The competitive oxidation of 13CH3OH and 13CD3OH has been observed using in vivo 13C NMR spectroscopy. Simultaneous 1H and 2H decoupling gave isotopically shifted 13C singlets for the two methanol isotopomers. The measured enzymic isotope effect, kH/kD is approx. 1.8, indicating that CH bond cleavage is not rate-determining.