Multidimensional analysis of the complex composition of impact polypropylene copolymers: Combination of TREF, SEC-FTIR-HPer DSC, and high temperature 2D-LC

  • Cheruthazhekatt S
  • Pijpers T
  • Harding G
 et al. 
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Abstract

A new multidimensional fractionation technique, temp. rising elution fractionation (TREF) combined with high temp. size exclusion chromatog. FTIR (HT-SEC-FTIR), HT-SEC-DSC and high temp. two-dimensional liq. chromatog. (HT-2D-LC) is used for the comprehensive anal. of a com. impact polypropylene copolymer. HT-SEC-FTIR provides information regarding the chem. compn. and crystallinity as a function of molar mass. Thermal anal. of selected SEC fractions yields the melting and crystn. behavior of these fractions which is related to the chem. heterogeneity of this complex copolymer. The thermal anal. of the fractions is conducted using a novel DSC method - high speed or high performance differential scanning calorimetry (HPer DSC) - that allows measuring of minute amts. of material down to micrograms. The most interesting and complex "midelution temp." TREF fraction (80 °C) of this copolymer is a complex mixt. of ethylene-propylene copolymers (EPC's) with varying ethylene and propylene contents and sequence length distributions, as well as iPP. High temp. solvent gradient HPLC has been used to show that there is a significant amt. of PE homopolymer and EPC's contg. long ethylene sequences in this TREF fraction. High temp. 2D-LC anal. reveals the complete sepn. of this TREF fraction according to the chem. compn. of each component along with their molar mass distributions. on SciFinder(R)]

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