Precolumn derivatization with glyoxal as a new approach to the highly sensitive HPLC-UV determination of unsymmetrical dimethylhydrazine

Smirnov, R. S.; Smolenkov, A. D.; Bolotnik, T. A.; Шпигун, О. А.

doi:10.1134/s1061934813090116

Cited by 16 publications

(1 citation statement)

References 21 publications

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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%

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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Section: Introductionmentioning

confidence: 99%

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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1-Methyl-1H-1,2,4-triazole as the main marker of 1,1-dimethylhydrazine exposure in plants

Karnaeva

Milyushkin

Khesina

et al. 2022

Environ Sci Pollut Res

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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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Precolumn derivatization with glyoxal as a new approach to the highly sensitive HPLC-UV determination of unsymmetrical dimethylhydrazine

Cited by 16 publications

References 21 publications

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

1-Methyl-1H-1,2,4-triazole as the main marker of 1,1-dimethylhydrazine exposure in plants

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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Precolumn derivatization with glyoxal as a new approach to the highly sensitive HPLC-UV determination of unsymmetrical dimethylhydrazine

Cited by 16 publications

References 21 publications

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

1-Methyl-1H-1,2,4-triazole as the main marker of 1,1-dimethylhydrazine exposure in plants

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

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