Gas-chromatographic determination of 1,1-dimethylhydrazine in water

Sotnikov, E. E.; Moskovkin, A. S.

doi:10.1134/s1061934806020079

Cited by 16 publications

(5 citation statements)

References 3 publications

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“…Analytical methods should consider and minimize chemical transformations especially during sample preparation. Research during the last 15 years was mainly focused on the methods for determination of UDMH [13,14,15,16,17,18,19]. However, to date, there are no robust methods for determination of its transformation products.…”

Section: Current Analytical Methods For Analysis Of Udmh Transformatimentioning

confidence: 99%

“…The use of SPME for sampling and sample preparation resulted in detection of the total of 55 new compounds, i.e., 12 new transformation products of UDMH (compounds No. 6,7,10,12,14,16,17,18,19,23,25,26,27); 9 compounds with lower MS match (and therefore lower degree of confidence in proper identification) and 34 compounds which can potentially be transformation products of UDMH (Table 2). This represents 80% increase of confirmed compounds known to be products of UDMH transformation in soil.…”

Section: Tablementioning

confidence: 99%

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Screening of transformation products in soils contaminated with unsymmetrical dimethylhydrazine using headspace SPME and GC–MS

Kenessov

Kozieł

Grotenhuis

et al. 2010

Analytica Chimica Acta

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The paper describes a novel SPME-based approach for sampling and analysis of transformation products of highly reactive and toxic unsymmetrical dimethylhydrazine (UDMH) which is used as a fuel in many Russian, European, Indian, and Chinese heavy cargo carrier rockets. The effects of several parameters were studied to optimize analyte recovery. It was found that the 85 microm Carboxen/polydimethylsiloxane fiber coating provides the highest selectivity for selected UDMH transformation products. Optimal sampling/sample preparation parameters were determined to be 1-h soil headspace sampling time at 40 degrees C. The GC inlet temperature was optimized to 170 degrees C held for 0.1 min, then 1 degrees C s(-1) ramp to 250 degrees C where it was held for 40 min. Temperature programming resulted in a fast desorption along with minimal chemical transformation in the GC inlet. SPME was very effective extracting UDMH transformation products from soil samples contaminated with rocket fuel. The use of SPME resulted in high sensitivity, speed, small labor consumption due to an automation and simplicity of use. It was shown that water addition to soil leads to a significant decrease of recovery of almost all target transformation products of UDMH. The use of SPME for sampling and sample preparation resulted in detection of the total of 21 new compounds that are relevant to the UDMH transformation in soils. In addition, the number of confirmed transformation products of UDMH increased from 15 to 27. This sampling/sample preparation approach can be recommended for environmental assessment of soil samples from areas affected by space rocket activity.

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Section: Current Analytical Methods For Analysis Of Udmh Transformatimentioning

confidence: 99%

Section: Tablementioning

confidence: 99%

Screening of transformation products in soils contaminated with unsymmetrical dimethylhydrazine using headspace SPME and GC–MS

Kenessov

Kozieł

Grotenhuis

et al. 2010

Analytica Chimica Acta

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“…As they are explosive, toxic and carcinogenic in nature, many methods for detection (followed by determination) of these hydrazines have been proposed by many researchers to protect the personnel working in such a hazardous chemical environment. These include spectrophotometry, 7-10 uorescence, [11][12][13][14][15][16][17][18] gas chromatography [19][20][21][22][23][24][25][26][27][28] and liquid chromatography [29][30][31] methods.…”

Section: Introductionmentioning

confidence: 99%

“…Several derivatization-based GC methods for the determination of hydrazines have been reported in the past. They are mainly based on derivative formation from 2,4-pentanedione, 19 1,1,1-triuoroacetylacetone, 20 pentauoro benzaldehyde, 21,22 p-nitrobenzaldehyde, 23,24 ethylchloro formate, 25 acetone, 26 and o-phthalaldehyde 27 (Table 1). These methods are selective either to hydrazine or MMH or UDMH only.…”

Section: Introductionmentioning

confidence: 99%

“…In addition to this, some of these methods are more time consuming 21,23,24,33 with poor recovery records obtained from non-universal detectors such as the Electron Capture Detector 22 (ECD) and Nitrogen Phosphorous Detector 21,23 (NPD). There is a need for catalysts for such types of reactions with pre-concentration step requirement 25 and high temperature application 20,27 or extraction of derivatives with low boiling solvents is involved.…”

Section: Introductionmentioning

confidence: 99%

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Single step derivatization with CF₃ enone of thiophene at ambient temperature to determine propellant grade hydrazines: a study by GC and GC-MS

Selvasekarapandian

Somanathan

Reddy

2015

Analyst

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A simple, highly selective and rapid gas chromatography method (packed column with flame ionization detection) has been developed to determine hydrazine and monomethylhydrazine individually and for selective determination of hydrazine in the UH 25 mixture in organic medium. This method is based on the derivatization of hydrazine (at ambient temperature) with 1,1,1-trifluoro-4-(3-thienyl) (CF3 enone) in the absence of catalyst/buffer which leads to the formation of corresponding pyrazolidine/pyrazoline/pyrazole. The organic derivatives thus formed are then detected and their presence is confirmed by GC-MS. The GC method provides good resolution between CF3 enone and its derivatives with a total analysis time of 20 min. The concentration of CF3 enone and derivatization time are optimized to determine hydrazines in the concentration range of 0.4 mM to 0.2 M. The calibration curves based on peak areas of CF3 enone and its derivatives showed good linearity with r(2) ≈ 0.999 for the working range and the precision was found to be less than 1% for hydrazine, MMH and hydrazine in UH25. The recovery was found by the standard addition method. Under the established conditions, limits of detection were 20 μM for hydrazine, 10 μM for MMH and 20 μM for hydrazine in UH25. The tolerance limit for interfering amines was also found. The advantage of this method is the selective detection and determination of hydrazine in the UH25 mixture as 1,1-dimethylhydrazine present in UH25 cannot be derivatized with CF3 enone.

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A novel simple and sensitive approach for determination of 1,1-dimethylhydrazine in aqueous samples by high performance liquid chromatography with ultraviolet and tandem mass spectrometric detection after derivatization with unsubstituted aromatic aldehydes

et al. 2021

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Gas-chromatographic determination of 1,1-dimethylhydrazine in water

Cited by 16 publications

References 3 publications

Screening of transformation products in soils contaminated with unsymmetrical dimethylhydrazine using headspace SPME and GC–MS

Screening of transformation products in soils contaminated with unsymmetrical dimethylhydrazine using headspace SPME and GC–MS

Single step derivatization with CF₃ enone of thiophene at ambient temperature to determine propellant grade hydrazines: a study by GC and GC-MS

A novel simple and sensitive approach for determination of 1,1-dimethylhydrazine in aqueous samples by high performance liquid chromatography with ultraviolet and tandem mass spectrometric detection after derivatization with unsubstituted aromatic aldehydes

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Gas-chromatographic determination of 1,1-dimethylhydrazine in water

Cited by 16 publications

References 3 publications

Screening of transformation products in soils contaminated with unsymmetrical dimethylhydrazine using headspace SPME and GC–MS

Screening of transformation products in soils contaminated with unsymmetrical dimethylhydrazine using headspace SPME and GC–MS

Single step derivatization with CF3 enone of thiophene at ambient temperature to determine propellant grade hydrazines: a study by GC and GC-MS

A novel simple and sensitive approach for determination of 1,1-dimethylhydrazine in aqueous samples by high performance liquid chromatography with ultraviolet and tandem mass spectrometric detection after derivatization with unsubstituted aromatic aldehydes

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Single step derivatization with CF₃ enone of thiophene at ambient temperature to determine propellant grade hydrazines: a study by GC and GC-MS