Abstract
An intercalated graphite was prepared by reaction of polycrystalline graphite with AsF 5 followed by reaction with NO 2SbF 6. At −73%, four narrow lines are found in the 19F n.m.r. spectrum at +124.1, +112.7, +66.7, and +46.8 ppm (relative to CFCl 3). These lines are attributed to SbF 6 − , SbF 5, AsF 6 − in rapid chemical exchange with AsF 5, and AsF 3, respectively. This demonstrates the use of n.m.r. for the qualitative analysis of the chemical species present in the interlamellar space. As the temperature is increased, the lines broaden (except for that of AsF 3) and subsequently narrow, indicating, further, that chemical exchange of fluorine is occurring among SbF 6 − , SbF 5, AsF 6 − and AsF 5. At 22 °C the exchange rate is ∼ 10 3 s −1 for SbF 6 − and >3 × 10 3 s −1 for the other species. The data are interpreted in terms of a model in which fluorine exchange between SbF 6 − and the fluoro-arsenic species occurs via SbF 5.
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