CO2, N2O, NO, NH3 and NO2 were found to be evolved from potassium cobalt hexacyanoferrate, K2CoFe(CN)(6) . 1.4H(2)O, when heated at temperatures between 240 and 360 degrees C in synthetic air, Determinations of the gases were carried out with an FTIR spectrometer. The amount of carbon dioxide released corresponded closely with the amount of carbon initially present in the sample, However, the total amount of nitrogen obtained in the nitrogen-containing gases was only 39% of the initial nitrogen. It is assumed that N,, which is undetectable by IR spectroscopy, was also released and made up the remaining 61% of the total nitrogen emission, Since the compound does not contain any hydrogen other than that in water, we assume that the hydrogen in the ammonia released originated from the water evaporated at lower temperatures and condensed on the tube walls between the pyrolysis oven and the detector gas cell.