“…Not only the variety of chemical compositions, physicochemical, thermal, and mechanical changes, but also the mechanisms of degradation are some of the issues that make the investigation of the aging process a very complex topic. Although many researh groups have investigated the aging process of NC‐based formulations, some behaviors as well as the appearance of new formulations are still open for the development of new methodologies. Broadly, the change in properties of a NC‐based formulations subjected to natural aging takes a very long time, and in order to obtain advanced information concerning the aging characteristics in a relatively reasonable time, accelerated aging at elevated temperatures is usually performed .…”
In this work, Fourier transform infrared spectroscopy (FTIR) and X-ray powder diffraction (XRD) were selected as reliable, fast, and nondestructive techniques to assess their potentialities for characterization and discrimination of nitrocellulose (NC)-based formulations containing different kinds of stabilizers and subjected to accelerated aging. Preliminary results based on visual comparison of the spectra point out that spectra obtained by both spectroscopic techniques were useful for a rapid detection of the aging process without additional sample preparation. Additionally, the existence of compatibility issues between NC and one of the stabilizers is easily recognized. The spectral data were subjected to principal component analysis (PCA) for visualization and to reveal differences between samples. The obtained results demonstrated that PCA plots were able to distinguish and classify the NC samples with respect to their respective stabilizers and aging.
“…Not only the variety of chemical compositions, physicochemical, thermal, and mechanical changes, but also the mechanisms of degradation are some of the issues that make the investigation of the aging process a very complex topic. Although many researh groups have investigated the aging process of NC‐based formulations, some behaviors as well as the appearance of new formulations are still open for the development of new methodologies. Broadly, the change in properties of a NC‐based formulations subjected to natural aging takes a very long time, and in order to obtain advanced information concerning the aging characteristics in a relatively reasonable time, accelerated aging at elevated temperatures is usually performed .…”
In this work, Fourier transform infrared spectroscopy (FTIR) and X-ray powder diffraction (XRD) were selected as reliable, fast, and nondestructive techniques to assess their potentialities for characterization and discrimination of nitrocellulose (NC)-based formulations containing different kinds of stabilizers and subjected to accelerated aging. Preliminary results based on visual comparison of the spectra point out that spectra obtained by both spectroscopic techniques were useful for a rapid detection of the aging process without additional sample preparation. Additionally, the existence of compatibility issues between NC and one of the stabilizers is easily recognized. The spectral data were subjected to principal component analysis (PCA) for visualization and to reveal differences between samples. The obtained results demonstrated that PCA plots were able to distinguish and classify the NC samples with respect to their respective stabilizers and aging.
“…NC-based smokeless gunpowders are classified according to the number of energetic materials in their composition [3,4]: i) single-base propellants, which mainly contain NC, ii) double-base propellants consisting of NC and nitroglycerin, and iii) triple-base propellants containing NC, nitroglycerin, and nitroguanidine. Most smokeless gunpowders are formulated with graphite and various other chemicals (such as dinitrotoluene) to monitor burning, reduce muzzle flash, and make them more water resistant.…”
A new method was proposed to determine the nitrogen content of nitrocelluloses (NCs). It is based on the finding of a linear relationship between the nitrogen content and the molar ratio of nitrite-to-nitrate ions released after alkaline hydrolysis. Capillary electrophoresis was used to monitor the concentration of nitrite and nitrate ions. The influences of hydrolysis time and molar mass of NC on the molar ratio of nitrite-to-nitrate ions were investigated, and new insights into the understanding of the alkaline denitration mechanism of NCs, underlying this analytical strategy is provided. The method was then tested successfully with various explosive and non-explosive NC-containing samples such as various daily products and smokeless gunpowders. Inherently to its principle exploiting a concentration ratio, this method shows very good repeatability in the determination of nitrogen content in real samples with relative standard deviation (n = 3) inferior to 1.5%, and also provides very significant advantages with respect to sample extraction, analysis time (1h for alkaline hydrolysis, 3 min for electrophoretic separation), which was about 5 times shorter than for the classical Devarda's method, currently used in industry, and safety conditions (no need for preliminary drying NC samples, mild hydrolysis conditions with 1M sodium hydroxide for 1h at 60 °C).
“…Several analytical techniques have been used for the qualitative and/or quantitative detection of smokeless powders, either in their pre-and/or post-blast forms [9,10], including highperformance liquid chromatography (HPLC) [17][18][19], liquid chromatography-mass spectrometry (LC-MS) [8,[20][21][22], Fourier transform infrared spectroscopy [23], gas chromatography (GC) [12,14,24], capillary electrophoresis (CE) [25,26], ion m o b i l i t y s p e c t r o m e t r y ( I M S ) [ 2 7 ] , s o l i d -p h a s e microextraction-ion mobility spectrometry (SPME)-IMS [12,28], (nano)electrospray ionization (nESI)-tandem mass spectrometry [29][30][31], laser electrospray-mass spectrometry (LEMS) [15,32], desorption electrospray ionization-mass spectrometry (DESI) [33,34], direct analysis in real timemass spectrometry (DART-MS) [35], time-of-flight secondary ion-mass spectrometry (ToF-MS) [36] and Raman spectroscopy [23,37]. Most of the abovementioned techniques require time-consuming sample preparation step(s)-exception of DESI and DART-or if not, they require complicated setups, such as the use of lasers as the means for sample vaporization (LEMS) or heated purified gases (DART).…”
Analysis of smokeless powders is of interest from forensics and security perspectives. This article reports the detection of smokeless powder organic additives (in their pre-detonation condition), namely the stabiliser diphenylamine and its derivatives 2-nitrodiphenylamine and 4nitrodiphenylamine, and the additives (used both as stabilisers and plasticisers) methyl centralite and ethyl centralite, by means of swab sampling followed by thermal desorption and direct injection soft chemical ionisation-mass spectrometry. Investigations on the product ions resulting from the reactions of the reagent ions H 3 O + and O 2 + with additives as a function of reduced electric field are reported. The method was comprehensively evaluated in terms of linearity, sensitivity and precision. For H 3 O + , the limits of detection (LoD) are in the range of 41-88 pg of additive, for which the accuracy varied between 1.5 and 3.2%, precision varied between 3.7 and 7.3% and linearity showed R 2 ≥ 0.9991. For O 2 + , LoD are in the range of 72 to 1.4 ng, with an accuracy of between 2.8 and 4.9% and a precision between 4.5 and 8.6% and R 2 ≥ 0.9914. The validated methodology was applied to the analysis of commercial pre-blast gun powders from different manufacturers.Research Highlights • Use of direct injection soft chemical ionisation-mass spectrometry for smokeless powder organic additive analysis
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