Determination of transformation products of 1,1-dimethylhydrazine by gas chromatography–tandem mass spectrometry

Ul’yanovskii, N. V.; Kosyakov, D. S.; Покрышкин, С. А.; Боголицын, К. Г.

doi:10.1134/s1061934815130080

Cited by 25 publications

(5 citation statements)

References 19 publications

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“…Due to not using the sample preconcentration during AWASP, the sensitivity of the method is inferior to the approaches based on the use of SPME; however, it provides the detection of even the most toxic of the studied compounds, NDMA, at the level of 0.5 MPC (the established level in Russia and Kazakhstan MPC in natural water is 10 µg L −1 ). Despite the much simpler extraction procedure, the LODs achieved are close to the values reported earlier by Ul'yanovskii et al [14] and obtained using liquid-liquid extraction with acetonitrile from aqueous samples saturated with sodium chloride as salting-out agent.…”

Section: Analytical Methods and Its Validationsupporting

confidence: 87%

“…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%

“…The use of GC-MS for the analysis of aqueous samples is limited by the need to change the matrix, since the introduction of even small amounts of water into the chromatographic column leads to distortion of the shape of the chromatographic peaks, loss of separation efficiency, and instability of the analyte retention times. To solve this problem, liquid-liquid extraction (LLE) from a saturated saline solution [14,16,19], as well as solid-phase microextraction (SPME) from the vapor phase [20,21] were used. Despite the possibility of significant preconcentration of analytes, these methods also have a number of disadvantages.…”

Section: Introductionmentioning

confidence: 99%

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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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Section: Analytical Methods and Its Validationsupporting

confidence: 87%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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

2021

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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.…”

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

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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.

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“…However, the experiment shows that the radical traps increase the NDMA formation [11]. Furthermore, various analytical techniques such as high performance liquid chromatography-mass spectroscopy (HPLC-MS) [16][17][18], gas chromatography-mass spectroscopy (GC-MS) [3,19,20], and solid phase micro-extraction (SPME-GC/MS) [21] have been used for the identification and quantitative determination of these transformation products, and more than 30 oxidative products have been identified. However, the information about the products of the hydrazines reaction with ozone is scarce, and the HO• influence on NDMA formation mechanism is still in discussion.…”

Section: Introductionmentioning

confidence: 99%

Products and Mechanistic Investigations on the Reactions of Hydrazines with Ozone in Gas-Phase

et al. 2018

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The toxic transformation products of hydrazines are of great concern. These products’ properties combined with their formation mechanisms are needed to assess their potential environmental and human impacts. In this study, the gas-phase reaction of hydrazine (N2H4), monomethyldrazine (MMH) and unsymmetrical dimethyhydrazine (UDMH) with O3 have been studied at varying reactant ratios, both in the presence and absence of a radical trap. Gas chromatography-mass spectroscopy (GC-MS) has been implied to follow reactant consumption and product formation. Apart from the reported products detected by Fourier transform infrared spectroscopy (FT-IR), the newly found compounds (hydrazones, formamides, dimethylamine, 1,1,4,4-tetramethyl-1,2-tetrazene,dimethylamino-acetonitrile, N2, H2O, et al.) are identified by GC-MS. The relative yields of the organic products vary considerably at different O3/MMH or UDMH ratios. UDMH and MMH are confirmed as high potential precursors of N-nitrosodimethylamine (NDMA). The presence of hydroxyl radicals (HO·) hinders NDMA formation in MMH-O3 system. Meanwhile, it increases NDMA formation in UDMH-O3 system. The suggested reaction mechanisms which account for the observed products are discussed.

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Determination of transformation products of 1,1-dimethylhydrazine by gas chromatography–tandem mass spectrometry

Cited by 25 publications

References 19 publications

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

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

Products and Mechanistic Investigations on the Reactions of Hydrazines with Ozone in Gas-Phase

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