We investigated the degradation of sugars during acid hydrolysis and the effects of other aspects of sample preparation on measurement of wood sugars by anion exchange HPLC using pulsed amperometric detection. Loss of sugars in standards ranged from 6.4% for arabinose to 15.7% for mannose. Measurements of wood samples to which standard was added before hydrolysis were very close to the sum of wood samples and standards hydrolyzed and analyzed separately except in the case of galactose, which was in significantly lower amounts (4.7% lower) in the combined samples. There was greater variance among injections of individual replicates than among replicates. Other, minor procedural details were investigated.