1. (1) A very sensitive method has been presented for the determination of 0.01-0.5 [mu]moles of methylpentose.2. (2) Many compounds which give rise to acetaldehyde on oxidation with periodate can be determined by this procedure.3. (3) There is very little interference in this procedure from other aldehydes released on oxidation of sugars with periodate.4. (4) Free methylpentose can be detected in the presence of the glycosidically bound sugar.5. (5) The method has been used to determine the stability of fucose to hydrolysis and the lability of the fucosyl-glycosidic bond in furanosides, pyranosides, and a number of fucose-containig oligosaccharides and glycoproteins.Peer Reviewedhttp://deepblue.lib.umich.edu/bitstream/2027.42/33487/1/0000892.pd