GC–MS and GC–NPD Determination of Formaldehyde Dimethylhydrazone in Water Using SPME

Kenessov, Bulat; Sailaukhanuly, Yerbolat; Kozieł, Jacek A.; Carlsen, Lars; Nauryzbayev, Mikhail

doi:10.1007/s10337-010-1820-6

Cited by 31 publications

(7 citation statements)

References 16 publications

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“…The determination of enantiomeric excess ( ee ) is an integral part of asymmetric catalysis. For the ATH of dihydroisoquinolines (DHIQs), the ee of chiral products (tetrahydroisoquinolines, THIQs) is typically determined by using GC-MS [7,8] or liquid chromatography with UV-Vis [9,10], fluorescent [11] or MS [12,13] detection. The instruments are usually equipped with columns with a chiral stationary phase that allows direct separation of enantiomers.…”

Section: Analytical Methods Tailored For Athmentioning

confidence: 99%

Practical Aspects and Mechanism of Asymmetric Hydrogenation with Chiral Half-Sandwich Complexes

et al. 2013

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This review is oriented toward the asymmetric transfer hydrogenation (ATH) of imines regarding mostly fundamental, yet important topics from the practical point of view. Development of analytical methods for the monitoring of ATH (i.e., kinetics and stereoselectivity) belongs to those topics, as well as studies on the influence of reaction conditions and structural variations on the reaction performance. The second part is devoted to the reaction mechanism with the emphasis on imine ATH and catalyst behaviour under acidic conditions. The review also addresses the asymmetric hydrogenation (AH) of ketones and imines using molecular hydrogen and the application of ATH in pharmaceutical projects. The contributions of our group to each area are included.

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Section: Analytical Methods Tailored For Athmentioning

confidence: 99%

Practical Aspects and Mechanism of Asymmetric Hydrogenation with Chiral Half-Sandwich Complexes

et al. 2013

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“…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: 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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“…For the greatest accuracy at lower concentrations, portable GC‐MS can be used. A portable GC‐NPD instrument can be an alternative option due to its comparable LODs to GC‐MS [52].…”

Section: Resultsmentioning

confidence: 99%

Quantification of transformation products of rocket fuel unsymmetrical dimethylhydrazine in air using solid‐phase microextraction

Bukenov

Baimatova

Kenessov

2021

J of Separation Science

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Quantification of unsymmetrical dimethylhydrazine transformation products in ambient air is important for assessing the environmental impact of heavy rocket launches. There are very little data of such analyses, which is mainly caused by the low number of analytes covered by the available analytical methods and their complexity. A simple and cost‐efficient method for accurate simultaneous determination of seven unsymmetrical dimethylhydrazine transformation products in air using solid‐phase microextraction followed by gas chromatography‐mass spectrometry was developed. The method was optimized for air sampling and solid‐phase microextraction from 20‐mL vials, which allows full automation of analysis. The extraction for 5 min by Carboxen/polydimethylsiloxane fiber from amber vials and desorption for 3 min provided the greatest analytes' responses, lowest relative standard deviations, linear calibration (R2 ≥ 0.99), and limits of detection from 0.12 to 0.5 μg/m3. Samples with concentrations 500 μg/m3 can be stored at 21 ± 1°C without substantial losses (1–11%) for up to 24 h, while air samples with concentrations 10 and 50 μg/m3 stored for up to 24 h can be used for accurate quantification of only two and four out of seven analytes, respectively. The developed method was successfully tested for the analysis of air above real soil samples contaminated with unsymmetrical dimethylhydrazine rocket fuel.

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GC–MS and GC–NPD Determination of Formaldehyde Dimethylhydrazone in Water Using SPME

Cited by 31 publications

References 16 publications

Practical Aspects and Mechanism of Asymmetric Hydrogenation with Chiral Half-Sandwich Complexes

Practical Aspects and Mechanism of Asymmetric Hydrogenation with Chiral Half-Sandwich Complexes

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

Quantification of transformation products of rocket fuel unsymmetrical dimethylhydrazine in air using solid‐phase microextraction

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