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Theβ →γ transformation of Ca2SiO4 was investigated with regard to the disintegration of the sinter in alumina manufacturing. DTA was applied to study the effect of the reducing atmosphere upon the course of the polymorphic transitions of Ca2SiO4, and particularly the self-disintegration process. Pure synthetic dicalcium orthosilicate and blends of pure components from the system CaO-Al2O3-SiO2-Fe2O3 were compared with technological mixtures of limestone and fly ash. Data obtained from the DTA runs allowed the specification of technical parameter for both firing and cooling of the sinter.