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Pure quadrupole resonance of /sup 17/O compounds by proton double resonance

Thesis/Dissertation ·
OSTI ID:5960592
/sup 17/O pure quadruple resonance spectra were observed in ice, O/sub 3/, H/sub 2/O/sub 2/, IrClCO(PPh/sub 3/)/sub 2//sup 17/O/sub 2/ (Vaska's Compound) and the bromine analog of the latter. Double resonance between /sup 17/O and /sup 1/H in zero applied field was used as described by Slusher and Hahn except that the ice and O/sub 3/ samples did not require modulation of the resonant RF. Observed resonances were: ice 1.70(5), 3.40(5); O/sub 3/ 5.50(3), 11.23(8); H/sub 2/O/sub 2/ 3.475(20), 4.554(20), 8.05(5); and IrClCo(PPh/sub 3/)/sub 2/O/sub 2/ first site 3.50(3), 4.70(3), 8.20(7) second site 3.89(3), 4.20(3), 8.10(7). (Frequencies in MHz with last place uncertainty in parentheses) The lower four frequencies of the bromine analog were the same as the chlorine frequencies. The following electric field gradients result: ice 6.42(10), > 0.93; O/sub 3/ 21.5(4), 0.95(3); H/sub 2/O/sub 2/ 16.31(7), 0.687(11); and for Vaska's Compound first site 16.76(5), 0.658(17) second site 15.65(7), 0.907(17). (Coupling constants in MHz followed by asymmetry). Besides the fact that its quadrupole spectrum was unknown the ozone experiment is novel in two ways. First, double resonance was performed on a compound having no second spin. This was achieved by dissolving the ozone in a proton solvent, chloroform. This may be of general use for spinless, volatile, explosive or toxic samples. Second ozone was synthesized in a low pressure discharge at 77/sup 0/K where the ozone vapor pressure is very low. Chemical analysis shows this makes the synthesis at least 80% efficient. It may be much better. This is important because of the high cost of the isotope.
Research Organization:
California Univ., San Diego (USA)
OSTI ID:
5960592
Country of Publication:
United States
Language:
English

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Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400104 -- Spectral Procedures-- (-1987)
400201* -- Chemical & Physicochemical Properties
ABSORPTION SPECTROSCOPY
BROMIDES
BROMINE COMPOUNDS
CHEMICAL PREPARATION
CHLORIDES
CHLORINE COMPOUNDS
COMPLEXES
DOUBLE RESONANCE METHODS
EVEN-ODD NUCLEI
HALIDES
HALOGEN COMPOUNDS
HYDROGEN COMPOUNDS
HYDROGEN PEROXIDE
IRIDIUM CHLORIDES
IRIDIUM COMPLEXES
IRIDIUM COMPOUNDS
ISOTOPES
LIGHT NUCLEI
LOW TEMPERATURE
NUCLEAR QUADRUPOLE RESONANCE
NUCLEI
ORGANIC COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
ORGANIC PHOSPHORUS COMPOUNDS
ORGANOMETALLIC COMPOUNDS
OXYGEN 17
OXYGEN COMPOUNDS
OXYGEN ISOTOPES
OZONE
PEROXIDES
RESONANCE
SPECTROSCOPY
STABLE ISOTOPES
SYNTHESIS
TEMPERATURE DEPENDENCE
TRANSITION ELEMENT COMPLEXES
TRANSITION ELEMENT COMPOUNDS