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A Fast NIR Spectrometer for Examining Explosive Events: Emission of PETN Based Explosives and H₂O Absorption Method FeasibilityPiecuch, Scott. January 2009 (has links)
Thesis (M.S.)--Marquette University, 2009. / Jon D. Koch, John P. Borg, James M. Lightstone, Advisors.
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Explosive Residue Transfer from Various Explosive Ordinance Disposal (EOD) Render Safe Procedures (RSP)Stein, Joseph A 01 January 2019 (has links)
Before an IED is sent to a laboratory for analysis, it needs to be rendered safe if it did not already initiate. Render safe procedures (RSPs) include utilizing a percussion-actuated non-electric (PAN) disrupter or a mineral water bottle disrupter. Each disrupter utilizes explosives to render the device safe by breaking open the container or disrupting the fuzing system. However, the same explosives used in the RSP are also used by criminals in IED construction. As such, the explosives used in the RSP can cause problems with the interpretation of the results from forensic analysis of the IED fragments. Compounds of analytical interest in residue include nitroglycerin (NG), diphenylamine (DPA), ethyl centralite (EC), methyl centralite (MC), and pentaerythritol tetranitrate (PETN). Instrumentation used in the analysis of the residues included a gas chromatograph/mass spectrometer (GC/MS), a liquid chromatograph/mass spectrometer (LC/MS), and a gas chromatograph with an electron capture detector (GC/ECD).
The PAN disrupter smokeless powder contained NG, DPA, and EC while the bulk detonation cord contained PETN. Only DPA decomposed after being burned. No residue was detected on the PVC pipes while residue was detected on the steel pipes and backpack mock IEDs. Overall, finding such residue in casework should not rule out the possibility that an individual used a particular explosive in the construction of the IED, but examiners should be aware of residues left by disrupters especially if the device initiates during the RSP.
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Fabrication of stable biocatalyst networks for the manufacture of fine chemicalsHickling, Christopher January 2016 (has links)
There is an important need to immobilise enzymes for use in industry, to do this I have the promising idea that by conjugating the enzyme to a hydrogel network, thus fabricating a stable biocatalytic network would be a potential method for immobilising enzymes for the manufacture of fine chemicals, this has not been done before for octapeptide systems. Hydrogels have been previously shown as a viable way of immobilising and stabilising enzymes. In this thesis the octapeptide VKVKVEVK (V is valine, K is lysine and E is glutamic acid) is used to immobilise enzymes tagged with VKVKVEVK. This peptide sequence is chosen as it forms stable hydrogels at enzyme appropriate conditions (pH 7). The enzymes chosen are; PETNR as it is well understood and is therefore a good starting point, CDH and CHMO were also chosen as they could combine with PETNR to form a cascade reaction. PETNR was both chemically conjugated to VKVKVEVK (SpepPETNR) and also genetically modified to express the peptide tag (CpepPETNR), whilst CDH and CHMO were genetically modified to express the tag (NpepCDH and CpepCHMO respectively). For S/CpepPETNR retention within the hydrogels was superior to retention for untagged PETNR. NpepCDH was found to not precipitate within the hydrogel whilst untagged was found to do so. CpepCHMO functionalised hydrogels were found to be heterogeneous. Characterisation of CpepPETNR functionalised hydrogels was undertaken using micro differential scanning calorimetry (µDSC), rheology, small angle neutron scattering (SANS) and atomic force microscopy (AFM). From the µDSC evidence of 'protective immobilisation' was observed by the increase in denaturation energy (+253 kJ mol-1) in the hydrogel in comparison to in solution (+18 kJ mol-1). The ability of S/CpepPETNR functionalised hydrogels to perform the ketoisophorone to levodione biotransformation reaction was explored with yields of 86%. S/CpepPETNR within VKVKVEVK hydrogels was found to retain ~90% conversion for at least 9 months at room temperature. Incubation overnight at 90°C resulted in a yield of 84% of levodione. These two results added more evidence for 'protective immobilisation'. Hydrogels functionalised with NpepCDH or CpepCHMO were characterised using rheology and atomic force microscopy. The biotransformation ability of NpepCDH was elucidated; the overall yield of carvone was a maximum of 54% from the hydrogel phase. NpepCDH was used alongside CpepPETNR for the cascade reaction producing dihydrocarvone in low yields; however, an improvement from 2% to 13% in yield is presented. The yield of lactone products from CpepCHMO functionalised hydrogel was low at 15%. The CpepPETNR/ CpepPETNR cascade reaction proceeded with a yield of 36%. The initial activities of CpepPETNR, NpepCDH and CpepCHMO were assayed in both solution and in gel phase using a modified method. The activities were assessed with varying conditions; temperature, pH, quantity of ethanol and incubation at high and low temperatures. Generally, it was found that immobilisation within the hydrogel phase resulted in 'protective immobilisation' against non-optimal conditions. This work will be of benefit to those who are interesting immobilising enzymes within hydrogels in the future.
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Contaminants and decomposition products in naturally aged pentaerythritol tetranitrate (PETN)Brackett, Claudia L. 01 January 2005 (has links) (PDF)
PETN is characterized by its sensitivity to environmental conditions. However, anhydrous low-temperature decomposition is poorly understood. This research undertook the search for the decomposition products of naturally aged PETN. This study did not detect any decomposition products. The methods tried were NMR, HPLC, mass spectrometry, and HPLC. PETN's behavior was sensitive to mass spectral conditions and resulted in adduct formation and artifactual decomposition. Artifacts could be sources of misinterpretation for true decomposition. Such behaviors included PETN's autonitration and nitrate's clinging to instrument surfaces. Additionally, PETN seemed able to autooxidize which produced an [M] − ion and [M+H] − ion that obscured isotopic information. Conditions that enhanced the abundance of the [M−H] − ion also increased PETN artifactual decomposition. Because an ion at m/z 330 could represent PETRIN, it was studied and candidated to be an artifact. This PETRIN-acetate isobar was formed from PETN in the presence of acetate. An illusion that a new mass at m/z 330 materialized could be due to spray chamber temperatures. The ion stayed relatively constant throughout a temperature increase while the abundance for other PETN ions decreased. This created an illusion of increasing abundance when the mass spectrum was displayed in normalized mode. An HPLC gradient of acetonitrile/water with addition of 3% NH 4 OH and 0.1 M ammonium acetate in methanol produced chromatographic peaks. However, these species were artifacts formed in the presence of hydroxide ion. Hydroxide accelerated the disappearance of the ion at m/z 315, but not the ion at m/z 378. A second HPLC system used an acetonitrile/water gradient with added 3.3 M ammonium acetate in methanol. However, no difference between PETN and naturally aged PETN chromatograms was evident. In an additional experiment, with the HPLC effluent collected in aliquots and analyzed separately, no condensed phase decomposition product was observed. Because the NMR, HPLC and mass spectrometry experiments did not detect condensed phase decomposition products, the decomposition products might be gas(es). In support, the explosives HMX and RDX are known to decompose in gas phase reactions. It is reasonable that naturally aged PETN proceeds through the same mechanism. The findings of this dissertation supported this viewpoint.
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Detection of PETN Using Peptide Based Biologically Modified Carbon NanotubesKubas, George D. 24 May 2017 (has links)
No description available.
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Voltametrické stanovení pentritu pomocí rtuťových a stříbrných amalgamových elektrod / Voltammetric Determination of Penthrite Using Mercury and Silver Amalgam ElectrodesVyvadil, Jan January 2015 (has links)
This Diploma Thesis is focused on investigation of the voltammetric behavior of the explosive penthrite (pentaerythritol tetranitrate) (PETN) and on searching for optimum conditions for its determination using differential pulse voltammetry (DPV) at a hanging mercury drop electrode (HMDE) (this part of the Diploma Thesis follows the topic investigated in the author's Bachelor Thesis; in this Diploma Thesis, the results of the Bachelor thesis are applied to the determination of PETN in environmental matrices) and at a mercury meniscus modified silver solid amalgam electrode (m-AgSAE) and on investigation of voltammetric behavior in real samples (deionized, drinking, and river water). For investigating the behavior of PETN in aqueous-methanolic media on the m-AgSAE, mixtures of Britton-Robinson buffers (BR-buffers) and methanol in various volume ratios were used. In non-aqueous media, methanolic solutions of tetramethylammonium bromide (TMAB), tetrabutylammonium iodide (TBAI), and tetrabutylammonium chloride (TBAC) were used as supporting electrolytes. Firstly, the influence of pH (in the range of 2 - 13) and methanol content (10 - 90 vol. %) on voltammetric responses of PETN was studied. The best response was obtained at each of those pH values at the volume ratio of BR-buffer - methanol of 1:9 or...
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Nanolithography on thin films using heated atomic force microscope cantileversSaxena, Shubham 01 November 2006 (has links)
Nanotechnology is expected to play a major role in many technology areas including electronics, materials, and defense. One of the most popular tools for nanoscale surface analysis is the atomic force microscope (AFM). AFM can be used for surface manipulation along with surface imaging.
The primary motivation for this research is to demonstrate AFM-based lithography on thin films using cantilevers with integrated heaters. These thermal cantilevers can control the temperature at the end of the tip, and hence they can be used for local in-situ thermal analysis. This research directly addresses applications like nanoscale electrical circuit fabrication/repair and thermal analysis of thin-films. In this study, an investigation was performed on two thin-film materials. One of them is co-polycarbonate, a variant of a polymer named polycarbonate, and the other is an energetic material called pentaerythritol tetranitrate (PETN).
Experimental methods involved in the lithography process are discussed, and the results of lithographic experiments performed on co-polycarbonate and PETN are reported. Effects of dominant parameters during lithography experiments like time, temperature, and force are investigated. Results of simulation of the interface temperature between thermal cantilever tip and thin film surface, at the beginning of the lithography process, are also reported.
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