Quantification of transformation products of unsymmetrical dimethylhydrazine in aqueous extracts from soil
based on vacuum-assisted headspace solid-phase microextraction

et al. 2022

Environ Sci Pollut Res

Self Cite

Quanti cation of unsymmetrical dimethylhydrazine (UDMH) transformation products (TPs) in solid samples is an important stage in monitoring of environmental pollution caused by heavy rockets launches. The new method for simultaneous quanti cation of UDMH TPs in sand samples using vacuum-assisted headspace solid-phase microextraction (Vac-HSSPME) followed by gas chromatography-mass spectrometry (GC-MS) is proposed. Compared to regular HSSPME, Vac-HSSPME yielded 1.3-4.8 times higher responses for NDMA, MTA and PAl. Increasing air-evacuation time from 20 to 120 s at 23 ºC resulted in decreased responses of analytes by 25-46%. Freezing of samples (-30 ºC) had negligible effect on responses of analytes at air-evacuation time 20 s. The best combination of responses of analytes and their RSDs was achieved after air-evacuation of a sample (m = 1.00 g) for 20 s at 23 ºC, incubation for 30 min and 30-min extraction at 40°C by Car/PDMS ber. Vac-HSSPME provided linear calibration plots in studied ranges of concentrations with coe cients of determination ranging from 0.9912 to 0.9938. The limits of detection for spiked sand samples varied from 0.035 to 3.6 ng g − 1 .Spike recoveries of target analytes from sand samples were 84-97% with RSDs 1-11%. The developed method was successfully tested in the experiment on studying losses of analytes from open vials with model sand spiked with UDMH TPs. The developed method can be recommended for analysis of trace concentrations of UDMH TPs when studying their transformation, migration and distribution in contaminated sand.

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Quantification of trace transformation products of rocket fuel unsymmetrical dimethylhydrazine in sand using vacuum-assisted headspace solid-phase microextraction

Zhakupbekova

Baimatova

et al. 2022

Environ Sci Pollut Res

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“…In 2012, Psillakis et al presented the theoretical model describing the pressure dependence of the so-called vacuum-assisted HS-SPME (Vac-HS-SPME) for water [12,13], and in 2015, for solid matrices [14]. Vac-HS-SPME has been successfully applied to a variety of analytes and matrices including solids [15][16][17] and complex food matrices like wine [18], dairy products [19,20], and extra virgin olive oil [21]. In 2017, the applicability of the approach was expanded by Trujillo-Rodríguez et al to headspace SDME (HS-SDME) and the resulting method, termed vacuum-assisted HS-SDME (Vac-HS-SDME), yielded shorter equilibration times for short-chain free fatty acids compared with atmospheric pressure sampling [22].…”

Section: Introductionmentioning

confidence: 99%

The effect of vacuum: an emerging experimental parameter to consider during headspace microextraction sampling

2020

Anal Bioanal Chem

The effect of vacuum is an emerging experimental parameter to consider during optimization of a variety of headspace microextraction methodologies. The positive effect of vacuum was initially demonstrated for headspace solid-phase microextraction and was recently expanded to single-drop microextraction and higher capacity sorbents i.e. stir bar sorptive extraction. In all cases, sampling under vacuum greatly accelerated the extraction kinetics of analytes exhibiting long equilibration times under atmospheric pressure. At the same time, the extraction of analytes that reached equilibrium fast was not affected. In all optimized methods, extraction times were greatly reduced and/or sampling temperatures were lower to those reported with the standard methodology under atmospheric pressure. This work succinctly overviews the effect of vacuum on the different headspace microextraction technologies reported so far. The fundamental concepts describing the pressure dependence of each methodology are pulled together and presented in a simplified manner. The latest findings on the combined effects of vacuum and several selected experimental parameters typically examined during method optimization are then presented and the practical aspects of past outcomes are highlighted. The discussion also includes the air-evacuation step and the analysis of complex matrices. This article is intended for readers who are either new to the field of vacuum headspace microextraction sampling or its use and want to exploit this powerful approach.

“…Trace amounts of UDMH transformation products (TPs) in soils can be detected several decades after the landing of rocket stage (Kenessov et al 2010b(Kenessov et al , 2012Rodin et al 2012;Kolesnikov 2014). Up until today, more than fty UDMH TPs were identi ed (Rodin et al 2008 Most prospective sample preparation methods for determination of UDMH TPs in soil samples (Kenessov et al 2010a(Kenessov et al , 2011Yegemova et al 2015;Bakaikina et al 2018;Orazbayeva et al 2018b) are based on headspace solid-phase microextraction (HSSPME). HSSPME is a simple, low cost and environmentally friendly technique that is widely used in a variety of applications.…”

Section: The Total Percentage Of Unsuccessful Launches Of Proton Rockmentioning

confidence: 99%

Quantification of trace transformation products of rocket fuel unsymmetrical dimethylhydrazine in sand using vacuum-assisted headspace solid-phase microextraction

Zhakupbekova

Baimatova

et al. 2021

Preprint

Self Cite

Quantification of unsymmetrical dimethylhydrazine (UDMH) transformation products (TPs) in solid samples is an important stage in monitoring of environmental pollution caused by heavy rockets launches. The new method for simultaneous quantification of UDMH TPs in sand samples using vacuum-assisted headspace solid-phase microextraction (Vac-HSSPME) followed by gas chromatography-mass spectrometry (GC-MS) is proposed. Compared to regular HSSPME, Vac-HSSPME yielded 1.3–4.8 times higher responses for NDMA, MTA and PAl. Increasing air-evacuation time from 20 to 120 s at 23 ºC resulted in decreased responses of analytes by 25–46%. Freezing of samples (-30 ºC) had negligible effect on responses of analytes at air-evacuation time 20 s. The best combination of responses of analytes and their RSDs was achieved after air-evacuation of a sample (m = 1.00 g) for 20 s at 23 ºC, incubation for 30 min and 30-min extraction at 40°C by Car/PDMS fiber. Vac-HSSPME provided linear calibration plots in studied ranges of concentrations with coefficients of determination ranging from 0.9912 to 0.9938. The limits of detection for spiked sand samples varied from 0.035 to 3.6 ng g− 1. Spike recoveries of target analytes from sand samples were 84–97% with RSDs 1–11%. The developed method was successfully tested in the experiment on studying losses of analytes from open vials with model sand spiked with UDMH TPs. The developed method can be recommended for analysis of trace concentrations of UDMH TPs when studying their transformation, migration and distribution in contaminated sand.