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An Application of Thin Layer Chromatography Combined with Optical Densitometry to Quantitative Analysis of Diphenylamine and Its Initial Daughter Reaction Products in Single-Base Propellants Aged under Natural Conditions

Miszczak M.

Central European Journal of Energetic Materials

2011

Vol. 8, nr 2

107-116

Thin Layer Chromatography (TLC) was used for the quantitative measurement of the composition of stabilizers used to retard chemical decomposition of single-base (SB) propellants i.e. diphenylamine (DPA), and its initial reaction products due to natural ageing of these propellants under natural (ambient) conditions with test results and certain observations in this matter, are presented. The quantitative determination of DPA and its reaction products was possible by a combination of TLC with the densitometric spectrophotometry technique in the UV detection region. The crucial stage of TLC analytical quantitations was complete extraction of the substances to be analysed from SB propellants nitrocellulose (NC), which was done by rapid dissolution of the SB propellant samples followed by dilution of the solutions obtained to such degree as to make possible TLC separation of the substances to be analysed from the NC "matrix" in which they are "trapped" when the solution is too viscous. Initial chemical changes of DPA in SB propellants resulting in the appearance of DPA initial daughter reaction products such as N-nitroso-DPA, 2-nitro-DPA and 4-nitro-DPA, gave important information on the natural ageing of these homogeneous propellants starting from their very short storage period (some days, weeks or months just after their manufacture) up to long storage lasting even 50 years.