A microstructured capillary electrophoresis method for nitrocellulose detection in dynamite

In this article we present a microstructured-capillary electrophoresis method for the determination of minimal amounts of nitrocellulose in dynamite samples. A 6-hole microstructured capillary (MSC) was selected for the method development. First, the hydrodynamic behaviour of the MSC was studied at...

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Detalles Bibliográficos
Autores: Calcerrada Guerreiro, Matías, Fernández de la Ossa, María de los Ángeles, Roy, Philippe, González Herráez, Miguel|||0000-0003-2555-2971, García Ruiz, Carmen|||0000-0001-5925-3449
Tipo de recurso: artículo
Fecha de publicación:2015
País:España
Institución:Universidad de Alcalá (UAH)
Repositorio:e_Buah Biblioteca Digital Universidad de Alcalá
Idioma:inglés
OAI Identifier:oai:ebuah.uah.es:10017/50060
Acceso en línea:http://hdl.handle.net/10017/50060
https://dx.doi.org/10.1016/j.microc.2015.06.008
Access Level:acceso abierto
Palabra clave:Capillary electrophoresis
dynamite
forensic analysis
hydrodynamic study
microstructured capillary
optical fiber
Chemistry
Química
Descripción
Sumario:In this article we present a microstructured-capillary electrophoresis method for the determination of minimal amounts of nitrocellulose in dynamite samples. A 6-hole microstructured capillary (MSC) was selected for the method development. First, the hydrodynamic behaviour of the MSC was studied at varying lengths (31, 41 and 51 cm), which had never been studied before. Next, one of the MSC segments (31 cm) was employed to develop a microstructured-capillary electrophoresis method to determine nitrocellulose in dynamite. In a first evaluation, the dynamite derivatization process was investigated to obtain an efficient derivatization yield. Afterwards, the instrumental parameters, more specifically voltage and capillary cartridge temperature, were optimized. Afterwards, the analytical performance of the developed methodology was assessed. Dynamite analyses during a period of 15 days were performed to establish intra-day (10 analyses) and inter-day (40 analyses) precision, obtaining RSDs lower than 6 and 10%, respectively. Besides, RSDs for migration time (<0.5%), peak asymmetry (<3%), resolution (<3.9%) and S/N (<9%) were obtained. Finally, a diluted sample of dynamite was analysed, detecting amounts of nitrocellulose in the order of 220-400 pg.