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The basic theories of Nuclear Quadrupole Resonance are outlined, together with some basic NMR theory and its application to double resonance techniques. An improved design of spectrometer using double resonance is presented, including a description of a new flow cryostat which can operate down to 4.2°K with low (250 cc/hour) consumption of liquid He. The whole apparatus may be used to detect NQR signals in solids over the frequency range 100 kHz-5 MHz. The theory of double resonance with spin mixing by continuous coupling (D R CC) is developed and illustrated by experiments performed on HCOOD, HDO and several nitrogen-containing compounds, including Imidazole. Further experiments were then carried out on samples dilute in deuterium, including the detection of NQR in formic acid (HCOOH) due to naturally abundant deuterium. Other experiments on proton-deuteron interactions in amide groups and in water molecules are also described and compared with results previously published on fully-deuterated amides and D₂0 as a water of crystallisation in L-serine hydrate. The NQR spectrum of Lanthanum Nicotinate Dihydrate is obtained using F.M. techniques and related to its structure. The theory of Zeeman NQR in spin 3/2 nuclei is developed with reference to the double resonance technique, and the measured quadrupole coupling constants of ²³Na and ²D in NaOH and some of its hydrates are discussed. Finally, some standard theories concerning proton relaxation times in solids at low temperatures (4°K-300°K) are outlined and related to some, measured relaxation times, illustrating their significance to the double resonance technique. The concluding chapter outlines a speculative proposal for a new spectrometer design.

This thesis discusses in general terms the theory and application of time-differential perturbed angular correlation gamma-ray spectroscopy (TDPAC) to the study of solid state physics. The technique yields valuable information on the electric field gradients experienced by radionuclides which have been substituted for nonradioactive isotopes or inserted as impurities into various inorganic compounds. The indium halides are examined in a series of experiments. The first applications of this technique to the study of graphite intercalation compounds are discussed. / Science, Faculty of / Physics and Astronomy, Department of / Graduate

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Electrostatic interactions such as halogen bonding and pnictogen bonding interactions have gained a lot of interest in the field of crystal engineering and pharmaceutical science. In the first part of this thesis, we expand our knowledge on anion coordinated halogen bonded cocrystals by looking at a series of cocrystals made from 3-iodoethynyl pyridine and 3-iodoethynylbenzoic acid. We utilize the power of mechanochemistry to create the new cocrystals made with phosphonium salts and use multinuclear solid-state nuclear magnetic resonance spectroscopy and X-ray diffraction and characterize them. We found that mechanochemistry is a fast and powerful tool to explore and synthesize new halogen bonded cocrystals and ³¹P solid-state NMR is a rapid way to identify the formation of a cocrystal. In the second part, we look at the versatility of the pnictogen atom, specifically antimony, as a pnictogen bond donor and a halogen bond acceptor. We evaluate these electrostatic interactions with nuclear quadrupolar resonance and found that nuclear quadrupole resonance is a strong spectroscopy tool to probe these types of electrostatic interactions.

Land mines are a major humanitarian problem with millions of active mines in place around the world. Since these mines can have little metal in them, novel detection techniques are needed. Nuclear Quadrupole Resonance (NQR) is one such technique. Unfortunately, NQR is highly succeptible to radio frequency interference (RFI). A significant contribution of this thesis is the development of a custom, experimental data acquisition system designed and built specifically for capturing RFI at frequencies significant to NQR land mine detection systems. Another major contribution is the development of data analysis techniques for determining the number of reference antennas required to effectively cancel out RFI at frequencies and in environments typical of an NQR land mine detection system.

La Résonance Quadrupolaire Nucléaire (RQN) est une technique spectroscopique appliquée à l’état solide et qui ne nécessite aucun champ magnétique statique contrairement à la Résonance Magnétique Nucléaire (RMN). Elle permet de détecter, les molécules qui contiennent un noyau quadrupolaire (tel que l'azote-14). La RQN de l’azote-14 suscite un intérêt particulier car elle s'avère utile dans la détection de drogues et d’explosifs, qui contiennent, pour la plupart, des molécules azotées. Cette thèse porte en premier lieu sur l’amélioration de la qualité spectrale en résonance quadrupolaire (RQN) de l’azote-14. Ainsi, nous nous sommes préoccupés des signaux transitoires (ringing) qui suivent l’impulsion radiofréquence (rf) et qui masquent en partie le signal RQN. Nous avons d’abord montré, par une étude théorique et expérimentale, que les mesures à basse puissance (< 3Watts) étaient possibles, ce qui nous a permis de diminuer l’amplitude du ringing. De plus, grâce à ce mode de fonctionnement (basse puissance), nous avons pu proposer un circuit original de commutation du facteur de qualité (Q-switch) basé sur un commutateur rf CMOS et qui a permis de diminuer la durée du ringing. La seconde partie traite de l’influence d’un champ magnétique statique faible amplitude et des divers paramètres expérimentaux en RQN de l’azote-14. Dans le cas où le tenseur de gradient de champ électrique est de symétrie axiale, nous avons observé des élargissements, voire des doublets Zeeman. En revanche, dans le cas général (absence de symetrie), nous avons mis en évidence la possibilité définir le tenseur de gradient de champ électrique à partir de la forme de raie d’une seule transition au lieu de deux transitions (sans champ magnétique statique). Ce dernier résultat pourrait permettre de diminuer de moitié le temps nécessaire à la caractérisation d’une nouvelle molécule azotée. / Nuclear quadrupole resonance (NQR) is a solid-state spectroscopic technique which doesn't require a static magnetic field in contrast to Nuclear Magnetic Resonance (NMR). It is used to detect molecules containing quadrupole nuclei (such as nitrogen-14). Nitrogen-14 quadrupole resonance is of particular interest because it is useful in the detection of drugs and explosives, which contain mostly of nitrogen molecules. In this thesis we have primarily focused on improving the spectral quality in nitrogen-14 quadrupole resonance (NQR) . Thus, we were concerned with the transient signals ( ringing ) following the radiofrequency (rf) pulse and which partly overwhelm the NQR signal. First, we demonstrated by theoretical and experimental study that low power measurements (< 3Watts ) were possible, allowing us to reduce the ringing amplitude. In addition, through this mode ( low power ), we have proposed an original quality factor switching circuit (Q -switch ) based on rf CMOS switch and which has reduced the ringing duration. The second part deals with the effect of a weak static magnetic field and various experimental parameters in nitrogen-14 quadrupole resonance. In the case of an axially symmetric electric field gradient tensor, we observed broadening or Zeeman doublets. By contrast, in the general case (no symmetry), we demonstrated the possibility to define the electric field gradient tensor from the line shape of a single transition instead of two transitions ( without static magnetic field ). This result reduces by half the time required for the characterization of a new nitrogen molecule.

The thesis deals with the NQR spectroscopy, which is one of the modern non-destructive measurement and diagnostic methods for the characterization of various materials. It is using a quadrupole moment - a property of atomic nuclei of certain isotopes. A method of nuclear quadrupole resonance (NQR) is in principle very similar to nuclear magnetic resonance (NMR). Thesis in the theoretical part analyse the principles of NMR and NQR, describes the possible use of this method to detect for example explosives, drugs, and other chemicals. In the following chapters are analysed the key parameters of NQR spectrometer and the principle of the chosen measurement method. The practical part deals with the individual components of NQR spectrometer, the design of possible improvements and programming of the measuring sequence. In the final chapter are processed the measurements of the submitted samples.

Nuclear quadropole spectroscopy is a modern analytical method for detecting specific solid state materials, e.g. explosives, drugs etc. It uses phenomenon of atomic nucleus called nuclear quadrupole moment. NQR method is very similar to common nuclear magnetic resonance (NMR) that is why major principles are explained using NMR. The thesis deals with basic principle of NQR, its usage for explosives detection and also detection of other chemical compounds and many other useful applications. The thesis deals with specific circuit design, techniques for sufficient sensitivity, impedance matching and circuit isolation. Practical part consists of simulations as well as designs of a few impedance transformers, pi-networks, and coils. Also experimental probe was created. In the last part, NQR workplace was assembled and a few chemical compounds were detected. These were KClO3, NaClO3 and NaNO2 . Finally minimum detectable amount of potassium chlorate as the strongest signal of these was determined.