ANALYTICAL CHEMISTRY (3)

Author: PULIDO TOFIÑO PAULA.
Year: 2005.
University: COMPLUTENSE DE MADRID [www.ucm.es].
Place of defense: FACULTAD DE CIENCIAS QUÍMICAS.
Place of preparation: FACULTAD DE CIENCIAS QUÍMICAS.

Summary: The main objective of the research work which is presented in this report is the development of biosensors in flux for the determination of iron in the two states of oxidation and herbicide isoproturon. These analytes were selected because of the interest that presents its determination in environmental and food samples. The first by the need to monitorizarlos primarily on groundwater and sea in order to determine the content of Fe (II) and Fe (III) and thus be able to study the properties redoz of water analyzed, so this Related content and chemical form of trace elements present in them. The second is a herbicide of the family of fenilureas widely used especially in the cultured creales and potato, which could contaminate food and water effluent coming to places you apply, be legislated limits maximum allowable limit 0 , 05 ug / g in food and 0.1 ug / l in drinking water. Both methods require analytes sensitive, rapid and selective enabling its determination in situ and in real time. This work has identified a naturally fluorescent pigment virtually specific to the Fe (III) called Pioverdina which has enabled us to design and characterize a device analytically to determine the total inorganic iron, ferric and ferrous. This biosensor has been successfully applied to the specification of iron in water samples pit and the water and wine. The determination of isoproturon is carried out through a inmunosensor flow based on the immobilization targeted anti-isoproturon in various media as CPG-Proteína A GPC and only sol-gel glass, using different mechanisms such as covalent bond and entrapment. The biosensor has proved entirely selective for this herbicide and the limit of detection, 2-3, ug / l allows its determination in food, the limit permitted by law. Finally, we have developed methods precocentración in discontinuous and continuous in order to reduce the limit of detection and can apply the biosensor for the determination of isoproturon in drinking water. Through the use of a inmunoadsorbente online and the terminal sensitive glass sol-gel-antiisoproturon has developed a method for determining this herbicia level of 0.1 ug / l which allows monitorizarlo in drinking water.

Author: GUZMÁN VÁZQUEZ DE PRADA ANA.
Year: 2005.
University: COMPLUTENSE DE MADRID [www.ucm.es].
Place of defense: FACULTAD DE CC. QUÍMICAS.
Place of preparation: FACULTAD DE CIENCIAS QUÍMICAS.

Summary: The work has been to study and optimization of print molecular polymers synthesized with sulfametazaina (SMZ) and fenbendazole (FBZ) molecules as mold, and the development of methods for determining preconcentration SMZ in milk and FBZ in liver the maximum levels permitted by the European Union and the Commission of Codez Alimentarius. The work plan developed to achieve the goal be summarized as follows: * Electrochemical Studies. * Developing methods voltamperométricos and injection flow detection amperométrica for the determination of analytes. * Summaries of polymer molecular printing. * Analysis of real samples.

Author: BENITO PEÑA MARÍA ELENA.
Year: 2005.
University: COMPLUTENSE DE MADRID [www.ucm.es].
Place of defense: FACULTAD DE CIENCIAS QUÍMICAS.
Place of preparation: DPTO. QUÍMICA ANALÍTICA, FACULTAD DE CIENCIAS QUÍMICAS, UNIVERSIDAD COMPLUTENSE.

Summary: Doctoral Thesis This has been done within the framework of a project V Framework Program, funded by the EU within l area of Quality of Life and Management of Living Resources, "Cartridges with molecularly imprinted recognition elements for monitoring antibiotic residues in milk ". CREAM (Ref. QLK -1999-00902) Research conducted in the framework of the thesis presented can be summarized in the following points: 1-Characterization fotofísica and photochemistry of derivatives fluorescent penicillins for application in the analysis of antibiotics. 2-Developing an fluoroensayo competitive, based on the use of MIPs, as elements of appreciation for selective analysis of the family of antibiotics penicillins in food and medicine. 3-Development of a fluoroinmunoensayo competitive, fully automated, based on the use of derivatives fluorescent penicillins and polyclonal antibodies selective beta-lactámicos to antibiotics. Implementation of bionsensor analysis of samples of milk and the environment. 4-Development of a chromatographic method based on the technique of HPLC with UV detection for the determination of antibiotic residues beta-lactámicos (amoxilina, ampicillin, penicillin G, penicillin V, oxacillin, cloxacillin, nafcillin and dicloxacilina) in biological samples environmental and for the purpose of validating the devices developed. This objective includes optimization method in solid phase extraction (SPE) for the preconcentration and cleaning of the samples selected.

Author: PÉREZ ALONSO MAITE.
Year: 2005.
University: PAÍS VASCO [www.ehu.es].
Place of defense: FACULTAD DE CIENCIA Y TECNOLOGÍA.
Place of preparation: FACULTAD DE CIENCIAS.

Summary: The stone is not only the basic construction material of many monumental buildings, but it also is the main constituent of many artistic items of cultural and historical value. But as soon as the object is created begin the physical, chemical or biological processes that cause deterioration and threaten the continuity of the work. In this Doctoral Thesis shows the need to understand and study the properties that make up the Cultural Heritage from a multidisciplinary, and the importance of chemical analysis in the diagnosis and evaluation of cultural property. The first part presents the construction of a database (available on-line) based on technical vibrational spectroscopic FT-IR, FT-Raman and dispersive Raman as proposed methodology for the characterization and diagnosis of carbonate materials. In addition presents several examples of its application on real samples, reaching elucidate the main processes of deterioration taking place, and giving greater value to the analysis on the spot and completely non-destructive. The second part proposes an innovative treatment for protective materials with a high carbon content. This treatment called "LIPROX" is based on the technology of ion exchange and promotes the formation of a patina of calcium oxalate carbonated material on the surface. This will get greater resistance to acid attack generated by air pollution. The formation of the layer formed has been studied using techniques vibrational following the methodology presented in the first part.

Author: MACANÁS DE BENITO JORGE.
Year: 2005.
University: AUTÓNOMA DE BARCELONA [www.uab.es].
Place of defense: FACULTAT DE CIÉNCIES.
Place of preparation: FACULTAT DE CIÉNCIES.

Summary: The research contained in this report relate to the development of new materials and membranes with improved properties prepared by the technique of Reagents Incorporated in Solid Phase (Solid-Phase Incorporated Reagents, SPHINER). This technique is based on the incorporation of reagents in a solid phase through different procedures as a first step towards the development of composite materials. For this reason, we have prepared Membranes Composite Activadas (Activated Composite Membranes. ACM) acid di (2-ethylhexyl) ditiofosfórico as conveyor metal ions. This type of membrane bilayer membranes are formed by a support microporoso of polysulphone and a dense layer of polyamide and thin at the top. The interior is built trapping reagent is able to form stable complexes with the metals of interest. In this sense, the ACM has proven its ability to transport selective and effective in several metal ions such as zinc, cadmium, bismuth, copper, tin and indium. Based on data collected in the course of investigations, has developed a semi model to predict the flow of ions in a specific system in the light of the constant balancing of the species involved. Moreover, it has done a caracterizaicón morphological exhaustive associate for the structural parameters of the membrane with its transport properties. This characterization has shown that the formation of the layer of polyamide on commercial carriers polysulphone membrane produces some unsatisfactory properties without transportation required. In addition, new materials have been developed that incorporate in its interior metal nanoparticles (Metal Nanoparticles, MNP) by the procedure synthesis intermatricial both polymers funcionalizados as not funcionalizados. This has succeeded in synthesizing nanoparticles and solid metal nanoparticles mixed with structure "core-shell." The nanoparticles formed have been characterized by various microscopic techniques to determine the size, distribution and grade crystalline. All parameters have been considered satisfactory certain. Finally, nanoobjetos developed membranes have been incorporated as sensors amperométricos and as a result has increased its efficiency significantly.

Author: MERINO RODRÍGUEZ FRANCISCO.
Year: 2005.
University: CÓRDOBA [www.uco.es].
Place of defense: FACULTAD DE CIENCIAS.
Place of preparation: FACULTAD DE CIENCIAS.

Summary: The research contained in this doctoral thesis primarily aim to resolve the problem of the treatment of solid and liquid samples, slow and complex, as a prelude to the determination of organic contaminants in emerging environmental analysis. This proposed new procedures for extraction / preconcentration systems coacervados and absorbent, based on the use of aggregates micelares formed by surfactants, which obviate organic solvents is therefore compatible with the principles of sustainable chemistry. The major innovative aspects are summarized as follows: A - are proposed for new systems coacervados induced acid, using an anionic surfactant for the extraction of PAHs in soil, sediment and sludge focal. The coacervado increases their power extraction when it forms a agragado mixed between the analyte and extracting. This has been demonstrated by the removal of cationic surfactants (analytes) type alquil-amonio in sludge treatment plants in coming. Factors concentration in the phase rich in surfactant (caocervado) are very high. Separation / qualification identification of these pollutants are carried out by LC-fluorescencia (PAHs) and LC / (ESI-IT) -MS (for alquil-amonio). B - is proposed for the first time adsorbents new systems consist of a metal oxide coating of a agragado micelar (hemimicela / admicela) for use in PES. The technique was developed validated by adsolubilización of surfactants counterparts benzalkonio (BAS) and herbicides ammonium quaternario (quats). In order to adapt these systems adsorbents analysis routine has designed a device to link online to LC-MS. C-were developed new analytical methodologies based on the formation of aggregates mixed permicelares for the determination of cationic surfactants type dialquil-amonio in wastewater. The method is of great simplicity and selectivity.

Author: GUERRERO PEÑA ARMANDO.
Year: 2005.
University: SALAMANCA [www.usal.es].
Place of defense: EDIFICIO HISTORICO.
Place of preparation: DEPARTAMENTO QUIMICA ANALITICA, NUTRICION Y BROMATOLOGIA.

Summary: In this paper, have been a methodology for the rapid detection of soils contaminated with crude oil based on the coupling of a generator head space of a mass spectrometer. The samples were subjected to the process of generating head space without pretreatment and volatile generated are introduced directly into the mass spectrometer. This produces a spectral fingerprint of the sample tested contained information on the volatile generated and used as an analytical signal for the characterization of samples. It has been proposed the use of chromatography rapid gases-espectrometría mass coupled to a generator head space for the identification of major hydrocarbons present in samples of mineral and organic soils contaminated. The main advantages of the proposed methods is that manipulation of the sample prior to analysis is minimized. The method is rapid, simple and highly suitable for the detection of contaminated soil and the identification of pollution sources.

Author: GUTIÉRREZ TAMAYO FERNANDO.
Year: 2005.
University: COMPLUTENSE DE MADRID [www.ucm.es].
Place of defense: FACULTAD DE CC. QUÍMICAS.
Place of preparation: FAC. CC. QUÍMICAS.

Summary: The research work done in this thesis describes the synthesis and characterization of polymers post molecular printing (IPM) using different methodologies polymerization. These methodologies were employed to obtain spherical particles of known and desired morphology. Among them, was investigated by precipitation polymerization, the use of silica and silica-modified initiators type iniferter. Once prepared materials were evaluated using adsorption isotherms, electron microscopy, IR and elemental microanalysis. Finally, the IPM synthesized were employed as stationary phases for SPE and HPLC, which were obtained stationary phases for selective screening of various herbicides in plant samples.

Author: Esteve Turrillas Francesc Albert.
Year: 2006.
University: VALENCIA [www.uv.es].
Place of defense: Facultat de Química.
Place of preparation: Facultat de Química.

Summary: The objective of this thesis is the development of analytical methodologies for the determination of pesticides, using alternatives to traditional methods, such as pressurized fluid extractions and assisted by microwave for subsequent action through gas chromatography detection spectrometry masses. Additionally has evaluated the applicability of devices semipermeable membrane (SPMDs) as a passive samplers of pesticides, both air and water. The compounds have been studied pesticides for various families, including organochlorines, organophosphates, pyrethroids, carbamates and others, for which they have developed methodologies based on mass spectrometry in tandem for their determination, which provides a high selectivity and sensitivity. We have developed different methods for extracting samples, such as soil, food (and vegetable oils) and SPMDs. Methodologies classics as Soxhlet extraction, ultrasound or dialysis for the case of SPMDs employ large quantities of solvents, generating a very high volume of waste also require the extraction time high. The alternatives based on microwave assisted extraction (MAE) and pressurized fluids (PFE), provide the same results in less time and using fewer solvents, both methodologies being environmentally sustainable. In studies with SPMDs, the benefits of using MAE instead of dialysis are even more important because of the considerable reduction in the extraction time (from 48 to 1 h) and the solvent consumption (from 400 to 60 mL) . The procedure based EDP was used in the extraction of organochlorine pesticides in lettuce. Using this methodology as a tool of analysis, a study of pesticide absorption by plants lettuce, using as a means of cultivation, soil fortified Endosulfan two concentration levels 10 and 50 Â µ g / g. The absorption of a-Endosulfan, Ã-Endosulfan and Endosulfan sulfate per plant lettuce in these soils was very low, finding maximum levels of 2.5 Â µ g / g in roots and 0.8 Â µ g / g in sheets on the floor more contaminated. It has developed a methodology for cleaning extracts for determining pyrethroid insecticide residues in samples fat, using a partition acetonitrile: hexane followed by a solid phase extraction with alumina and C18. Extracts obtained with solid waste coming to 2 mg allows direct injection into the gas chromatograph without polluting the system. In addition, this procedure can be used for cleaning extracts of different pesticides families studied. Absorption tests were conducted using SPMDs for pesticide passive sampling air and water. For the deployment of these devices, only requires a small technical support, thereby considerably reduce the cost of monitoring campaigns. He also confirmed the efficiency of these samplers to control pyrethroid insecticides in the air inside homes. Similarly, a study of absorption of various families of pesticides in water, using SPMDs, obtaining a high absorption for compounds pyrethroids, and the majority of organochlorine pesticides and orqanofosforados. Finally, it was observed that the absorption of pesticides by SPMDs does not depend on the composition of the water (salinity, pH and the presence of organic matter), but slightly increased with temperature. As we conclude that can be used SPMD as pesticides water samplers.

Author: Cortina Puig Maria Montserrat.
Year: 2006.
University: AUTÓNOMA DE BARCELONA [www.uab.es].
Place of defense: Universitat Autonoma de Barcelona.
Place of preparation: Universitat Autonoma de Barcelona.

Summary: The history of chemical sensors them from the beginning of the last hundred years is a sequence of discoveries sensor selective. However, during the past decade, have suggested new applications such as the use of non-selective sensor arrays, which are often combined with mathematical methods of signal processing based on artificial intelligence and pattern recognition, such as artificial neural networks (RNAs). These systems, known as artificial senses, and working in a similar manner to the human senses, have led to the electronic noses and tongues, for gaseous and liquid samples, respectively. The main objective of this work involves the development and optimization of several languages based on different principles electronic measurement. The sensors have been used over the potentiometric, although they have made significant contributions with sensors impedimétricos, where the signal is derived from a range of impedances. It also has developed a language-based electronic biosensors inhibition. In all cases, the RNAs have been used as a tool quimiométrica to process the information obtained. As the volume of information required to train a RNA is very high, it is proposed to use a system of sequential injection analysis (SIA) to automatically generate. Thus, this information can be obtained quickly, easily, and without manual intervention. This contribution represents a major improvement for this system, as can be developed, quickly and automatically, electronic different languages for the simultaneous determination of the species of interest without the need to remove interfering. Another important innovation has been the use of dynamic component of the signal-instead of using the signal static potential, which is widely used in the field of electronic languages. This new process has yielded better results in the simultaneous quantification of species of interest present in a sample, without the need to remove interfering. In summary, this paper presents four different electronic language, along with other additional work required to optimize these and future electronic languages.

Author: PARRA MANZANARES ALEJANDRO.
Year: 2006.
University: LA RIOJA [www.unirioja.es].
Place of defense: UNIVERSIDAD DE LA RIOJA.
Place of preparation: CENTRO CIENTÍFICO TECNOLÓGICO UNIVERSIDAD DE LA RIOJA.

Summary: The bioaerosols are a particular type of air pollutant because of its organizational structure complex and varied, with an impact on health for their properties biológicas.Se has conducted a study to try to classify bacteria in the form of bioaerosol through the technique of Laser Induced Fluorescence (IBF). Such a classification has been carried out according to name, morphology, order and Gram of bacterias.En First, it has been designed and optimized using a system FIL design of experiments, after which have been analyzed 46 bioaerosols pattern. The data obtained have enabled correctly classify the bacteria through Discriminante Linear Analysis. As a direct application, have been collected air samples and the results obtained using the system have been optimized contrasted with microbiological methods convencionales.Finalmente, has conducted a study in the Department of Chemistry, University of Florida (Gainesville, USA) in collaboration with the group of teachers J. Winefordner and N. Omenetto. This study has used a system FIL for measuring fluorescence decay, using the data obtained as a complement to the classification of bioaerosols.

Author: Teodoro José Antonio.
Year: 2006.
University: A CORUÑA [www.udc.es].
Place of defense: Escuela Universitaria Politécnica de Ferrol.
Place of preparation: Universidad Luterana do Brasil-Portoalegre.

Summary: From a case study of ethnographic type, which investigated the practice of environmental education, in the municipality of caarapó, in the village caarapó. The research has as its main objective, from the relationship of indigenous peoples with lso their territories and natural resources, contributing to the construction of subsidies for a program of environmental education. At first, the investigator introduced the practice of research, trying on the beaten paths for the construction of field work and the choice of descriptive research in the form of case study. There was some discussion, in a second stage, the history of the guarani and Kaiowa, roads traveled, their questions about the culture of people. Afterwards, it was conceptuón training for environmental preservation. Data originating in the field work were presented and discussed. One of them was the proposal and the concept of environmental education, and the other analyzed data found, presenting styles practice crítico and técnico-reproductivo present in the making of the Kaiowa / Guarani. Analysis and interpretation of the data revealed interesting aspects, which can contribute to a more realistic approach in environmental education. The comparison of these data with theoretical formulations initially designed evidención that investigators of this ethnic group need not go cualificándose to develop a practical proposal thoughtful, pedagogical conscious actions, and that will bring emancipation, forming in critical sense and commitment to social and environmental.

Author: LÓPEZ SOTO M. DOLORES.
Year: 2006.
University: EXTREMADURA [www.unex.es].
Place of defense: FACULTAD DE CIENCIAS.
Place of preparation: UNIVERSIDAD DE EXTREMADURA.

Summary: Olive oil, one of the key foods in the diet of the Mediterranean Basin, and from which Spain, in general, and Extremadura, in particular, are major producers and consumers, this is the kind of memory. It will develop analytical methods for identifying compounds which affect the quality of olive oil. It identified metals as copper and iron, in addition to pesticides. Pesticides subject of study in olive oil have been dimethoate, fenton and fenirrotión, pesticides organofosforedos that are widely used in Extremadura to combat pests that affect the quality of olives. Moreover pesticides have been studied for their determination in river water. The techniques that have been used have been spectrophotometry, chromatography and techniques voltamperométricas.

Author: SUAREZ GONZALEZ BEATRIZ.
Year: 2006.
University: CÓRDOBA [www.uco.es].
Place of defense: CAMPUS DE RABANALES.
Place of preparation: CAMPUS DE RABANALES.

Summary: This Doctoral Thesis has focused on: 1 - The development of analytical processes effective and reliable procedures for the characterization and quantification of carbon nanostructures (mainly carbon nanotubes mono-and multilayer). 2-Developing new analytical tools based on the use of nanostructures of carbon comprising two basic aspects: as absorbent material in processes in solid phase extraction and as a stage pseudoestacionaria with a view to developing new ways electroforéticas separation. The report comprises an extensive introduction in which he made a thorough review of the nature, properties and types of carbon nanotubes: the synthesis and characterization techniques and applications developed to date in the various fields of science, being the dedicated last part to the present and future applications of nanotubes in Analytical Chemistry. In the following chapters are collected experimental data highlights of the research and these results are discussed critically. As most significant findings are the following: 1 - has been shown potential as capillary electrophoresis technique for the separation and characterization of carbon nanotubes, funcionalizados or not. 2-It has been shown that the combined use of surfactants and polymers is an effective strategy to achieve stable dispersions of nanotubes and homogeneous. 3-It has been revealed the advantages of incorporating carbon nanotubes as tools within the analytical process, as phase pseudoestacionaria in electroferesis capillary and absorbent material for the treatment and conditioning of the sample. On this last point it has been demonstrated that nanotubes funcionalizados and immobilized on glass capable of performing more effective retention and selective.

Author: SANTOS MORCILLO JUAN LUIS.
Year: 2006.
University: SEVILLA [www.us.es].
Place of defense: FACULTAD DE BIOLOGÍA.
Place of preparation: FACULTAD DE QUÍMICA.

Summary: In recent years, the increase in the consumption of drugs, both for human and veterinary use, is causing a new environmental problem. As a result, studies on the fate of these pollutants in the aquatic environment and its potential effects on humans and ecosystems have been increased. After eating, drugs are partially processed by the body, through various metabolic processes, and released to the environment. The concentration at which these substances are found in the environment will depend on the quantities manufactured, dose effect, pharmacokinetic characteristics, properties of adsorption, etc.. Once released, the drug reaches the plants wastewater treatment (WWTPs), which are partially removed, and subsequently discharged to the receiving channels. As a result, WWTPs can consider as the major source of drugs to the environment. Moreover, the concentration of drugs, its temporal evolution and the potential synergistic and antagonistic effects depend not only content downloaded by WWTPs, but also depend on the geographic location and climatic conditions. Thus, it becomes necessary to track time in connection with climatic conditions in the study area in order to assess the possible negative effects of these pollutants in the environment. In this dissertation work is optimized and validated an analytical method for determining the content so routine in five anti-inflammatory drugs (acetaninofeno, diclofenac, ketoprofen, naproxen and ibuprofen), an antiepileptic (carbamazepine), and a nervous stimulant (caffeine ) in waste water from the four WWTPs conducting sanitation water from the city of Seville. We carried out the characterization of sewage from the city of Seville, through the identification of drugs and physicochemical characterization parameters for a period of one year, thus discriminating between the influence of the weather and of industrial inputs in the presence of these compounds in WWTPs. In addition, we performed an assessment of the data obtained, establishing distribution profiles of the drugs studied and elimination yields achieved in each of the WWTPs on which conducts sampling. Lastly was conducted environmental impact assessment that these chemicals may have on the aquatic environment of the city of Seville.