A homoger~eous poly~~ronide hemicellulose has beer1 prepared fro111 a crude hemicellulose isolated from wheat straw holocellulose by hot water. The method of preparation consisted of fractional precipitation of the acetylated hemicellulose from chloroforn~ solution by petroleum ether. Approximately 50% of the recovered fractiorls consisted of a polysaccharide made up of 28 moles of D-xylose, 5 moles of L-arabirlose, and 3 moles of uror~ic acid and having an [a]ho = -92" and a molar ratio, methoxyl: uronic anhydride, of approxinlately 1.0. Intrillsic viscosity measurements indicated a degree of polymerization of approximately 30. Separation of hexosans present in the original hemiccllulose showed that they were not chen~ically combined with the main pentosan fraction. They were recovered admixed with short chain pcntosan material containing a higher proportion of arabinose to xylose than the main homogeneous fraction.