Abstract The composition of the hemicellulose fractions of wholemeal and flours of about 70% extraction in terms of anhydro‐arabinose, xylose and uronic acid units has been investigated. It has been shown that the hemicelluloses, on distillation with hydrochloric acid, behave in the same manner as an equimolecular mixture of arabinose and xylose. Xylose is a suitable standard for the distillation process, and the ‘xylose equivalent’ of a wheat fraction multiplied by 0.97 is a quantitative measure of the hemicellulose present, provided this is not less than 1.8%.