Amylose inclusion complexes are prepared by complexation of synthetic amylose having a covalently attached PTHF block (PTHF-b-amylose) with guest polytetrahydrofuran of molecular weights of 650 and 1000 g · mol−1 (PTHF650 and PTHF1000). Differential Scanning Calorimetry (DSC) analysis of the products shows a characteristic melting peak of the complexes at 140 °C. Compared to PTHF650, the PTHF1000 displays lower complexing ability with PTHF-b-amylose which is indicated by visible amylose retrogradation. The possible structures of the resulting products are estimated from Thermo Gravimetric Analysis (TGA) which reveals differences between PTHF-b-amylose and the corresponding complexes. In addition, X-Ray Diffraction (XRD) analysis demonstrate...