A process for preparing .alpha., .omega.-functional siloxane compounds in a purity of greater than or equal to 90% includes contacting a monohydrosiloxane compound of formula 1 ##STR00001## with oxygen in the presence of a platinum group catalyst, without adding water, to form the .alpha., .omega.-functional siloxane compound in a purity of greater than or equal to 90%; wherein n is 0, 1, or 2; R.sub.1 is fluoroethyl, methyl or phenyl; and R.sub.2 is substituted alkyl, epoxyalkyl, oxetanylalkyl, substituted oxaalkyl, epoxyoxaalkyl, oxetanyloxaalkyl, alkenyl, alkylalkoxysilyl, substituted alkylaryl, and substituted arylalkyl.