The short chain branching distribution (SCBD) and thermal properties of ethylene/1-pentene copolymers were studied using SEC-FTIR and SEC-HPer DSC. The copolymers, synthesized with Cp2ZrCl2/MAO, were fractionated using size exclusion chromatography (SEC). The infrared analysis of the fractions showed that the copolymers had-on average-higher 1-pentene concentration in the low molecular weight range. Furthermore, the thermal properties of the SEC deposits of these copolymers on a Germanium disc were studied using high performance differential scanning calorimetry (HPer DSC. Single SEC separations were used to accumulate fractions in the microgram range that were directly analyzed with regard to their thermal properties, thus allowing us to study SCBD as well as thermal behavior simultaneously. When these fractions (with masses ranging from 10-80 mu g) were analyzed using HPer DSC, good melting and crystallization temperature distributions were obtained, proving that HPer DSC can be used as a complementary method to SEC-FTIR. (C) 2007 Wiley Periodicals, Inc.