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The effect of heating cycles of polyether ether ketone up to 420 °C on the thermophysical properties was studied by the method of differential-scanning calorimetry. It is shown that with each subsequent heating the glass transition temperature increases, while the melting and crystallization temperature decreases, which may indicate an increase in the molecular weight of the polymer due to the structuring processes. The main degradation products of polyether ether ketone in air at temperatures of 350-450 °C were determined by gas chromatography and thermal decomposition schemes were proposed.