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Institutional Repository [SANDBOX]
Technical University of Crete
Technical University of Crete
EN
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| URI: | http://purl.tuc.gr/dl/dias/B61974D9-0C71-48C0-A5E1-4D645F0576B7 | ||
| Year | 2018 | ||
| Type of Item | Peer-Reviewed Journal Publication | ||
| License |
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| Bibliographic Citation | D. Orazbayeva, B. Kenessov, E. Psillakis, D. Nassyrova and M. Bektassov, "Determination of transformation products of unsymmetrical dimethylhydrazine in water using vacuum-assisted headspace solid-phase microextraction," J. Chromatogr. A, vol. 1555, pp. 30-36, Jun. 2018. doi: 10.1016/j.chroma.2018.04.048 https://doi.org/10.1016/j.chroma.2018.04.048 | ||
| Appears in Collections |
A new, sensitive and simple method based on vacuum-assisted headspace solid-phase microextraction (Vac-HSSPME) followed by gas chromatography-mass-spectrometry (GC–MS), is proposed for the quantification of rocket fuel unsymmetrical dimethylhydrazine (UDMH) transformation products in water samples. The target transformation products were: pyrazine, 1-methyl-1H-pyrazole, N-nitrosodimethylamine, N,N-dimethylformamide, 1-methyl-1Н-1,2,4-triazole, 1-methyl-imidazole and 1H-pyrazole. For these analytes and within shorter sampling times, Vac-HSSPME yielded detection limits (0.5–100 ng L−1) 3–10 times lower than those reported for regular HSSPME. Vac-HSSPME sampling for 30 min at 50 °C yielded the best combination of analyte responses and their standard deviations (<15%). 1-Formyl-2,2-dimethylhydrazine and formamide were discarded because of the poor precision and accuracy when using Vac-HSSPME. The recoveries for the rest of the analytes ranged between 80 and 119%. The modified Mininert valve and Thermogreen septum could be used for automated extraction as it ensured stable analyte signals even after long waiting times (>24 h). Finally, multiple Vac-HSSME proved to be an efficient tool for controlling the matrix effect and quantifying UDMH transformation products.
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