The alkali extract (5% KOH) from beech holocellulose was fractionated by ion exchange chromatography, resulting in several fractions containing different amounts of polyoses and lignin. The separated polyoses varied to some extent in the ratios of their sugar components. Three different 4-0-methylglucurono-xylans and three arabinogalactans were isolated. There was a direct relationship between the chemical composition and the ultrastructure of the fractions. Those containing a pure 4-0-methylglucurono-xylan showed bundles of thin and stiff fibrils while in fractions with a high percentage of lignin coiled fibrils and globular particles could be observed in the electron microscope.