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

Philipsen, H. J. A.; Wubbe, F. P. C.; Klumperman, B.; German, A. L.

doi:10.1002/(sici)1097-4628(19990411)72:2<183::aid-app4>3.3.co;2-a

Cited by 5 publications

(12 citation statements)

References 16 publications

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“…The separation of the DC sample was carried out by gradient polymer elution chromatography (GPEC), according to a general method described in the literature 30–32…”

Section: Resultsmentioning

confidence: 99%

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Molecular level differentiation between end‐capped and intramolecular azofunctional oligo(ε‐caprolactone) positional isomers through liquid chromatography multistage mass spectrometry

Peptu

Brink

Harabagiu³

et al. 2012

J. Polym. Sci. A Polym. Chem.

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End-capped and intramolecular azofunctional oligocaprolactones were characterized at molecular level by liquid chromatography electrospray ionization mass spectrometry (ESI MS) and NMR spectroscopy. The Disperse Red 19 (DR19) azofunctional oligomers, DC, were synthesized by ring-opening oligomerization of e-caprolactone (e-CL) initiated by the hydroxyl groups of DR19 azo dye. The reaction products consist of a minor fraction of end-capped azo functional oligocaprolactone (a-DC), that is, a single CL arm oligomer, and a major fraction of intramolecular azo functional oligocaprolactone (b-DC), that is, a two CL arms oligomer. The chromatographic separation was used to discriminate between a-DC and b-DC, and the results were confirmed by MS/MS performed on an ESI ion trap instrument. The results supported by accurate mass data obtained for product ions using an ESI quadrupole time of flight instrument demonstrate the qualitative discrimination at the molecular level between intramolecular and end-capped azofunctional oligoesters isomers through a relatively simple multistage mass spectrometry experiment.

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“…The separation of the DC sample was carried out by gradient polymer elution chromatography (GPEC), according to a general method described in the literature 30–32…”

Section: Resultsmentioning

confidence: 99%

“…GPEC30–32 experiments were performed using an Agilent 1100 series LC system (Agilent Technology, Santa Clara, CA) equipped with simultaneous DAD and MS (ESI IT) detection. The chromatographic column was Kromasil® C18—4.6 mm × 150 mm, 5‐μm particle size (Alltech).…”

Section: Methodsmentioning

confidence: 99%

Molecular level differentiation between end‐capped and intramolecular azofunctional oligo(ε‐caprolactone) positional isomers through liquid chromatography multistage mass spectrometry

Peptu

Brink

Harabagiu³

et al. 2012

J. Polym. Sci. A Polym. Chem.

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“…GPEC was applied using an UV diode array detector for quantification and online ESI TOF for identification of the oligomers in the MWD. GPEC is based on a combination of precipitation/redissolution, sorption, and exclusion processes. , The technique requires a gradient LC system with at least two solvents. One of the solvents, which is often a bad solvent for the polymer of interest, results in a precipitation of the polymer after injection on the column.…”

Section: Resultsmentioning

confidence: 99%

“…The polymers used for this study are the homopolyesters poly(dipropoxylated bisphenol A/adipic acid) and poly(dipropoxylated bisphenol A/isophthalic acid) and the copolyester poly(dipropoxylated bisphenol A/adipic acid/isophthalic acid). These polymers were a gift from Océ Technologies (Venlo, The Netherlands) and are from the same batch as the polyesters described in a previous publication …”

Section: Methodsmentioning

confidence: 99%

Quantitative Analysis of Copolymers: Influence of the Structure of the Monomer on the Ionization Efficiency in Electrospray Ionization FTMS

Koster¹,

Mulder²,

Duursma³

et al. 2002

Macromolecules

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The influence of the ionization efficiency on the measured copolymer sequence distribution is presented. Large differences in ionization efficiency were observed for mixtures of homopolyesters containing dipropoxylated bisphenol A/adipic acid and dipropoxylated bisphenol A/isophthalic acid and the corresponding copolyester dipropoxylated bisphenol A/isophthalic acid/adipic acid. The adipic acid structure has a higher affinity for the sodium cation, which results in more intense peaks for adipic acid containing oligomers. Relative sodium affinities of the oligomers were found to increase with an increasing number of acid end groups in favor of adipic acid containing oligomers. The ESI response of the oligomers depends on the polymer concentration in the sprayed mixture. This makes it impossible to correct for the ionization efficiency necessary for copolymer analysis. If differences in ionization efficiency are not corrected, the ion intensities in the copolymer mass spectra will show large deviations from the real composition and no conclusion can be drawn about the chemical (in)homogeneity of the MWD nor the random or block structure of the copolymer. This will also be valid for other cationization techniques like MALDI and FAB.

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“…Both isocratic [1] and gradient-based liquid chromatography [2,3] have been utilized to characterize oligomer, [4] polymer [5,6] or copolymer blend, [7] statistical, [2] block, [8,9] and graft copolymers [10] as well as to separate homopolymers according to their tacticity. [11,12] Based on the different elution behavior of homopolymers with respect to the eluent composition (exclusion, transition, adsorption), [1] several attempts have been made to develop isocratic elution methods for the determination of statistical or block copolymer composition.…”

Section: Introductionmentioning

confidence: 99%

Characterization of Random Copolymers by Liquid Chromatography under Limiting Conditions of Adsorption

Sauzedde

Bartkowiak

Hunkeler

2006

International Journal of Polymer Analysis and Characterization

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Liquid chromatography under limiting conditions of adsorption (LC LCA) can be considered as a new tool to perform, simultaneously, molar mass and composition determination of statistical copolymers and to separate copolymer blends as a function of copolymer composition or microstructure. The suitability of LC LCA has been demonstrated for two series of statistical copolymers, poly(styrene-co-methyl methacrylate), poly(S=MMA), varying either in molar mass or composition. The binary eluent consisted of a mixture of n-hexane and THF, containing either 26 or 30 vol.% of n-hexane, respectively, for low and high LC LCA. Two parameters, the ratio of peak area over height and the ratio of peak area of chromatograms obtained by LC LCA and size exclusion chromatography (SEC), were employed to evaluate statistical copolymer elution through LC LCA. From the peak analyses, macromolecule recovery was complete over the entire composition and the molar mass ranges. LC LCA and SEC were further compared, and off-line fractionation was subsequently performed using a combination of both methods, with different statistical copolymer solutions having narrow, broad, and bimodal composition distributions.

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

Cited by 5 publications

References 16 publications

Molecular level differentiation between end‐capped and intramolecular azofunctional oligo(ε‐caprolactone) positional isomers through liquid chromatography multistage mass spectrometry

Molecular level differentiation between end‐capped and intramolecular azofunctional oligo(ε‐caprolactone) positional isomers through liquid chromatography multistage mass spectrometry

Quantitative Analysis of Copolymers: Influence of the Structure of the Monomer on the Ionization Efficiency in Electrospray Ionization FTMS

Characterization of Random Copolymers by Liquid Chromatography under Limiting Conditions of Adsorption

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