Measurement of the degree of crystallinity of the polymer matrix in a composite is complicated by the presence of the reinforcing additive. This is particularly the case in poly(ether ether ketone) carbon fibre composite, APC-2, which may contain as much as 70% carbon fibre. A First Law procedure, developed for determining the degree of crystallinity of poly(ether ether ketone) (PEEK), has been outlined previously. It involved direct measurement of the enthalpy changes associated with melting, crystallization and heat capacity changes, and was found to be an effective method for determining the crystallinity of the PEEK matrix. The procedure has been applied to carbon fibre and glass fibre PEEK composites.