Polymer blends were prepared to obtain a new material with specific characteristics. To prepare a miscible polymer blend, it is necessary to evaluate the chemical structure and molecular dynamics of all polymers involved and to thereby establish a structure-property relationship for these materials. In this work, ternary blends for application in plates chromatography were formed with styrene/ butadiene/acrylinotrile (ABS), poly(vinyl chloride) (PVC), and gypsum, and were studied by solid-state carbon-13 nuclear magnetic resonance ( 13 C NMR). Magic-angle spinning (MAS), cross-polarization magic-angle spinning (CP-MAS), variable contact time (VCT), and proton spin-lattice relation time in the rotating frame (T 1 H ) were the techniques used to evaluate the miscibility, homogeneity, and compatibility of polymer blends at the molecular level. From the values of T 1 H , it was verified that ABS/PVC/gypsum formed good polymer blends with some specific physical interaction at the molecular level.