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Field detection of drugs and explosives by SPME-IMS [Documento electrónico] : final technical report / Jose Almirall .. [et al.].- [Miami, FL] : ed. do a., 2012.- 1 CD-ROM ; 12 cm
Research report from the Department of Chemistry and Biochemistry and
International Forensic Research Institute (Florida International University) submitted to the U.S. Department of Justice - Award nr. 2006-DN-BX-K027. Ficheiro de 5,98 KB em formato PDF (275 p.). Disponível também através de: https://www.ncjrs.gov/pdffiles1/nij/grants/237837.pdf. Acedido a 31 de maio de 2012.
DETECÇÃO DE DROGA, DETECÇÃO DE EXPLOSIVOS, ANÁLISE DE VESTÍGIOS, ANÁLISE LABORATORIAL, ESPECTROMETRIA
CHAPTER PAGE. Abstract. Executive Summary. Chapter 1 STATEMENT OF THE PROBLEM - Security concerns. Explosives. Illicit drugs. Research approach in response to current needs. Project goals and hypotheses. Chapter 2 EXPLOSIVES AND ILLICIT DRUGS. Chemistry of explosives. Propellants. Military explosives. Chemistry of illicit drugs. Cocaine. Marijuana. MDMA. Field analysis of explosives and illicit drugs. Biological detection. Chemical detection. Chapter 3 VOLATILE CHEMICAL SIGNATURES. Definition of volatile chemical signatures. Volatile chemical signatures of explosives. Volatile chemical signatures of drugs. Delivery methods for volatile chemical signatures. Chapter 4 SOLID PHASE MICROEXTRACTION. Theory of solid phase microextraction. Historical aspects of SPME. Thermodynamics. Kinetics. Practical aspects of sampling. Extraction modes. Microextraction. Sorbent chemistry. Phase chemistry. Sol-gel coating technology. Chemical reactions in the sol-gel process. Sol-gel SPME coatings. La (dihed) phase chemistry. Characterization of sorbent polymers. Scanning electron microscopy. 1H Nuclear magnetic resonance spectroscopy. Direct-infusion mass spectrometry. Infrared spectroscopy. Chapter 5 ION MOBILITY SPECTROMETRY - Ion chemistry. IMS response. Forensic applications of ion mobility spectrometry. IMS Modifications to improve contraband detection. Sampling improvements. Operating condition optimization. Chapter 6 METHODOLOGY AND LAB PREPARATION TECHNIQUES. Development of Planar SPME (PSPME) devices for static extractions. Preparation of the substrate. Coating techniques. Dip-coating. Spin-coating. Preparation of the coating solutions. Sol-gel PDMS. PDMS by a chlorine-terminated PDMS route. Activated Charcoal/Sol-Gel PDMS. La (dihed). Validation experiments for static PSPME. IMS detection. Performance comparison of the SPME Fiber, PDMS, and sol-gel PDMS PSPME devices using TNT as the target analyte. Quantitation of TNT using response curves. Determination of equilibrium extraction time and recovery. Extraction efficiency experiments at equilibrium. Comparison of Sol-Gel PDMS PSPME and Fiber SPME for sampling piperonal. Gas Chromatography- Mass Spectrometry (GC/MS). IMS operating conditions. SPME-IMS sampling. SPME-IMS quantitation. SPME-IMS Limit of Detection (LOD) and Linear Dynamic Range (LDR) Determinations. Piperonal IMS response curve. Method development for PSPME-IMS of Piperonal. Performance of PSPME for other volatile chemical signatures. Performance of PSPME for the smokeless powder volatile chemical signatures. Determination of equilibrium extraction time. PSPME static sampling of TNT from a large volume vessel. Comparison of Planar La (dihed) SPME devices with control planar sol-gel and PDMS devices for the extraction of TNT and 2,4-DNT. Aging study. Coating study. Development of dynamic PSPME. Preparation of dynamic PSPME devices. Coating method development. Characterization of final dynamic PSPME devices. Dynamic sampling. Volatile chemical signature standards for dynamic PSPME sampling. Controlled Odor Mimic Permeation Systems (COMPS). Validation experiments for dynamic PSPME. Dynamic PSPME retaining capability studied by analyte solution spiking. Dynamic PSPME retaining capability studied by COMPS vapor source. Dynamic PSPME LOD. Chapter 7 RESULTS AND DISCUSSION. Development of PSPME devices for static extractions. Sol-gel PDMS. PDMS PSPME via a chlorine-terminated PDMS route. Activated charcoal in PDMS formulations. La (dihed). Structure determination. La (dihed) SPME coatings. Summary of PSPME devices developed. Validation experiments for static PSPME. Performance comparison of the SPME Fiber, PDMS, and Sol-gel PDMS PSPME devices using TNT as the target analyte. Quantitation of TNT using response curves. Determination of equilibrium extraction time and recovery. Extraction efficiency experiments at equilibrium. Study of TNT adsorption to vessel walls. Comparison of Sol-Gel PDMS PSPME and fiber SPME for sampling piperonal. SPME-IMS sampling. SPME-IMS quantitation. SPME-IMS Limit of Detection (LOD) and Linear Dynamic Range (LDR) determinations. Method development for PSPME-IMS of Piperonal. Sampling real MDMA cases at a Local Crime Laboratory. Performance of PSPME for other volatile chemical signatures. Performance of PSPME for the smokeless powder volatile chemical signatures. Smokeless powder volatile chemical signature IMS response curves. Determination of equilibrium extraction time. Sampling of unburned smokeless powders. PSPME static sampling of TNT from a large volume vessel. Comparison of Planar La (dihed) SPME devices with control planar Sol-gel and PDMS devices for the extraction of TNT and 2,4-DNT. Aging study. Coating study. Development of dynamic PSPME. Coating method development. Characterization of final dynamic PSPME devices. Volatile chemical signature standards for dynamic PSPME sampling. Spike on manufacturer provided filters. Controlled Odor Mimic Permeation Systems (COMPS). Validation experiments for dynamic PSPME. Dynamic PSPME retaining capability studied by analyte solution spiking. Dynamic PSPME retaining capability studied by COMPS vapor source. Dynamic PSPME LOD. Application of dynamic PSPME- IMS for screening of illicit compounds. Chapter 8 Controlled odor mimic permeation system (COMPS). Polymers. Polyethylene. Polypropylene. Creation of Controlled Odor Mimic Permeation System (COMPS) devices. Permeation of odor compounds. COMPS odor delivery of narcotics. Field trials and validation of COMPS for narcotics. COMPS odor delivery of explosive. Field trials and validation of COMPS for explosives. Chapter 9 CONCLUSIONS. Static PSPME. Dynamic PSPME. PSPME terminology. Implications of PSPME-IMS for security. Future directions. Controlled Odor Mimic Permeation System. REFERENCES. ANNEX A - Static PSPME preparation. ANNEX B - Dynamic PSPME preparation. Dissemination of research findings. Appendix A – Peer-reviewed publications derived from this work. Appendix B – Peer-reviewed presentations derived from this work. Appendix C – Copies of publications listed in Appendix A.