2015
DOI: 10.1039/c5ra17951c
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Low hazard small-scale synthesis and chemical analysis of high purity nitroglycerine (NG)

Abstract: A previously reported two-phase (99.5% fuming nitric acid/dichloromethane) batch method 1 to prepare high purity 1,2,3propanetriyl trinitrate (nitroglycerine, NG) was evaluated, simplified and adapted specifically for low hazard small-scale synthesis. The purity of the product, as determined by NMR spectroscopy, HPLC and IR spectroscopic analysis was found to be greater than 99%. The quick synthetic method is highly recommended when small amounts of highly pure NG are required for analytical and related purpos… Show more

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Cited by 6 publications
(3 citation statements)
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“…Synthesis of diethyleneglycol dinitrate was conducted following a previously reported method. 23 Nitric acid (99.5%, 4 ml) was added dropwise to sulphuric acid (98%, 4 ml) in a 50 ml 3 neck round bottom ask, ensuring that the temperature of the mixture remained below 15 C. Dichloromethane (30 ml) was then added to the mixed acid. The magnetically stirred mixture was then cooled to 5 C. Diethylene glycol (2.12 g) was slowly added (during 15 min) to the acid/dichloromethane mixture under vigorous stirring.…”
Section: Diethyleneglycoldinitrate Synthesismentioning
confidence: 99%
“…Synthesis of diethyleneglycol dinitrate was conducted following a previously reported method. 23 Nitric acid (99.5%, 4 ml) was added dropwise to sulphuric acid (98%, 4 ml) in a 50 ml 3 neck round bottom ask, ensuring that the temperature of the mixture remained below 15 C. Dichloromethane (30 ml) was then added to the mixed acid. The magnetically stirred mixture was then cooled to 5 C. Diethylene glycol (2.12 g) was slowly added (during 15 min) to the acid/dichloromethane mixture under vigorous stirring.…”
Section: Diethyleneglycoldinitrate Synthesismentioning
confidence: 99%
“…The composition of the nitroglycerin‐loaded polyester matrix was investigated qualitatively by comparing the individual infrared spectra of nitroglycerin and the polyester matrix with that of the NG/PM material (Figure 1). The two strong bands observed at 1265 cm −1 and 1633 cm −1 in the nitroglycerin spectrum correspond to −NO 2 symmetric and asymmetric stretches, respectively [12]. These bands, which are not found in the IR spectrum of the polyester matrix, are observed in the one of the NG/PM material, which confirms the presence of nitroglycerin in the elastomer matrix.…”
Section: Resultsmentioning
confidence: 61%
“…The absence of the characteristic broad and intense band attributed to the stretching of hydroxyl functional groups in FT-IR spectra (3200-3700 cm −1 ) of Mel/NG-SE and Mel/NG-SFE materials also shows that they do not contain the solvents (ethanol and ethanol/water, respectively) which were used to formulate them. The bands observed in the nitroglycerin spectrum at 1265 cm −1 and 1630 cm −1 , which respectively correspond to the symmetric (ν s ) and asymmetric stretching (ν as ) of -NO 2 groups [ 25 ], are found in Mel/NG-SE and Mel/NG-SFE materials. While there is no significant wavenumber shift of these bands for Mel/NG-SE, shifts of ∼8 cm −1 and ∼6 cm −1 to higher and lower wavenumbers are respectively observed for symmetric and asymmetric stretching of –NO 2 groups for Mel/NG-SFE.…”
Section: Resultsmentioning
confidence: 99%