A microstructured capillary electrophoresis method for nitrocellulose detection in dynamite
Autores
Calcerrada Guerreiro, Matías; Fernández de la Ossa, María de los Ángeles; Roy, Philippe; González Herráez, Miguel; García Ruiz, CarmenIdentificadores
Enlace permanente (URI): http://hdl.handle.net/10017/50060DOI: 10.1016/j.microc.2015.06.008
ISSN: 0026-265X
Fecha de publicación
2015-11Filiación
Universidad de Alcalá. Departamento de Electrónica; Universidad de Alcalá. Departamento de Química Analítica, Química Física e IngenieríaQuímicaPatrocinadores
Ministerio de Economía, Industria y Competitividad (MINECO)
Cita bibliográfica
Microchemical Journal, 2015, v. 123, p. 218-223
Palabras clave
Capillary electrophoresis
dynamite
forensic analysis
hydrodynamic study
microstructured capillary
optical fiber
Proyectos
info:eu-repo/grantAgreement/MINECO//TEC2012-37958-C02-01/ES/TECNOLOGIAS DE SEGURIDAD CIVIL BASADAS EN FIBRA OPTICA/
Tipo de documento
info:eu-repo/semantics/article
Versión
info:eu-repo/semantics/publishedVersion
Derechos
Attribution-NonCommercial-NoDerivatives 4.0 International (CC BY-NC-ND 4.0)
© Elsevier, 2015
Derechos de acceso
info:eu-repo/semantics/openAccess
Resumen
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.
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