Homemade Explosives Based in Ammonium and Urea Nitrates

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Homemade Explosives Based in Ammonium and Urea Nitrates Joana Quaresma Joana Filipa Pires d’Oliveira Quaresma Homemade Explosives based in Ammonium and Urea Nitrates Forensic Chemistry Master Degree Chemistry Department FCTUC September, 2013 Homemade Explosives based in Ammonium and Urea Nitrates and Urea in Ammonium based Explosives Homemade September 2013 (primeira folha no interior da tese, em branco nas costas) Joana Filipa Pires d’Oliveira Quaresma HOMEMADE EXPLOSIVES BASED IN AMMONIUM AND UREA NITRATES Dissertação apresentada para provas de Mestrado em Química, Área de especialização em Química Forense Professor Doutor José Leandro Simões de Andrade Campos Professora Doutora Marta Piñeiro Gomez Setembro de 2013 Universidade de Coimbra HOMEMADE EXPLOSIVES BASED ON AMMONIUM AND UREA NITRATES Quando se luta nem sempre se ganha. Quando não se luta perde-se sempre. Álvaro Cunhal i Joana Quaresma ii Joana Quaresma HOMEMADE EXPLOSIVES BASED ON AMMONIUM AND UREA NITRATES ACKNOWLEDGMENTS Este projecto científico é o culminar da grande Luta Académica que foi para mim a passagem pela Universidade de Coimbra. Apesar de todos os contratempos, não lutar nunca foi uma hipótese. Por isso, nunca perdi. Muitas vezes me faltaram as forças, sobretudo no Departamento de Física - o terreno das mais duras batalhas e de onde saí victoriosamente licenciada. Algo que sempre me ensinaram (e que bem aprendi) é que só podemos lutar se tivermos objectivos e, sem luta, a vida perde o seu encanto. Esta Luta Académica não é só a mim que se deve. Muitos intervenientes tiveram um papel fundamental para que nunca me esquecesse dos objectivos que moviam a minha Luta Académica. A todos estou eternamente grata. Aos meus pais agradeço por cedo me terem ensinado o significado da palavra “luta”, por nunca terem desistido de mim, por sempre terem acreditado nos meus potenciais. À minha mãe, por sempre ter sido e ainda ser um modelo a seguir e que muito admiro. Ao meu pai, por todo o esforço económico e apoio ao longo destes anos, que muito reconheço e agradeço. Ao meu irmão João, que sempre me apoiou e que teve um papel fundamental no meu crescimento. À Teresa, que é como uma mãe para mim e a primordial incentivadora do meu percurso escolar. Talvez também graças à tabuada feita por ela (à mão) ter nascido o meu gosto pelas ciências. Aos meus orientadores, um muito obrigada por toda a atenção prestada e conhecimento partilhado. À Professora Doutora Marta Piñeiro, por ter sido a primeira Professora a acreditar em mim e nas minhas capacidades, por toda a boa disposição e empenho ao longo dos últimos três anos. Ao Professor Doutor José Campos por, além de acreditar e confiar nas minhas capacidades, as testar todos os dias e investir nelas, por toda a sabedoria partilhada, dedicação empenhada e por todos os dias me fazer ver o mundo um pouco mais além. Sem dúvida que são pessoas que deixarão para sempre a sua marca na minha vida, mesmo que ausentes um dia. iii Joana Quaresma ACKNOWLEDGMENTS Aos meus colegas de laboratório, Jaqueline e João, agradeço sobretudo o companheirismo. À Jaqueline agradeço pelo empenho, compreensão e pelas boleias que tanto me facilitaram a vida durante esta luta final. Ao João, um muito obrigada pelo bom humor constante, positivismo, acessibilidade e amizade que se gerou num tão curto espaço de tempo. Aos meus amigos, Carolina e Leandro, estou agradecida pelo apoio dado em casa, sobretudo nas horas de maior agonia por que passei, que se traduziram num mau feito insuportável que eles estoicamente suportaram. A todos os meus amigos, com especial relevo para o Paulo, a Inês, a Mariana e a Sara, um muito obrigada por fazerem parte da minha vida e por sempre me terem apoiado ao longo dela, mesmo quando as escolhas não eram as melhores. Ao Laboratório de Energética e Detónica, ao Departamento de Engenharia Mecânica e ao Departamento de Química, obrigada pelo fornecimento de infraestruturas e material, essenciais em toda esta Luta. iv Joana Quaresma HOMEMADE EXPLOSIVES BASED ON AMMONIUM AND UREA NITRATES RESUMO Nitrato de Amónio (NH4NO3) é a componente base de uma conhecida família de misturas geradoras de gases e compósitos pirotécnicos. Nitrato de Ureia ((NH2)2COHNO3) é um nitrato recentemente utilizado em estudos de deflagração e detonação. Ambos os nitratos foram utilizados em grandes atentados terroristas e são frequentemente utilizados em explosivos ocasionais. Foram testadas misturas de nitrato de amónio (AN) e de nitrato de ureia (UN). Foram utilizados poliuretano como ligante e, como aditivos, pó de Al e uma mistura de Magnésio com Teflon (MT). A decomposição dos reagentes foi prevista em função da temperatura através do código THOR. As temperaturas de combustão também foram teoricamente previstas, de modo a optimizar composições e a avaliar as performances esperadas. Os termogramas dos reagentes, adquiridos por DSC/TGA, ajudaram a definir as composições testadas, pois demonstram os seus níveis de decomposição. Os termogramas adquiridos do AN e do UN mostram algumas diferenças significativas entre eles. O UN apresenta um pico exotérmico a baixas temperaturas. Os testes experimentais recorreram a duas configurações: amostras cilíndricas, cuja ignição era feita no topo, e contentores em forma de disco, compostos por uma base cilíndrica de PVC e uma tampa de PMMA. As amostras cilíndricas foram testadas antes dos discos para verificar propriedades de combustão. O sistema de termopares permitiu a medição de temperaturas de combustão. Filmagens, acima de 1000 fps, permitiram a visualização directa da propagação da chama. Assim, as velocidades fundamentais de chama puderam ser medidas. A combustão com aditivos, Al e MT, demonstram aumentos de temperatura de chama na ordem dos 1300ºC e apresentam, sempre para a pressão atmosférica, velocidades de propagação de chama de mm/s e velocidades fundamentais de chama superiores a cm/s. A mistura de MT, como aditivo, parece aumentar a expansão dos produtos de combustão, mais do que o Al. O UN tem um comportamento semelhante ao do AN neste tipo de composições energéticas. Foi observada a auto-ignição de uma mistura de UN/PU com MT durante o tempo de cura. Este facto parece ser devido a complexos fenómenos (reacções entre os reagentes), onde foi observada a produção de gás proveniente do UN. Estudos suplementares são necessários antes de realizar novas experiências. v Joana Quaresma RESUMO A espectroscopia de infra-vermelho (IV) foi utilizada para caracterizar os reagentes utilizados nas misturas, bem como a sua presença nas respectivas misturas, e para avaliar a formação de novas ligações, devido a reacções entre os reagentes. Os espectros de IV confirmam as capacidades de detecção para este tipo de misturas e provam a existência dos reagentes “frescos” nos resíduos de combustão. Palavras-chave: Nitrato de Amónio, Nitrato de Ureia, ligante Poliuretano, explosivos ocasionais, aditivo alumínio, aditivo Magnésio/Teflon, código THOR, termogramas DSC/TGA, testes de combustão de amostras, velocidades fundamental de propagação de chama, espectroscopia de infra-vermelho. vi Joana Quaresma HOMEMADE EXPLOSIVES BASED ON AMMONIUM AND UREA NITRATES ABSTRACT Ammonium Nitrate (NH4NO3) is the base component of a known family of gas generators and pyrotechnic composite mixtures. Urea Nitrate ((NH2)2COHNO3) is a recent used nitrate in deflagration and detonation studies. Both of these nitrates were used in huge terrorist attacks and are frequently used on Homemade Explosives (HME). Mixtures of Ammonium Nitrate (AN) and Urea Nitrate (UN) with polyurethane solution, as binder, were tested, having Al and a mixture of Magnesium/Teflon as additives. Decomposition of reactants, as a function of temperature, was predicted using THOR code. Combustion temperatures were also theoretically predicted in order to optimize compositions and evaluate expected performances. DSC/TGA thermograms of reactants help to define tested compositions, showing their decomposition levels. AN and UN thermograms show some significant differences between them. UN presents an exothermic peak at quite low temperature. Experimental tests use two configurations: cylindrical samples, ignited at the top, and a cylindrical disk box, formed by a PVC cylindrical cup covered by a PMMA lid. Cylindrical samples were tested before cylindrical disk boxes, verifying burning properties. A thermocouples system allowed to measure burning temperatures. Video records, up to 1000 fps, allowed the direct visualization of the flame propagation. Fundamental flame velocities can then be measured. Combustion with additives, Al and MT, show an increasing flame temperature on the levels of 1300 ºC and present, always for atmospheric pressure, flame propagation velocities of mm/s and fundamental flame velocities higher than cm/s. MT additive seems to present an increased contribution, to the expansion of combustion products, more than Al. UN has a quite similar behaviour of AN in this kind of energetic compositions. It was observed the self-ignition of one of UN/PU compositions with MT, during curing time. It seems to be due to complex phenomena (reactions between reactants) where the production of gas, from UN, was observed. Supplementary studies are required before new experiences. Infra-Red (IR) spectroscopy was used to characterize the reactants used on the mixtures and their presence on respective mixtures, to evaluate the formation of new bounds due to the reactions between reactants. IR spectra confirm detection capabilities for these kind of mixtures and prove the existing unburnt reactants at found residues. vii Joana Quaresma
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