In accordance with the rising amount of vegetable biomass waste, scientists and experts from different branches of industry have noticed the potential for agro-industrial waste utilization and its use as a secondary raw material. The aim of this study was the extraction of xylan from walnut shell, as well as its characterization in order to examine its potential for further utilization. For this purpose, the effect of previous delignification (2 h and 4 h), time and alkaline concentration (2 M and 4 M) was observed during alkaline extraction. Three fractions were isolated using different extraction conditions (the soluble and the insoluble hemicellulose and the cellulose residue) in which it was determined monomeric composition using high performance liquid chromatography (HPLC) with previous PMP derivatization. Almost 53 % of the dry matter of the raw material (walnut shell) is composed of structural polysaccharides, whose composition is dominated by xylose and glucose (total glucan and total xylan). The share of xylan in walnut shell is 19,9 %, which is around 38 % of the carbohydrate portion of structural polysaccharides. The utilization of xylan in the soluble and the insoluble hemicellulose fraction expressed as % of the initially present xylan in the raw material is approximately 100 % in all samples. Previous delignification of the samples improved the xylan extraction, while alkaline concentration and duration of alkaline extraction did not have a significant effect on xylan extraction. Walnut shell is a good source of xylan, which is mostly separated in a soluble hemicellulose fraction.