Rapid determination of 1,1-dimethylhydrazine transformation products in soil by accelerated solvent extraction coupled with gas chromatography–tandem mass spectrometry

Kosyakov, D. S.; Ul’yanovskii, N. V.; Покрышкин, С. А.; Lakhmanov, Dmitry E.; Шпигун, О. А.

doi:10.1080/03067319.2015.1090569

Cited by 27 publications

(7 citation statements)

References 32 publications

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“…Common analytical methods used for the determination of UDMH TPs in soil are based on gas (Kenessov et al 2010b; Kosyakov et al 2015; Ul'yanovskii et al 2015; Bakaikina et al 2018) and liquid (Kosyakov et al 2014) chromatography coupled to various detectors. Conventional sample preparation methods for this type of determination are based on solvent extraction (Rodin et al 2010; Kosyakov et al 2014Kosyakov et al , 2015. Despite these methods provide high sensitivity and reliability, they are quite labor-intensive and costly.…”

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

Psillakis

et al. 2022

Environ Sci Pollut Res

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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.

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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

Psillakis

et al. 2022

Environ Sci Pollut Res

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“…The accuracy of the developed method was estimated by spike recovery test using real samples of river water and peat bog soil extract (Samples 1 and 2) at three concentration levels—20, 2, and 0.2 mg L −1 (n = 3, P = 0.95). The use of lower concentrations, close to LOQ, is not justified due to the high reactivity of many nitrogen-containing compounds and the occurrence of reactions of their binding with dissolved organic matter in natural waters, which leads to inadequate characteristics of the method accuracy [ 10 , 15 ]. The obtained results ( Supplementary, Tables S2–S4 ) clearly confirm the substantial effect of natural organic matter on the recoveries of analytes.…”

Section: Resultsmentioning

confidence: 99%

“…Gas chromatography is a more universal solution for separating the widest possible range of UDMH transformation products (with the exception of hydrazines and some thermolabile compounds). In combination with mass spectrometric detection, it has found application for the search, identification, and determination of dozens of UDMH transformation products in soils [5,[14][15][16][17][18][19].…”

Section: Introductionmentioning

confidence: 99%

Gas Chromatography–Mass Spectrometry Quantification of 1,1-Dimethylhydrazine Transformation Products in Aqueous Solutions: Accelerated Water Sample Preparation

2021

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The use of highly toxic rocket fuel based on 1,1-dimethylhydrazine (UDMH) in many types of carrier rockets poses a threat to environment and human health associated with an ingress of UDMH into wastewater and natural reservoirs and its transformation with the formation of numerous toxic nitrogen-containing products. Their GC-MS quantification in aqueous samples requires matrix change and is challenging due to high polarity of analytes. To overcome this problem, accelerated water sample preparation (AWASP) based on the complete removal of water with anhydrous sodium sulfate and transferring analytes into dichloromethane was used. Twenty-nine UDMH transformation products including both the acyclic and heterocyclic compounds of various classes were chosen as target analytes. AWASP ensured attaining near quantitative extraction of 23 compounds with sample preparation procedure duration of no more than 5 min. Combination of AWASP with gas chromatography–mass spectrometry and using pyridine-d5 as an internal standard allowed for developing the rapid, simple, and low-cost method for simultaneous quantification of UDMH transformation products with detection limits of 1–5 μg L–1 and linear concentration range covering 4 orders of magnitude. The method has been validated and successfully tested in the analysis of aqueous solutions of rocket fuel subjected to oxidation with atmospheric oxygen, as well as pyrolytic gasification in supercritical water modelling wastewater from carrier rockets launch sites.

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“…Common analytical methods used for the determination of UDMH TPs in soil are based on gas (Kenessov et al 2010b; Kosyakov et al 2015;Ul'yanovskii et al 2015;Bakaikina et al 2018) and liquid (Kosyakov et al 2014) chromatography coupled to various detectors. Conventional sample preparation methods for this type of determination are based on solvent extraction (Rodin et al 2010; Kosyakov et al 2014Kosyakov et al , 2015. Despite these methods provide high sensitivity and reliability, they are quite labor-intensive and costly.…”

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

Psillakis

et al. 2021

Preprint

View full text Add to dashboard 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.

show abstract

Rapid determination of 1,1-dimethylhydrazine transformation products in soil by accelerated solvent extraction coupled with gas chromatography–tandem mass spectrometry

Cited by 27 publications

References 32 publications

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

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

Gas Chromatography–Mass Spectrometry Quantification of 1,1-Dimethylhydrazine Transformation Products in Aqueous Solutions: Accelerated Water Sample Preparation

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

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