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Thermal and spectroscopic analysis of nitrated compounds and their break-down products using gas chromatography/vacuum UV spectroscopy (GC/VUV)

NCJ Number
304064
Journal
Analytica Chimica Acta Volume: 1143 Dated: 2021 Pages: 117-123
Author(s)
C. A. Cruse; J. V. Goodpaster
Date Published
2021
Length
7 pages
Annotation

This project used gas chromatography/vacuum UV spectroscopy (GC/VUV) to study various explosives and pharmaceuticals in the nitrate ester and nitramine structural classes.

 

Abstract

In addition to generating specific VUV spectra for each compound, VUV was used to indicate the onset of thermal decomposition based upon the appearance of break-down products such as nitric oxide, carbon monoxide, formaldehyde, water, and molecular oxygen. The effect of temperature on decomposition could be fit to a logistical function where the fraction of intact compound remaining decreased as the transfer line/flow cell temperature was increased from 200 °C to 300 °C. Using this relationship, the decomposition temperatures for the nitrate ester and nitramine compounds were determined to range between 244 °C and 277 °C. It was also discovered that the decomposition temperature was dependent on the GC carrier gas flow rate and, therefore, the residence time of the compounds in the transfer line/flow cell; for example, the measured decomposition temperature of nitroglycerine ranged from 222 °C to 253 °C across four flow rates. Tracking the appearance/disappearance of decomposition products across this temperature range indicated that NO, CO, and H2CO are final decomposition products while O2 and H2O are intermediate products. The decomposition temperatures for all explosives were highly correlated to similar decomposition measurements taken by differential scanning calorimetry (DSC) (r = 0.91) and thermal gravimetric analysis (TGA) (r = 0.90–0.98). In addition, the decomposition temperatures for all explosives were negatively correlated to the heat of explosion at constant volume (r = −0.68) and strongly positively correlated to the oxygen balance (r = 0.92). (publisher abstract modified)