CARBON AND DEUTERIUM NUCLEAR MAGNETIC RESONANCE IN SOLIDS

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In Chapter I we present the results on a study of cross polarization dynamics, between protons and carbon-13 in adamantane, by the direct observation of the dilute, carbon-13, spins. These dynamics are an important consideration in the efficiency of proton enhancement double-resonance techniques and they also provide good experimental models for statistical theories of cross relaxation. In order to test these theories we present a comparison of the experimental and theoretical proton dipolar fluctuation correlation time {tau}{sub c}, which is experimentally 110 {+-} 15 {micro}sec and theoretically 122 {micro}sec for adamantane. These double resonance considerations provide the background for extensions ... continued below

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347 p.

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Shattuck, Thomas Wayne July 1, 1976.

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In Chapter I we present the results on a study of cross polarization dynamics, between protons and carbon-13 in adamantane, by the direct observation of the dilute, carbon-13, spins. These dynamics are an important consideration in the efficiency of proton enhancement double-resonance techniques and they also provide good experimental models for statistical theories of cross relaxation. In order to test these theories we present a comparison of the experimental and theoretical proton dipolar fluctuation correlation time {tau}{sub c}, which is experimentally 110 {+-} 15 {micro}sec and theoretically 122 {micro}sec for adamantane. These double resonance considerations provide the background for extensions to deuterium and double quantum effects discussed in Chapter II. In Chapter II an approach to high resolution nmr of deuterium in solids is described. The m = 1 {yields} -1 transition is excited by a double quantum process and the decay of coherence Q({tau}) is monitored. Fourier transformation yields a deuterium spectrum devoid of quadrupole splittings and broadening. If the deuterium nuclei are dilute and the protons are spin decoupled, the double-quantum spectrum is a high resolution one and yields information on the deuterium chemical shifts {Delta}{omega}. The relationship Q({tau}) {approx} cos 2{Delta}{omega}{tau} is checked and the technique is applied to a single crystal of oxalic acid dihydrate enriched to {approx} 10% in deuterium. The carboxyl and the water deuterium shifts are indeed resolved and the anisotropy of the carboxyl shielding tensor is estimated to be {Delta}{sigma} = 32 {+-} 3 ppm. A complete theoretical analysis is presented. The extension of cross relaxation techniques, both direct and indirect, to proton-deuterium double resonance is also described. The m = 1 {yields} -1 double quantum transition and the m = {+-} 1 {yields} 0 single quantum transitions may all be polarized and we present the derivation of the Hartmann-Hahn cross polarization conditions for each case. In addition the dynamics of the double quantum process, for monodeutero benzene are discussed, giving proton dipolar fluctuation correlation times, and spin heat capacities for the double quantum transition.

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347 p.

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  • Related Information: Designation of Academic Dissertation: Masters; Academic Degree: M.S.; Name of Academic Institution: UC Berkeley

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  • Report No.: LBL-5458
  • Grant Number: DE-AC02-05CH11231
  • Office of Scientific & Technical Information Report Number: 937066
  • Archival Resource Key: ark:/67531/metadc901165

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  • July 1, 1976

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  • Sept. 27, 2016, 1:39 a.m.

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  • Sept. 30, 2016, 7:21 p.m.

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Shattuck, Thomas Wayne. CARBON AND DEUTERIUM NUCLEAR MAGNETIC RESONANCE IN SOLIDS, thesis or dissertation, July 1, 1976; Berkeley, California. (digital.library.unt.edu/ark:/67531/metadc901165/: accessed November 20, 2018), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.