Application of specific deuterium labeling and nuclear magnetic resonance spectroscopy to the study of the mechanism of pyrolysis of tert-butylarsine and tert-butylarsine-d sub 2
- Univ. of Minnesota, Minneapolis (USA)
The synthesis of tert-butylarsine-d{sub 2} from tert-butylarsenic dichloride and LiAlD{sub 4} is described. No resonances at 2.65 ppm (from AsH{sub 2}) are observed in the {sup 1}H NMR spectrum, indicating the isotopic purity is greater than 95%. The pyrolyses of tert-butylarsine and tert-butylarsine-d{sub 2} were studied by using a flow reactor operated between 425 and 550{degree}C at total pressures of 0.001, 5, and 700 Torr. At 5 and 700 Torr, nitrogen was used as the carrier gas. The volatile products of the reaction were trapped in a liquid nitrogen cooled trap, transferred under vacuum into an NMR tube, and quantitatively analyzed by using {sup 1}H NMR spectroscopy. Three important results from the study are (1) the isobutane produced during the pyrolysis of tert-butylarsine-d{sub 2} was Me{sub 3}CD, (2) C{sub 2}Me{sub 6} was proven not to be a product of the reaction, (3) isobutane was found to be the major product at atmospheric pressure, while isobutene was predominant at low pressures in agreement with previous studies.
- OSTI ID:
- 5410753
- Journal Information:
- Chemistry of Materials; (United States), Journal Name: Chemistry of Materials; (United States) Vol. 2:5; ISSN CMATE; ISSN 0897-4756
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
360601* -- Other Materials-- Preparation & Manufacture
656002 -- Condensed Matter Physics-- General Techniques in Condensed Matter-- (1987-)
75 CONDENSED MATTER PHYSICS
SUPERCONDUCTIVITY AND SUPERFLUIDITY
ARSENIC COMPOUNDS
ARSENIDES
CHEMICAL PREPARATION
CHEMICAL REACTIONS
DECOMPOSITION
EPITAXY
GALLIUM ARSENIDES
GALLIUM COMPOUNDS
LABELLED COMPOUNDS
MAGNETIC RESONANCE
MATERIALS
MEASURING INSTRUMENTS
MEASURING METHODS
NUCLEAR MAGNETIC RESONANCE
ORGANIC ARSENIC COMPOUNDS
ORGANIC COMPOUNDS
PNICTIDES
PYROLYSIS
RESONANCE
SEMICONDUCTOR MATERIALS
SYNTHESIS
THERMOCHEMICAL PROCESSES
VAPOR PHASE EPITAXY