A new method for the determination of the nitrogen content of nitrocellulose based on the molar ratio of nitrite-to-nitrate ions released after alkaline hydrolysis

JOURNAL OF HAZARDOUS MATERIALS

卷:286

Article

Alinat, Elodie^1,2,3,5  Delaunay, Nathalie^1,3,5  Archer, Xavier²  Mallet, Jean-Maurice^4,5,6  Gareil, Pierre^1,3,5 

[1] PSL Res Univ, Chim ParisTech, Lab Physicochem Elect Colloids & Analyt Sci PECSA, F-75005 Paris, France

[2] Cent Lab Police Prefecture LCPP, F-75015 Paris, France

[3] CNRS, PECSA, UMR 7195, F-75005 Paris, France

[4] PSL Res Univ, Ecole Normale Super, Dept Chim, F-75005 Paris, France

[5] Univ Paris 06, Sorbonne Univ, LBM, F-75005 Paris, France

[6] CNRS, LBM, UMR 7203, F-75005 Paris, France

关键词: Nitrocellulose;    Nitrogen content;    Alkaline hydrolysis;    Smokeless gunpowder;   

DOI  :  10.1016/j.jhazmat.2014.12.032

来源: Elsevier

【 摘 要 】

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 (1 h 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 1 M sodium hydroxide for 1 h at 60 degrees C). 2014 Elsevier B.V. All rights reserved.

【 授权许可】

Free