By Harald Pasch, Muhammad Imran Malik
This Springer Laboratory quantity introduces the reader to complex innovations for the separation and fractionation of polyolefins. It comprises exact info on experimental protocols and strategies, addressing the experimental heritage of alternative polyolefin fractionation techniques in nice aspect. The ebook summarizes vital purposes in all significant fractionation methods with emphasis on multidimensional analytical ways. It includes the main strong smooth strategies, comparable 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). newbies in addition to skilled chromatographers will take advantage of this concise creation to a good kind in instrumentation, separation procedures and functions. With exact descriptions of experimental methods for the research of advanced polyolefins, the readers are provided a toolbox to unravel uncomplicated in addition to subtle separation tasks. The e-book begins with an creation into the molecular complexity of polyolefins - the main normal man made polymers with swiftly growing to be creation capacities. It systematically discusses crystallization established fractionation techniques together with TREF, CRYSTAF and CEF and column chromatographic recommendations for molar mass, chemical composition and microstructure, in addition to the mix 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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Extra info for Advanced Separation Techniques for Polyolefins
The fractions obtained between these two extreme temperatures are assumed to be semi-crystalline with compositional differences. All fractions were analysed by DSC, 13C-NMR and SEC-FTIR for determination of their chemical composition and thermal properties. The relationships established by Ray et al. 1. The method described by Kanezaki et al. 2. The results indicate that the TREF fractionation was governed by decreasing comonomer content and increasing isotacticity. The fractionation also depended upon the increasing sequence length; the average length (nx) of both ethylene and propylene sequences increased with increasing elution temperature.
G. eicosane) as well as well defined single-site catalyst resins were used. It is known that for high molar mass linear PE the methyl chain ends contribute little to the visible complexity of the spectrum. Thus, the linear PE provided the total polymer concentration (CH2) while the endgroups of the hydrocarbon provided the methyl group concentration (CH3). 9 shows expanded IR spectra of the linear PE and the hydrocarbon with corresponding peak deconvolutions to determine the polymer concentration and the methyl content.
SEC, however, separates according to molecular size and not chemical composition. Therefore, bimodality in the SEC profiles does not conclusively prove a chemical heterogeneity. One way to overcome this problem is to couple SEC with a selective detector such as FTIR, as has been shown in Sect. 1. In the present case, however, the LC-Transform interface is used instead of a flow cell. The operation of this device has been described elsewhere and a number of important applications have been presented [14, 69].
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