In order to determine volatile fatty acids (short chain monocarboxylic acids with 2 to 6 carbon atoms in a molecule) in leachates formed in organic waste piles a procedure based on static headspace (HS) coupled with gas chromatography (GC) have been proposed and optimized. The conditions of HS extraction and sample introduction into a gas chromatograph as well as of chromatographic separation were considered. Using flame ionization detection LODs were of the order of 0.02-0.37 mg/L. The analyzed leachate collecting on and close to a zoo organic waste pile contained VFAs (Volatile Fatty Acids) at a concentration ranging from 5.5 mg/L to 0.88 g/L and from below LOD to 10.1 mg/L for pool water at some distance from the pile, respectively.