By Harald Pasch, Muhammad Imran Malik
This Springer Laboratory quantity introduces the reader to complex thoughts for the separation and fractionation of polyolefins. It comprises exact info on experimental protocols and strategies, addressing the experimental heritage of other polyolefin fractionation techniques in nice aspect. The ebook summarizes vital functions in all significant fractionation methods with emphasis on multidimensional analytical techniques. It contains the main strong glossy concepts, 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, hot temperature two-dimensional liquid chromatography (HT-2D-LC), solvent and temperature gradient interplay chromatography (SGIC and TGIC) and crystallization elution fractionation (CEF). newcomers in addition to skilled chromatographers will take advantage of this concise creation to a good sort in instrumentation, separation procedures and functions. With particular descriptions of experimental techniques for the research of advanced polyolefins, the readers are provided a toolbox to unravel uncomplicated in addition to refined separation tasks. The e-book starts off with an creation into the molecular complexity of polyolefins - the main universal artificial polymers with quickly turning out to be construction capacities. It systematically discusses crystallization established fractionation techniques together with TREF, CRYSTAF and CEF and column chromatographic thoughts for molar mass, chemical composition and microstructure, in addition to the combo of alternative fractionations in multidimensional experimental setups. This e-book additionally comprises uncomplicated details at the program of high-temperature field-flow fractionation.
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Additional resources for Advanced Separation Techniques for Polyolefins
Typically, a set of well defined copolymers with narrow CCDs and known compositions (from NMR) is measured by TREF and the peak maximum elution temperature for each sample is determined. 1 Temperature Rising Elution Fractionation 23 % comonomer to give a suitable calibration curve. Quite frequently, copolymer composition is expressed as the number of methyl groups per 1,000 carbons (CH3/ 1,000C). A much more feasible approach is the ‘real time’ measurement of the copolymer composition using an online FTIR detector.
The correlation of molecular structure and mechanical properties of ethylene-1-hexene copolymer film grade resins produced by a metallocene catalyst by varying the molar mass and branching distribution was studied by Alamo and co-workers . Molar mass fractionation was achieved by solvent/non-solvent techniques, while fractionation with respect to 1-hexene content was obtained by P-TREF. The hyphenation of TREF with SEC-FTIR offered a simple alternative to conventional and time-consuming methods for characterizing the compositional heterogeneity of IPCs .
The results of the SEC-FTIR analysis of the TREF fractions are summarized in Figs. 16. 2 Crystallization-Based Fractionation Techniques A(1376cm )/A(1462cm ) Intensity (2800-3200cm ) 32 50 Elution volume (ml) Fig. 15 SEC-FTIR analysis of the ethylene and propylene distribution within the 60 C, 80 C, 90 C and 100 C TREF fractions of IPC (reprinted from  with permission of Wiley-VCH) The Gram–Schmidt plots represent the total FTIR absorption over the 2,800– 3,200 cmÀ1 range of the spectrum.