Linear fluoral oligomers initiated with tert-butoxide or bornyl oxide and acetate end-capped were analyzed by potassium ionization of desorbed species (K+IDS) combined with gas chromatography (GC). Using K+IDS it was possible to identify fluoral diacetate and the oligomers up to the undecamer. tert-Butoxide initiated oligomers showed masses from the unimers of 253 daltons up to the mass of 1233 daltons, the undecamer. The individual lower oligomers were also identified by GC. Bornyl oxide terminated, acetate capped fluoral oligomers were also analyzed and characterized to masses up to 1215 daltons, the decamer, by K+IDS; GC characterization was also carried out.