On-site gas chromatographic quantitation of transformation products of unsymmetrical dimethylhydrazine in soil using vacuum-assisted headspace solid-phase microextraction
Kurmanbayeva T. Bukenov B. Imangabassov A. Rymzhanova Z. Yermakhan M. Karimkyzy N. Smail A. Kenessov B.
August 2025Elsevier Inc.
Microchemical Journal
2025#215
Soil samples contaminated with residues of rocket fuel unsymmetrical dimethylhydrazine (UDMH) often require quick analysis, particularly after accidents with major spills. This study reports a novel green analytical method for on-site quantitation of UDMH transformation products (TPs) using vacuum-assisted headspace solid-phase microextraction (Vac-HSSPME) and portable gas chromatograph with nitrogen‑phosphorus detection (GC-NPD). To minimize matrix effects during Vac-HSSPME, analytes were preliminary extracted with distilled water that was experimentally proven advantageous over 1 M HCl and 1 M NaOH. During the on-site measurements at a fall site of the first stage of Proton-M carrier rocket in the Ulytau Region, Kazakhstan, screening was initially conducted by Vac-HSSPME from 1.00 g of soil at 50 °C without preliminary extraction. After screening, the contaminated soil samples (m = 1.00 g) were extracted with 10.0 mL distilled water and then centrifuged. Supernatants were subjected to Vac-HSSPME with 85 μm Car/PDMS fiber for 30 min at 50 °C under stirring. Matrix-matched external standard calibration plots were obtained by analyzing spiked aqueous extracts from soil collected at the same site where analytes were not detected during screening. Concentrations of the analytes determined in the samples were 6.9–150 μg/kg at 50 cm depth and 9.2–139 μg/kg (except for MTA and MFA) at 100 cm depth. The highest concentration (8500 μg/kg) was determined for MTA. The limits of detection (LODs) estimated from the obtained results were 3–60 μg/kg. The developed method is recommended for on-site quantitation of main UDMH TPs when rapid results are required.
Matrix-matched calibration , On-site soil analysis , Portable gas chromatography , SPME , Transformation products , Unsymmetrical dimethylhydrazine
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Center of Physical Chemical Methods of Research and Analysis, Faculty of Chemistry and Chemical Technology, Al-Farabi Kazakh National University, Almaty, Kazakhstan
Center of Physical Chemical Methods of Research and Analysis
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