Development and applications of a low-field portable NMR system : a thesis presented in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Physics at Massey University, Manawatu, New Zealand
Open Access Location
Nuclear magnetic resonance (NMR) is a phenomenon similar to MRI in which radio frequency signals are used to excite and manipulate atomic nuclei within a static magnetic field. Following excitation, the nuclei return to equilibrium, all the while offering valuable molecular level information pertaining to the sample. Within the last decade, the development of small and inexpensive NMR spectrometers and permanent magnet NMR sensors has been a significant focus within the NMR community. More recently, application scientists have sought practical applications for the new technologies. In this thesis, a prototype NMR apparatus consisting of a spectrometer and 3.2MHz permanent magnet sensor was extended to enable scientifc measurements. This involved developing radio frequency electronic circuitry for the spectrometer front-end, and electromagnetic noise shielding and temperature regulation for the magnetic sensor. Experimental results confirmed that repeatable measurements using the modified apparatus were indeed possible. The NMR apparatus was thereafter successfully used to study flow, diffusion and kiwifruit using several different experimental techniques. A significantly larger effort was then expended upon the study of T2 relaxation in pectin model systems using pH as the adjustable parameter. The fascinating experimental results were successfully interpreted and modeled across three pH zones in terms of a proton chemical exchange model and molecular conformational changes. In addition, it was found that pectin carboxyl de-protonation was significantly less than expected. Further experiments performed upon galacturonic acid monomers, dimers and trimers appeared to further illuminate the pectin results. Future experiments are planned. Also while studying pectin solutions, an unexpected pH-dependent water transverse relaxation behavior was observed at both 3.2MHz and 400MHz. The only references found in the literature were from a small publication almost 50 years ago, and a 2011 publication. Altogether, this thesis contributed to original knowledge in several ways: it showed how a low- eld apparatus and single-sided sensor could be improved and utilized for a variety of scientific measurements; it showed both experimentally and theoretically how T2 for pectin solutions change with pH; it revealed an unexpected de-protonation limit for pectin molecules; it revealed a T2 pH dependence for water.
Nuclear magnetic resonance spectroscopy, Magnetic spectrometer, NMR, Diffusion, Dimer, Galacturonic acid, Heptamer, Kiwifruit, Mole probe, Momomer, Nuclear magnetic resonance, Octamer, Pectin, Polysaccharides, Pre-amp duplexer, Radio frequency, Sensors, Signal processing, Spectrometer, Titration, Trimer, pH