A high performance liquid chromatography (HPLC) method has been developed for analysis of wood sugars in samples from the pulp and paper industry. Using a Bio-Rad HPX-87P carbohydrate analysis column, it is possible to separate the sugars using isocratic elution with distilled water. Glucose, mannose, and xylose in 100:1:1 ratio, occurring in a pulp hydrolyzate, can be separated in 20 min. Using two columns in series, a separation of free glucose, mannose, galactose, arabinose, and xylose, present in very unequal proportions in spent sulfite liquor, can be done in 60 min.