| 001 - ETIQUETA DE REGISTO |
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| Identificador do registo |
384330 |
| 100 ## - DADOS GERAIS DE PROCESSAMENTO |
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| Dados gerais de processamento |
20070606d2006 y0pory50 ba |
| 101 ## - LÍNGUA DA PUBLICAÇÃO |
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| Língua do texto, banda sonora, etc. |
Inglês |
| 200 ## - TÍTULO E MENÇÃO DE RESPONSABILIDADE |
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| Título próprio |
Accurate mass analyses of peroxides explosives |
| Primeira menção de responsabilidade |
Filipa Belchior |
| 210 ## - PUBLICAÇÃO, DISTRIBUIÇÃO, ETC. |
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| Lugar da publicação, distribuição, etc. |
[Stoke on Trent] ; [Seven Oaks] |
| Nome do editor, distribuidor, etc. |
[s.n.] |
| Data da publicação, distribuição, etc. |
2006 |
| 215 ## - DESCRIÇÃO FÍSICA |
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| Indicação específica do tipo de material e extensão do item |
vi, 136 f., anexos |
| Dimensões |
30 cm |
| 300 ## - NOTAS GERAIS |
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| Texto da nota |
Degree of Masters of Science in Forensic Science, Faculty of Health and of Sciences (Staffordshire University) and Forensic Explosives Laboratory/Defense Science and Technology Laboratory. |
| 330 ## - SÚMULA OU RESUMO |
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| Texto da nota |
1. Introduction. 1.1 Aim of the project. 1.2 Background. 1.3 The Forensic Explosives Laboratory (FEL). 1.4 Explosives. 1.4.1 Definition. 1.4.2 Classification. 1.5 Historical reported use of he peroxide explosives 3,3,6,6,9,9-hexamethyl 1,2,4,5,7,8-hexoxonane (TATP) and 3,4,8,9,12,13-hexaoxa-1,6 diazabicyclo[ 4,4,4] tetradecane (HMTD). 1.5.1 TATP. 1.5.1.1 Molecular structure and properties. 1.5.1.2 Preparation of TATP. 1.5.1.3 TATP decompositions reactions. 1.5.2 HMTD. 1.5.2.1 Molecular structure and properties. 1.5.2.2 Preparation. 1.5.2.3 HMTD decompositions reactions. 1.6 Forensic analysis of peroxides explosives. 1.6.1 Spot tests. 1.6.2 Thermal methods. 1.6.3 Enzymatic reactions. 1.6.4 Separation methods. 1.6.5 Spectroscopic techniques. 1.6.6 Spectrometric techniques. 1.6.6.1 Mass spectrometry. 1.6.7 Chromatographic techniques hyphenated with mass spectrometry. 1.7 Liquid chromatography with mass spectrometry and tandem mass spectrometry (LC/MS and LC/MS/MS). 1. 7.1 Liquid chromatographic systems. 1.7.2 LC/MS and LC/MS/MS ion sources. 1.7.3 Quadrupole analysers. 1.7.4 Tandem mass spectrometry. 1.8 Mass spectra of TATP and HMTD. 1.8.1 TATP spectra. 1.8.2 HMTD spectra. 1.9 Accurate mass. 1.9.1 Accurate mass measurements. 1.9.2 Amount of error. 1.9.3 Lock fiasses. 2. EXPERIMENTAL. 2.1 Apparatus and laboratory conditions. 2.2 Preparation of solutions. 2.3 to 2.12 Methods and analyses. 2.3 LC/MS/MS initial conditions. 2.4 Liquid chromatography instrumental conditions. 2.5 Robustness and repeatability of the injection modes; sensitivity. 2.6 Instrument calibration for accurate mass measurements. 2.7 Optimisation of TATP m/z values and instrument parameters. 2.8 Accurate mass analyses of TATP parent ions m/z 89 and m/z 240. 2.8.1 With PEG-200 ammoniated species as lock masses. 2.8.2 With PEG-200 protonated species as lock masses. 2.8.3 With PEG-200 ammoniated species and methanol clusters as lock masses. 2.8.4 With methanol clusters as lock masses. 2.9 Optimisation of the method and mobile phase for the analysis of HMTD. 2.9.1 Mobile phase methanol/water. 2.9.2 Mobile phase acetonitrile/water. 2.10 Determination of HMTD product ions. 2.11 HMTD tune parameters optimisation and background evaluation. 2.12 Accurate mass analyses of HMTD ions. 2.12.1 Accurate mass analyses of parent ions m/z 179, m/z 207 and m/z 209. 2.12.2 Accurate mass analyses of product ions. 3. Results and discussion. 3.1. Liquid chromatography instrumental conditions. 3.1.1 Carry over and peak shape. 3.1.2 Robustness and repeatability of injection modes; sensitivity. 3.2 TATP methods and accurate mass analyses. 3.2.1 Optimisation of parent ions m/z values and instrument parameters. 3.2.2 Accurate mass measurements of m/z 89 and m/z 240. 3.2.2.1 With PEG-200 ammoniated species as lock masses. 3.2.2.2 With PEG-200 protonated species as lock masses. 3.2.2.3 With PEG-200 ammoniated species and methanol clusters as lock masses. 3.2.2.4 Using methanol clusters as lock masses. 3.3 HMTD methods and accurate mass analyses. 3.3.1 Optimisation of the method and mobile phase for HMTD analyses. 3.3.2 Determination of HMTD productions. 3.3.3. Evaluation of the background with PEG solution. 3.3.4 Accurate mass results of HMTD parent ions. 3.3.4.1 Accurate mass measurement of the m/z. 3.3.4.2 Accurate mass measurement of the m/z 209. 3.3.4.3 Accurate mass measurement of the m/z 207 . 3.3.5 Accurate mass determinations of HMTD product ions. 3.3.5.1 Accurate mass measurement of product ions of m/z 179. 3.3.5.2 Accurate mass measurement of product ions of m/z 207. 3.3.5.3 Accurate mass measurement of product ions of m/z 209. 4. Conclusions. 4.1. LC/MS/MS instrumental conditions. 4.2 Accurate mass measurements. 4.3 TATP accurate mass results. 4.4 HMTD accurate mass results. 4.5 Accurate mass results in the forensic field. 5. Further work. 6. References. Appendices. |
| 606 ## - NOME COMUM USADO COMO ASSUNTO |
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| Elemento de entrada |
ANÁLISE LABORATORIAL |
| ID Autoridade |
326721 |
| 606 ## - NOME COMUM USADO COMO ASSUNTO |
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| Elemento de entrada |
ENGENHO EXPLOSIVO |
| ID Autoridade |
344116 |
| 606 ## - NOME COMUM USADO COMO ASSUNTO |
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| Elemento de entrada |
QUÍMICA ANALÍTICA |
| ID Autoridade |
343110 |
| 606 ## - NOME COMUM USADO COMO ASSUNTO |
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| Elemento de entrada |
CIÊNCIA FORENSE |
| ID Autoridade |
321508 |
| 606 ## - NOME COMUM USADO COMO ASSUNTO |
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| Elemento de entrada |
TESE |
| ID Autoridade |
334284 |
| 700 ## - NOME DE PESSOA - RESPONSABILIDADE PRINCIPAL |
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| Palavra de ordem |
BELCHIOR |
| Outra parte do nome não tomada para palavra de ordem |
Filipa |
| ID Autoridade |
353764 |
| 955 ## - |
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| -- |
Oferta |
| 995 ## - LOCALIZAÇÃO E INFORMAÇÃO DE EXEMPLARES |
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0 |
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PJ_19_000000000000000_D_95 |
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2022-06-06 |
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2022-06-06 |
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0 |
