By Harald Pasch, Muhammad Imran Malik
This Springer Laboratory quantity introduces the reader to complex options for the separation and fractionation of polyolefins. It contains designated info on experimental protocols and techniques, addressing the experimental history of alternative polyolefin fractionation techniques in nice element. The ebook summarizes vital functions in all significant fractionation methods with emphasis on multidimensional analytical methods. It contains the main strong glossy innovations, similar to hot temperature measurement exclusion chromatography (HT-SEC) for molar mass research, temperature emerging elution fractionation (TREF) and crystallization research fractionation (CRYSTAF) for the research of chemical composition and branching, extreme temperature two-dimensional liquid chromatography (HT-2D-LC), solvent and temperature gradient interplay chromatography (SGIC and TGIC) and crystallization elution fractionation (CEF). newbies in addition to skilled chromatographers will take advantage of this concise creation to a superb style in instrumentation, separation procedures and functions. With unique descriptions of experimental techniques for the research of complicated polyolefins, the readers are provided a toolbox to unravel uncomplicated in addition to subtle separation tasks. The booklet starts off with an advent into the molecular complexity of polyolefins - the main wide-spread man made polymers with quickly becoming construction capacities. It systematically discusses crystallization dependent fractionation techniques together with TREF, CRYSTAF and CEF and column chromatographic recommendations for molar mass, chemical composition and microstructure, in addition to the combo of alternative fractionations in multidimensional experimental setups. This booklet additionally contains simple details at the program of high-temperature field-flow fractionation.
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Extra info for Advanced Separation Techniques for Polyolefins
Sample text
This is a clear indication that ethylene is only present in the higher molar mass components and the band at 1,378 cmÀ1 represents the methyl groups in PP only. There is a visible difference in the compositions of the lower and high molar mass components of the bimodal distribution. PP homopolymers are the sole component of the lower molar mass region, in contrast to the high molar mass part which is composed of EPCs with varying monomer distributions. The ethylene-rich copolymers appear on the higher molar mass side.
PP homopolymer will not elute entirely at high TREF temperatures, because PP fractions of lower isotacticity will become soluble within the same lower temperature range of the semi-crystalline EPC phase of corresponding crystallizability. Additional evidence for the complexity of the TREF fractions is obtained from the thermal behaviour, as shown in Fig. 14 for the DSC heating curves. As expected, no melting or crystallization is observed for the 30 C fraction. This fraction is amorphous and contains random EP rubber and (perhaps) some low molar mass PP with a low isotacticity.
Relatively uniform microstructures with long isotactic polypropylene (iPP) sequences and isolated 1-butene comonomer units were found by analysis of TREF fractions using CRYSTAF, SEC and 13C NMR. The increase in 1-butene content decreased the melting temperatures of the copolymers; therefore, higher temperature fractions contained less 1-butene content. Two LLDPE samples (comonomers 1-butene and 1-hexene) with similar densities were fractionated by van Reenen and co-workers. The melt flow index (MFI) values and comonomer contents were measured and the TREF fractions were analysed by high resolution solution and solid state NMR [27].