Abstract: | Terpolymers formed from styrene, α‐methylstyrene (AMS), and acrylonitrile (AN) were prepared in different proportions. According to the reaction conditions, the terpolymers presented random sequence distributions. AMS, because of steric hindrance, presented a high degree of instability, which promoted depolymerization. AN promoted a long insertion of AMS monomers, which caused an acceleration of the propagation reaction. This also caused a depolymerization process. With 13C‐NMR solution analysis, it was possible to detect the depolymerization process. With solid‐state NMR results, it was demonstrated that AMS constituted the highest mobility domain. Finally, the values determined for the proton spin–lattice relaxation time in the rotating frame confirmed that the prepared terpolymers were random, but a homogeneous monomer distribution sequence was also observed from this parameter. © 2003 Wley Periodicals, Inc. J Appl Polym Sci 88: 1004–1009, 2003 |