of twelve analytes by GC-MS/MS with chemical ionization are about 10 ng L−1. GC-MS provides similar detection limits for five studied analytes; however, the list of analytes detected by this method can be further expanded. Accuracies determined by GC-MS were in the range of 75–125% for six analytes. Compared to other available methods based on non-SPME sample preparation approaches (e.g., liquid–liquid and solid-phase extraction), the developed method is simpler, automated and provides lower detection limits. It covers more UDMH transformation products than available SPME-based methods. The list of analytes could be further expanded if new standards become available. The developed method is recommended for assessing water quality in the territories affected by space activities and other related studies.

Keywords

SPME GC-MS Quantification Transformation products Dimethylhydrazine Water 

Supplementary material

10337_2017_3286_MOESM1_ESM.docx (22 kb)
Supplementary material 1 (DOCX 21 kb)

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Copyright information

© Springer-Verlag Berlin Heidelberg 2017

Authors and Affiliations

  • Nadezhda V. Bakaikina
    • 1
  • Bulat Kenessov
    • 1
  • Nikolay V. Ul’yanovskii
    • 2
  • Dmitry S. Kosyakov
    • 2
  • Sergey A. Pokryshkin
    • 2
  • Miras Derbissalin
    • 1
  • Zhailaubay K. Zhubatov
    • 3
  1. 1.Faculty of Chemistry and Chemical Technology, Center of Physical Chemical Methods of Research and AnalysisAl-Farabi Kazakh National UniversityAlmatyKazakhstan
  2. 2.Core Facility Center ‘Arktika’Northern (Arctic) Federal UniversityArkhangelskRussia
  3. 3.Scientific Research Center “Garysh-Ecologiya”Aerospace Committee of the Ministry of Investments and Development of the Republic of KazakhstanAlmatyKazakhstan

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