Selective chromatographic separation of polycarbonate according to hydroxyl end-groups using a porous graphitic carbon column

Apel, Nico; Uliyanchenko, Elena; Moyses, Stephan; Rommens, Stijn; Wold, Christian; Macko, Tibor; Rode, Karsten; Brüll, Robert

doi:10.1016/j.chroma.2017.01.075

Cited by 16 publications

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“…a) Comparison of a) a critical diagram with b) the 2D contour plot of PC3. The axes of the HPLC and the SEC elution volume were interchanged to illustrate the similarity with the critical diagram.…”

Section: Resultsmentioning

confidence: 99%

“…Number ( M n ) and weight-average ( M w ) molar masses as determined by SEC are listed in Table . The experimental setup and details of the Mark–Houwink calibration are stated elsewhere . End-capping of the samples was analyzed by 1 H NMR according to the method described by Kim et al…”

Section: Methodsmentioning

confidence: 99%

“…Houwink calibration are stated elsewhere. 35 End-capping of the samples was analyzed by 1 H NMR according to the method described by Kim et al 36 Solvent Gradient at Near-Critical Conditions. An Agilent 1100 series HPLC system from Agilent, Waldbronn, Germany, consisting of a vacuum degasser, a quaternary gradient pump, an autosampler, a column oven, and a variable wavelength (UV) detector was used.…”

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Separation of Branched Poly(bisphenol A carbonate) Structures by Solvent Gradient at Near-Critical Conditions and Two-Dimensional Liquid Chromatography

et al. 2018

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Branching is a molecular metric that strongly influences the application properties of polymers. Consequently, detailed information on the microstructure is required to gain a deeper understanding of structure-property relationships. In the present case, we employ high-performance liquid chromatography to characterize the branching in a poly(bisphenol A carbonate) (PC). To this end, a method was developed based on a mobile phase gradient in a very narrow range (±1.4 vol %) around the point of adsorption (98.9/1.1 vol % chloroform/methyl tert-butyl ether), which we refer to as solvent gradient at near-critical conditions. Application of such gentle gradient enabled separation of PC according to end-groups. The separation mechanism was confirmed by collecting fractions of a separated sample and subsequently analyzing these by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. Hyphenating the developed gradient method with size-exclusion chromatography as the second dimension (2D-LC) enabled separation of linear and branched PC chains and determination of the molar mass distribution of the fractions. A reversed elution order was observed for branched species in 2D-LC, meaning that low molar mass chains exhibited higher elution volumes in the first dimension than higher molar masses. This finding was explained by influences of end-groups as well as the architecture of the branched polymer chains.

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Section: Methodsmentioning

confidence: 99%

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