Two-step etching procedures have been developed for binary polymer blends of linear low density polyethylene (LLDPE) with high density polyethylene (HDPE), and for blends of atactic and syndiotactic polystyrene. For both cases, two different etchants have been identified for the component neat polymers; sequential etching has been employed to reveal the distribution of the component polymers within the blend. It is believed that similar procedures may be applicable to other blend systems.