Characterization of low-molar-mass polymers by gradient polymer elution chromatography I. Practical parameters and applications of the analysis of polyester resins under reversed phase conditions

Philipsen, H. J. A.; Klumperman, Bert; German, Anton L.

doi:10.1016/0021-9673(96)00361-5

Cited by 42 publications

(58 citation statements)

References 31 publications

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“…In the first part of this series of papers, we clearly demonstrated the applicability of GPEC under reversed-phase conditions for the characterization of (co)polyester resins according to differences in chemical microstructure [8].…”

Section: Introductionmentioning

confidence: 86%

“…The molar ratio A:I:D is approximately 0.12:0.38:0.50 (NMR), the acid number is 20 mg KOH/g and the polystyrene equivalent molar masses as determined by SEC are 3500 (number-average molar mass, M,) and 7900 (weight-average molar mass, Mw), respectively. For more detailed information on the composition and characterization of the polyester sample we refer to [8].…”

Section: Polymer Sample and Narrow Disperse Fractionsmentioning

confidence: 99%

“…Since the contribution of these separate mechanisms can be different in each specific case, we prefer the use of the name gradient polymer 0021-9673/97/$17.00 Copyright © 1997 Elsevier Science B.V. All rights reserved PII S0021-9673(96)00807-2 elution chromatography (GPEC) [1,2] rather than existing names such as high-performance precipitation liquid chromatography (HPPLC) [3] or liquid adsorption chromatography (UAC) [4] which a priori assume a certain separation mechanism. Two main fields of application of GPEC include the characterization of copolymers according to their chemical composition distribution [5][6][7] and the fingerprinting of resins [8][9][10].…”

Section: Introductionmentioning

confidence: 99%

“…Therefore, a column filled with spherical glass beads, a bare silica column and a precolumn filter were tested for the use as an inert medium for polyester resins. A (co)polyester resin which has also been used for earlier experiments [8], was separated into several low polydispersity fractions by SEC. The obtained fractions were subjected to GPEC on several inert media and results were compared with a C J8 column, thus showing whether or not the absence of sorption influences the separation.…”

Section: Introductionmentioning

confidence: 99%

“…The obtained fractions were subjected to GPEC on several inert media and results were compared with a C J8 column, thus showing whether or not the absence of sorption influences the separation. The used S/NS system, tetrahydrofuran (THF)-water, was the same as used in the previous study [8]. Furthermore, for three different polyester fractions, results on the glass column were compared with maximum solubility measurements in various S/NS compositions under static equilibrium conditions.…”

Section: Introductionmentioning

confidence: 99%

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Characterization of low-molar-mass polymers by gradient polymer elution chromatography II. Solubility effects in the analysis of polyester resins under reversed-phase conditions

Philipsen¹,

Cooker

Claessens

et al. 1997

Journal of Chromatography A

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Section: Introductionmentioning

confidence: 86%

Section: Polymer Sample and Narrow Disperse Fractionsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Characterization of low-molar-mass polymers by gradient polymer elution chromatography II. Solubility effects in the analysis of polyester resins under reversed-phase conditions

Philipsen¹,

Cooker

Claessens

et al. 1997

Journal of Chromatography A

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Microstructural characterization of aromatic copolyesters made by step reactions, by gradient polymer elution chromatography

Philipsen¹,

Wubbe²,

Klumperman³

et al. 1999

J. Appl. Polym. Sci.

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The potentials of Gradient Polymer Elution Chromatography (GPEC) in both the Reversed‐Phase (RP) and Normal‐Phase (NP) mode, for the characterization of aromatic copolyesters made by step reactions, according to their chemical microstructure, were studied. Hereto, a number of copolyesters, varying in molar mass and chemical composition (CC) were synthesized, which allowed a systematic study on the effects of those parameters in GPEC. By RP‐GPEC, highly detailed separations were obtained. Information on chemical composition differences could, however, only be obtained for the lower molar masses. From these results, qualitative evidence for differences in the chemical microstructure of two strongly resembling copolyesters was found that could not be obtained by other methods such as SEC and NMR. Nevertheless, it was found difficult to unambiguously assign observed differences in the high molar mass parts of RP‐GPEC chromatograms. Therefore, RP‐GPEC must mainly be considered as a versatile, qualitative fingerprinting tool. In contrast, NP‐GPEC provides more and quantitative information on microstructural differences. By a combination of SEC and NP‐GPEC the Molar‐Mass‐Functionality‐Type‐Distribution (MMFTD) of the (co)polyesters, and the Molar‐Mass‐Chemical‐Composition‐Distribution (MMCCD) of the fraction containing two alcoholic end groups of the copolyesters could be studied. Significant differences between strongly resembling copolyesters were found which, for the MMCCDs, can only be the cause of the relative importance of reaction kinetics in step reaction copolymers. This makes the assumption that a predictable, theoretical statistically determined CCD is formed in all cases, questionable. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 72: 183–201, 1999

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Fractionation of Polymers

Lederer¹,

Ndiripo²

2023

Encyclopedia of Polymer Science and Technology

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Synthetic and natural polymers exist in microstructural distributions, such as chain length, size, chemical composition, branching, tacticity, or comonomer sequence distributions. Polymer fractionation techniques are essential for the analysis of these distributions and help in understanding polymerization mechanisms and material properties. In this article, the theoretical basics of general fractionation approaches and specific fractionation techniques are discussed. Details are given on fractionation techniques for molar mass and chemical composition distribution analysis, such as temperature rising elution fractionation (TREF), crystallization analysis fractionation (CRYSTAF), or crystallization elution fractionation (CEF). In addition, column‐based and channel‐based fractionation methods are extensively discussed. Theoretical and practical aspects of the analysis of molar mass distributions using size exclusion chromatography (SEC) as well as chemical composition distributions by interaction chromatography (SGIC, TGIC, LCCC) and multidimensional separations (2D‐LC) are reviewed and compared. General aspects and details on asymmetrical flow and thermal field flow fractionation techniques (AF4 and ThFFF) are discussed and examples of suitable physical and chemical detectors coupled to fractionation devices for the analysis of size, conformation, or chemical composition and topology are demonstrated.

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Characterization of low-molar-mass polymers by gradient polymer elution chromatography I. Practical parameters and applications of the analysis of polyester resins under reversed phase conditions

Cited by 42 publications

References 31 publications

Characterization of low-molar-mass polymers by gradient polymer elution chromatography II. Solubility effects in the analysis of polyester resins under reversed-phase conditions

Characterization of low-molar-mass polymers by gradient polymer elution chromatography II. Solubility effects in the analysis of polyester resins under reversed-phase conditions

Microstructural characterization of aromatic copolyesters made by step reactions, by gradient polymer elution chromatography

Fractionation of Polymers

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