Size Exclusion Chromatography

Podzimek, Štěpán

doi:10.1002/0471440264.pst058.pub2

Cited by 2 publications

(2 citation statements)

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“…The molar mass versus elution volume plot overlaid on the RI and MALS chromatograms is depicted in Figure 8. The upswing in the molar mass plot at the end of the chromatogram is often observed on the plots of branched polymers 22 . In order to improve the accuracy of the MMD at the region of lower molar masses, the molar mass plot was extrapolated from the region of lower elution volume forward to the end of the chromatogram in order to eliminate the upswing.…”

Section: Resultsmentioning

confidence: 99%

“…The two plots differ markedly by their slopes, that of PMMA indicates linear chain topology (the slope of linear polymers in thermodynamically good solvents ≈0.58), whereas that of SPEEK is typical for highly compact branched macromolecules. 22 The molar mass of unsulfonated PEEK is related to the molar mass of sulfonated PEEK by the following relation 7 :…”

Section: Discussionmentioning

confidence: 99%

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Size exclusion chromatography characterization of poly (ether ether ketone), PEEK, after chemical modification

Aboelanin

Arndt

Macko

et al. 2023

J of Applied Polymer Sci

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Characterization of the molar mass distribution (MMD) of poly (ether ether ketone) (PEEK) is very troublesome due to the insolubility of PEEK in common solvents. The solubility of PEEK may be substantially improved after its sulfonation. Sulfonated PEEK (SPEEK) was prepared by sulfonation of PEEK with 98% concentrated H2SO4 at room temperature. The presence of sulfonic acid group (‐SO3H) in PEEK matrix was confirmed by nuclear magnetic resonance and Fourier transform infrared spectroscopy. The degree of sulfonation (DS ~ 95%) was determined by proton nuclear magnetic resonance in deuterated dimethyl sulfoxide and by thermal analysis methods. The equivalent molar mass and MMD of sulfonated PEEK was determined at 30°C in three polar solvents (N,N‐dimethylacetamide, N,N‐dimethylformamide N‐methyl‐2‐pyrollidone) in PS/DVB column using calibration with PMMA standards. A salt (LiBr) was added to the solvents for suppression of undesired interactions of analytes with the column packing. Moreover, the sulphonated PEEK was separated with size exclusion chromatography (SEC) coupled to a multi‐angle light scattering (MALS) detector. It was found that the absolute average molar mass of SPEEK from the MALS detection is much closer to the value measured by SEC in N,N‐dimethylacetamide +LiBr than the values determined in N,N‐dimethylformamide and N‐methyl‐2‐pyrollidone.

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Section: Resultsmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%