Numerous compact NMR spectrometers have been designed for an easy measurement of proton NMR spectra. High sensitivity and resolution can be reached even with low field spectrometers (LFNMR) (i.e. 60 MHz), thanks to great improvements in electronic hardware, which open up a wide field of analytical quantification and relaxation applications. A specificity of Low field NMR spectrometer is the use of a permanent and cryogen free magnet technology, avoiding the need for weekly and expensive cryogenic services. Here we present and describe a low field NMR spectrometer fabricated in our laboratory. This spectrometer (ECBLFNMR) operates at basic resonant frequencies ranging from 1 to 60 MHz, with standard sample diameter (5-10 mm). All the embedded hardware is very compact and requires only a 24 V DC power supply, so this spectrometer is portable, easy to install and has a small footprint. This ECBFLNMR is dedicated to education and quantification, and enables low-field NMR research. It may be coupled with scientific experiments not requiring high magnetic fields.

Este projeto teve como objetivo a construção e automatização de um espectrômetro de baixo custo que tem como principal aplicação a caracterização de meios porosos. Para realizar a caracterização de um meio poroso é necessário que o campo magnético externo aplicado não seja intenso para diminuir os problemas relacionados com a diferença de susceptibilidade magnética na interface fluido-solido. Por este motivo, foi construído um magneto resistivo de baixo campo, operando na frequência de próton de 2MHz (0.047 Tesla) e de simples design. Para manter o equipamento com custo mais baixo possível foram construídos em laboratório a fonte de alimentação do magneto, um amplificador ajustado para 2MHz e os componentes λ/4 e os softwares necessários. O software desenvolvido tem a finalidade de controlar a placa de geração e aquisição de radiofrequência que foi adquirida pela empresa Spincore, denominada RadioProcessor. Para esta finalidade optou-se pela construção de uma nova API na linguagem C++, utilizando a API original do RadioProcessor como base, de forma a montar um conjunto de funções simples e intuitivas para a utilização do espectrômetro. Além disso, foi realizada a integração de uma linguagem script à biblioteca, que dá acesso ao usuário a todas as funções básicas de programação, permitindo que um usuário com pouca habilidade de programação possa criar um programa para o controle total do equipamento de forma simples e também tornando o software maleável, sendo possível que novas funções sejam integradas. Isso abre espaço para que o equipamento possa ser utilizado para outras aplicações além das citadas anteriormente. Somada à nova biblioteca, uma interface gráfica foi desenvolvida, a qual compreende o programa de controle do equipamento e também funções para tratamento e visualização de dados, como a transformada inversa de Laplace e transformada de Fourier. / The objective of this project was the assembling and automatization of a low cost NMR spectrometer for the characterization of porous media. The study of porous media through NMR spectroscopy requires a low intensity magnetic field in order to avoid the problems related to the difference of magnetic susceptibility on the fluid-solid interface. For that reason, a low field electromagnet, operating on the proton frequency of 2MHz (0.047 Tesla) and of simple design was built. As to keep all the equipment as low cost as possible, the following components were also assembled in laboratory: the magnets power supply, a 2MHz amplifier, the quarter-wave components and the necessary softwares. The goal of the software developed was to control the RF generation and acquisition board, which was acquired from the enterprise Spincore, further named RadioProcessor. To achieve this goal, it was decided the development of a new API, in the C++ language, which uses the original boards API as a base in order to assemble a group of functions that are simpler and more intuitive to the end user. In addition, a script language was integrated to the APIs library, allowing users with little programming knowledge to write a program which controls the whole equipment in an easy way and also adding flexibility to the software, as it becomes easy to add new functions. This permits that the equipment be easily changed to include other applications in the future. Finally, a graphical interface was developed, which comprehends the equipment control software and the visualization of the data.

Nuclear magnetic resonance (NMR) is a common tool utilized in core analysis. NMR can reveal important information about pore structure, fluid configuration and wettability. However, standard NMR core analysis techniques look at the sample as a whole or only at thin slices. Two NMR pulse sequences are introduced that allow for the determination of relaxation time or diffusion-relaxation time distributions as a function of sample height. One-dimensional T 2 and D-T 2 profiles can be determined with a low-field Maran Ultra spectrometer by implementing nuclear magnetic resonance imaging techniques. Frequency encoding gradients impart spatial resolution to the measurements and allow for the creation of T, and D-T 2 profiles without having to perform multiple slice selective measurements. The first technique, denoted as RARE, relies solely on resolving transverse relaxation, T 2 , as a function of height. The second method, D-T 2 profiling, allows for the determination of both the diffusion coefficient, D, and T 2 as a function of height. The ability to resolve D in addition to T 2 allows fluids with overlapping relaxation times to be distinguished, and therefore it is not necessary to use D 2 O in order to differentiate the water signal from the oil signal. Implementation of these two methods allows for the determination of porosity and saturation profiles. Experiments were performed with a sandpack in order to demonstrate the applicability of these two techniques, and saturation profiles of a sandpack were determined at various stages of the flooding process.

Este projeto teve como objetivo a construção e automatização de um espectrômetro de baixo custo que tem como principal aplicação a caracterização de meios porosos. Para realizar a caracterização de um meio poroso é necessário que o campo magnético externo aplicado não seja intenso para diminuir os problemas relacionados com a diferença de susceptibilidade magnética na interface fluido-solido. Por este motivo, foi construído um magneto resistivo de baixo campo, operando na frequência de próton de 2MHz (0.047 Tesla) e de simples design. Para manter o equipamento com custo mais baixo possível foram construídos em laboratório a fonte de alimentação do magneto, um amplificador ajustado para 2MHz e os componentes λ/4 e os softwares necessários. O software desenvolvido tem a finalidade de controlar a placa de geração e aquisição de radiofrequência que foi adquirida pela empresa Spincore, denominada RadioProcessor. Para esta finalidade optou-se pela construção de uma nova API na linguagem C++, utilizando a API original do RadioProcessor como base, de forma a montar um conjunto de funções simples e intuitivas para a utilização do espectrômetro. Além disso, foi realizada a integração de uma linguagem script à biblioteca, que dá acesso ao usuário a todas as funções básicas de programação, permitindo que um usuário com pouca habilidade de programação possa criar um programa para o controle total do equipamento de forma simples e também tornando o software maleável, sendo possível que novas funções sejam integradas. Isso abre espaço para que o equipamento possa ser utilizado para outras aplicações além das citadas anteriormente. Somada à nova biblioteca, uma interface gráfica foi desenvolvida, a qual compreende o programa de controle do equipamento e também funções para tratamento e visualização de dados, como a transformada inversa de Laplace e transformada de Fourier. / The objective of this project was the assembling and automatization of a low cost NMR spectrometer for the characterization of porous media. The study of porous media through NMR spectroscopy requires a low intensity magnetic field in order to avoid the problems related to the difference of magnetic susceptibility on the fluid-solid interface. For that reason, a low field electromagnet, operating on the proton frequency of 2MHz (0.047 Tesla) and of simple design was built. As to keep all the equipment as low cost as possible, the following components were also assembled in laboratory: the magnets power supply, a 2MHz amplifier, the quarter-wave components and the necessary softwares. The goal of the software developed was to control the RF generation and acquisition board, which was acquired from the enterprise Spincore, further named RadioProcessor. To achieve this goal, it was decided the development of a new API, in the C++ language, which uses the original boards API as a base in order to assemble a group of functions that are simpler and more intuitive to the end user. In addition, a script language was integrated to the APIs library, allowing users with little programming knowledge to write a program which controls the whole equipment in an easy way and also adding flexibility to the software, as it becomes easy to add new functions. This permits that the equipment be easily changed to include other applications in the future. Finally, a graphical interface was developed, which comprehends the equipment control software and the visualization of the data.

Thesis (MScEng (Electrical and Electronic Engineering))--University of Stellenbosch, 2010. / ENGLISH ABSTRACT: Assessing the quality of fruit has become vitally important for farmers and growers. With retailers placing ever stricter requirements on fresh produce, growers have to spend a greater amount of time and effort sorting and grading their harvest. Increasingly, vendors are placing requirements not only on external factors like colour, and firmness, but on internal quality factors such as sugar content and acidity, because, although consumers buy fruit based on their external appearances, the taste of the fruit is what determines whether the consumer will buy again. Different techniques exist that probe the internal quality of fruit non-destructively. The technique most widely used today is Near Infrared Spectroscopy. This technique is powerful, but has certain limitations such as poor reliability and the need for constant recalibration. This thesis suggests an alternative method for evaluating internal fruit quality based on low-field nuclear magnetic resonance detected by superconducting quantum interference devices. It introduces the theory of SQUIDs and NMR, and evaluates the use of SQUID detected NMR spectroscopy as a method for determining the internal quality of fruit. The fabrication techniques and processes are explained in detail and a design for a SQUID detected NMR spectrometer is given. Relevant simulations and simulation results are also given. No working SQUID could be fabricated and, as such, no working NMR spectrometer was demonstrated. This thesis serves as a reference work for future research. / AFRIKAANSE OPSOMMING: Bepaling van die gehalte van vrugte het vir boere uiters belangrik geword. Met kleinhandelaars wat al strenger vereistes plaas op vars produkte moet boere meer tyd en inspanning bestee met die sortering en gradering van hul oes. Handelaars plaas nie net vereistes op eksterne kwaliteitsfaktore soos kleur en fermheid nie, maar begin al hoe strenger vereistes plaas op interne kwaliteitsfaktore soos suikerinhoud en suurgehalte, want, hoewel verbruikers vrugte koop op grond van hul eksterne kwaliteitsfaktore, is dit die smaak van die vrug wat bepaal of die verbruiker weer die vrug sal koop. Verskillende tegnieke bestaan wat die interne kwaliteit van vrugte op ’n nie-destruktiewe manier kan bepaal. Die mees algemene tegniek is Naby Infrarooi Spektroskopie. Hierdie tegniek is kragtig maar het sekere beperkings soos swak betroubaarheid en die noodsaaklikheid van konstante herkalibrasie. Hierdie tesis stel ’n alternatiewe metode vir die evaluering van interne vrugkwaliteit gebaseer op lae-veld kernmagnetiese resonans waargeneem deur supergeleidende kwantum inmenging toestelle voor. Dit stel die teorie van SKWITs en KMR bekend, en evalueer die gebruik van SKWIT-bespeurde KMR spektroskopie as ’n metode vir die bepaling van die interne kwaliteit van vrugte. Die fabrikasie tegnieke en prosesse word in detail verduidelik en ’n ontwerp vir ’n SWKIT opgevangde KMR spektrometer word gegee. Toepaslike simulasies en simulasie resultate word ook gegee. Geen werkende SKWIT kon vervaardig word nie en as gevolg daarvan kon geen werkende KMR spektrometer gedemonstreer word nie. Hierdie tesis dien as ’n naslaan werk vir toekomstige navorsing.

L'objectif de ces travaux a été de démontrer l'intérêt d'appliquer la Résonance Magnétique Nucléaire (RMN) à des problématiques analytiques dans le domaine des produits de santé. Deux axes principaux ont été abordés. Le premier cible principalement les compléments alimentaires adultérés. Les études ont été menées par RMN à haut champ. Diverses expériences de RMN mono et bidimensionnelles ont permis de mettre en évidence la présence illicite, dans des compléments alimentaires déclarés comme naturels, de médicaments à visée érectile et/ou de leurs analogues structuraux. Ces substances actives peuvent induire, à l'insu du consommateur, des risques importants pour sa santé. De plus, des analyses menées par RMN 1H et 13C ont permis de révéler des cas d'adultération de compléments alimentaires pour sportifs par des substances considérées comme dopantes par la règlementation en vigueur. Le second axe a été mené en explorant les potentialités de la RMN à bas champ pour l'analyse de médicaments. Cette technique, moins onéreuse et plus adaptée à des analyses de routine que la RMN à haut champ, s'est avérée très efficace pour mettre en évidence des cas de médicaments falsifiés par de simples expériences RMN 1H monodimensionnelles. Des expériences bidimensionnelles de diffusion (DOSY : Diffusion Ordered SpectroscopY), qui permettent d'obtenir la séparation virtuelle des constituants d'un mélange complexe, ont été mises au point et appliquées, pour la première fois, à la dé-formulation d'un médicament. / The purpose of this research was to demonstrate the interest of Nuclear Magnetic Resonance (NMR) to deal with analytical issues in the field of health products. The studies focused on two main axes. The first one targeted adulterated dietary supplements and the studies were conducted with high-field NMR. Various mono and bidimensional experiments revealed the illegal presence in dietary supplements claimed as natural, of erectile drugs and/or their structural analogues. These active substances can induce, without the consumer's knowledge, significant risks to his health. Moreover, analyses conducted with 1H and 13C NMR, highlighted cases of adulteration of dietary supplements for exercise and athletic performance with doping substances. The second axis explored the potential of low-field NMR for drug analysis. This technique, which is less expensive and more suitable for routine analyses than high-field NMR, has proved very effective in detecting cases of falsified medicines by simple one-dimensional 1H NMR experiments. Two-dimensional diffusion experiments (DOSY: Diffusion Ordered Spectroscopy), which provide virtual separation of the constituents of a complex mixture, were developed and applied for the first time to the de-formulation of a drug.

L’un des objectifs du programme de recherche Opticook est d’équiper les fours avec des capteurs spectroscopiques qui permettront de piloter de façon non intrusive la cuisson de viande et de poisson. Le développement de ces capteurs est basé sur l’hypothèse que les protéines de ces aliments sont de bons marqueurs du degré de cuisson. Dans ce contexte, dans un premier temps, plusieurs outils ont été mis en œuvre pour caractériser l’effet de différents barèmes de cuisson sur les propriétés macroscopiques (texture, couleur) d’échantillons de bœuf, de poulet et de dos de cabillaud. Puis, pour étudier les transformations que subissent ces échantillons à l’échelle moléculaire, nous avons utilisé la calorimétrie et différentes spectroscopies. La spectroscopie dans le domaine du visible nous a permis d’observer la dénaturation des hémoprotéines grâce à l’évolution de l’état (oxy à met ). Ces protéines sont responsables du changement de couleur observé entre 50 et 75 °C. Les spectroscopies dans le moyen infrarouge et de fluorescence ont été utilisées pour suivre les changements de structures associées à la dénaturation des protéines fibrillaires. La myosine, purifiée à partir du blanc de poulet, a été étudiée en fonction de la température par fluorescence. Les résultats nous ont montré que des évolutions de la structure protéique se produisent dès 50 °C. À l’échelle microscopique, nous avons réalisé des expériences sur des échantillons de bœuf par RMN bas champ (séquences d’impulsion et gradient de champ), et par tomographie de neutrons pour rendre compte de la contraction des fibres et de la libération du jus selon le degré de cuisson. L’analyse des images 3D enregistrées par tomographie de neutrons et le traitement des données de RMN montrent des changements importants de la morphologie et de la densité de fibres des échantillons après la cuisson à haute température. Pour associer les deux approches (moléculaire et microscopique) des mesures couplées de spectroscopie et d’imagerie de neutrons ont été menées dans le four Opticook pendant la cuisson de tranches de bœuf. Ce couplage nous a permis de suivre l’évolution de la morphologie due à la contraction des fibres, la migration du jus, ainsi que le changement de couleur associé à la dénaturation des hémoprotéines. Nous en concluons qu’il est en effet possible de suivre le degré de cuisson de viande et de poisson à l’aide de différentes spectroscopies (la fluorescence et le visible) grâce aux signatures spectroscopiques de plusieurs marqueurs internes à ces matrices : la myosine, le collagène et les hémoprotéines. / One of the purposes of the Opticook project is to install spectroscopic sensors in ovens, so equipping them with non intrusive tools allowing following cooking process of meat and fish. The hypothesis on which sensors were developed was: are muscular proteins proper probes to discriminate among several cooking degrees? Thus, at the beginning of the project several tools were used to characterise effect of several cooking degrees on macroscopic properties (texture and colour) of beef, chicken and cod fillet samples. Following, calorimetry and spectroscopic techniques were used to study transformations at molecular scale. In particular, visible spectroscopy followed denaturation of haemproteins observing their evolution from oxy to met state. Colour change was observed between 50 and 75 °C. Middle infrared and fluorescence spectroscopies were used to observe evolution of fibrillar proteins which are associated with meat texture changes. One of myofibrils, myosin, was purified from chicken breast and was studied depending on temperature by fluorescence spectroscopy. Observations showed evolution of protein structure occurred around 50 °C. At microscopic scale, low field NMR (spin echo and gradient field configurations) and neutron tomography were used to observe morphology changes and juice release on beef samples according to cooking degree. 3D image analysis and NMR data showed morphology and fibre density changes at high temperature.We associated the two approaches (molecular and microscopic) in the last part of the research. So coupled measures were realised by combining neutron imaging and spectroscopy techniques during cooking process on beef slices by Opticook oven. Coupled measures allowed following morphology evolution because of fibre contractions, juice migration and colour modification as well associated to haemprotein denaturation. In conclusion, it is possible to follow cooking process of meat and fish by following several spectroscopic signatures (fluorescence and visible ones) of matrix own probes: myosin, collage and haemproteins.