Separation and quantitation of nitrocellulose, nitroglycerin, diethylphthalate, and centralite in double‐base powder

Abstract

A method is described which makes possible a direct determination of nitrocellulose in double‐base powder and powder paste after separation from low‐molecular components by gel permeation chromatography and subsequent integration of the nitrocellulose peak. It is also possible to determine nitroglycerin and stabilizers in the same sample by collecting the components in the low‐molecular peak and subsequent injection into a reversed‐phase chromatography system. The procedure is exemplified on a powder paste containing nitrocellulose, nitroglycerin, centralite I, and diethylphthalate. The whole quantitation procedure will take less than an hour.

Detection and differentiation of nitrocellulose traces of forensic science interest with reductive mode electrochemical detection at a pendent mercury drop electrode coupled with size-exclusion chromatography

“…Chromatography Conditions. Usually tetrahydrofuran (15,16) or, on one occasion, ethyl acetate (17) has been used as eluent in the size-exclusion chromatography of nitrocellulose, but because of their poor ion-solvating characteristics they are of restricted value in electrochemical work. In this respect, acetonitrile is superior.…”

“…Apart from the addition of water or other highly polar compounds, silanization of the silica supresses the adsorption (13,18). Some publications have dealt with the chromatography of nitrocelluloses on the commercially available columns of such materials, with ultraviolet absorbance detection (17,19). An in situ silanized column was used in the present work, with unchanged eluent, when adsorption effects might have influenced the results significantly, as in the subsequently described examination of flow rate effects.…”

Differential Pulse Polarographic Analysis of Powders and Explosives

“…The differential pulse polarogram for 2,4,6-trinitrotoluene appears at somewhat more positive potential when ammonium acetate is used as electrolyte. It may be of interest to note that when tetramethyl ammoniumbromide is used as electrolyte two double peaks are obtained (the third peak is completely overlapped by a maximum) in polarography of 2,4,6-trinitrotoluene, which would indicate that reduction of nitrogroups is in stages from nitro via hydroxyl amine to amine [see reactions (9) and (lo)]. This means that the polarogram is somewhat more difficult to interprete in a quantitative analysis.…”