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Determination of transformation products of unsymmetrical dimethylhydrazine in water using vacuum-assisted headspace solid-phase microextraction

Orazbayeva Dina, Kenessov Bulat, Psyllaki Eleftheria, Nassyrova Dayana, Bektassov Marat

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URI: http://purl.tuc.gr/dl/dias/B61974D9-0C71-48C0-A5E1-4D645F0576B7
Έτος 2018
Τύπος Δημοσίευση σε Περιοδικό με Κριτές
Άδεια Χρήσης
Λεπτομέρειες
Βιβλιογραφική Αναφορά 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
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Περίληψη

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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