Combined size exclusion chromatography, supercritical fluid chromatography and electrospray ionization mass spectrometry for the analysis of complex aliphatic polyesters

Pretorius, Nadine O.; Willemse, Chandré M.; Villiers, André de; Pasch, Harald

doi:10.1016/j.chroma.2014.01.018

Cited by 11 publications

(7 citation statements)

References 27 publications

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“…To help verify this material, we separately synthesized BTTT1.5; detailed synthesis is available in the Supporting Information. Fractionation of aliphatic polymers in SCF has previously been reported, , but this result is the first to show the fractionation and concurrent crystallization of conjugated materials.…”

supporting

confidence: 59%

Poly[2,5-bis(3-dodecylthiophen-2-yl)thieno[3,2-b]thiophene] Oligomer Single-Crystal Nanowires from Supercritical Solution and Their Anisotropic Exciton Dynamics

Colella¹,

Labastide²,

Cherniawski³

et al. 2017

J. Phys. Chem. Lett.

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Supercritical fluids, exhibiting a combination of liquid-like solvation power and gas-like diffusivity, are a relatively unexplored medium for processing and crystallization of oligomer and polymeric semiconductors whose optoelectronic properties critically depend on the microstructure. Here we report oligomer crystallization from the polymer organic semiconductor, poly[2,5-bis(3-dodecylthiophen-2-yl)thieno[3,2-b]thiophene] (PBTTT) in supercritical hexane, yielding needle-like single crystals up to several microns in length. We characterize the crystals' photophysical properties by time- and polarization-resolved photoluminescence (TPRPL) spectroscopy. These techniques reveal two-dimensional interchromophore coupling facilitated by the high degree of π-stacking order within the crystal. Furthermore, the crystals obtained from supercritical fluid were found to be similar photophysically as the crystallites found in solution-cast thin films and distinct from solution-grown crystals that exhibited spectroscopic signatures indicative of different packing geometries.

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supporting

confidence: 59%

Poly[2,5-bis(3-dodecylthiophen-2-yl)thieno[3,2-b]thiophene] Oligomer Single-Crystal Nanowires from Supercritical Solution and Their Anisotropic Exciton Dynamics

Colella¹,

Labastide²,

Cherniawski³

et al. 2017

J. Phys. Chem. Lett.

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“…Regarding some of the aspects, the SFC shows a faster separation and better resolution than LC. Several researchers have reported that SFC is an eminent technique used to separate simple polymers with unique degree of polymerization(n) . The SFC‐MS was used to analyze alkylpoly glycerylether , which provided further understanding on the surface activity products composition after etherification and was also developed for the fast determination of alkylphenol ethoxylates in leafy vegetables .…”

Section: Introductionmentioning

confidence: 99%

Development of supercritical fluid chromatography coupled with mass spectrometry method for characterization of a nonionic surfactant and comparison with liquid chromatography coupled with mass spectrometry method

et al. 2020

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The supercritical fluid chromatography coupled with mass spectrometry (SFC-MS) method and liquid chromatography coupled with mass spectrometry (LC-MS) method were developed for the separation and characterization of poly (ethylene oxide) methyl glucose sesquistearate (PEO-Glu-sesquistearate). The products of PEO-Glusesquistearate are composed of complex oligomers. The relationship between molecular structure of these oligomers and chromatographic retention behavior in both SFC and LC were discussed and compared. As compared with LC, hydrophobic moieties of compounds favor the fast elution in SFC. The different series can be better separated by LC, while the homologues compounds in same series can be better separated by SFC, and SFC-MS provided more comprehensive structural information. Different series such as PEO-distearate, PEO-stearate, PEO, PEO-Glu-tetrastearate, PEO-Glu-tristearate, PEO-Glu-distearate, PEO-Glu-stearate, and PEO-Glu were identified by MS/MS. K E Y W O R D S chromatographic retention behavior, fragment identification, LC-MS, nonionic surfactant, SFC-MS 1 | INTRODUCTION The poly (ethylene oxide) methyl glucose sesquistearate (PEO-Glusesquistearate) is a sugar-based nonionic surfactants with low toxicity and high surface activity, which is widely used as emulsifiers, solubilizers, and stabilizers in cosmetics 1 , drugs 2 , and biodegradation media 3 . PEO-Glu-sesquistearate, as amphiphilic polymers, contains varying quantities of by-products. The formulation of the by-products is complicated, which includes PEO, PEO stearate(s), and PEO-methyl glucose stearate(s) with varying numbers of EOs at varying degrees of esterification (none, mono-, di-, tri-, and quadri-). The structure of PEO-methyl glucose stearate is shown in

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“…Variations in their molecular mass, chemical composition, end group functionality and topology determine their physical properties and their use as materials for applications ranging from industrial construction products to drug delivery systems in the life sciences. Although significant advances have occurred in polymer synthesis, the focal point of characterization has been mostly on molecular weight distribution (MWD) [2,3]. Typically, the MWD of synthetic polymers is determined by size exclusion chromatography (SEC) and/or matrix assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) [3].…”

Section: Introductionmentioning

confidence: 99%

“…Although significant advances have occurred in polymer synthesis, the focal point of characterization has been mostly on molecular weight distribution (MWD) [2,3]. Typically, the MWD of synthetic polymers is determined by size exclusion chromatography (SEC) and/or matrix assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) [3]. The two techniques are essentially complementary.…”

Section: Introductionmentioning

confidence: 99%

Novel behavior of the chromatographic separation of linear and cyclic polymers

et al. 2015

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In various polymerization processes, the formation of a wide variety of chains, not only in length but also in chemical composition, broadly complicates comprehensive polymer characterization. In this communication, we compare different stationary and mobile phases for the analysis of complex polymer mixtures via size-exclusion chromatography-mass spectrometry (SEC-MS). To the best of our knowledge, we report novel chromatographic effects for the separation of linear and cyclic oligomers for polyesters (PE) and polyurethanes (PUR). A complete separation for the different structures was achieved for both polymer types with a single solvent system (ACN) and without extensive optimization. Additionally, cyclic species were found to show an inverse elution profile compared to their linear counterparts, suggesting distinct physical properties between species.

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Combined size exclusion chromatography, supercritical fluid chromatography and electrospray ionization mass spectrometry for the analysis of complex aliphatic polyesters

Cited by 11 publications

References 27 publications

Poly[2,5-bis(3-dodecylthiophen-2-yl)thieno[3,2-b]thiophene] Oligomer Single-Crystal Nanowires from Supercritical Solution and Their Anisotropic Exciton Dynamics

Poly[2,5-bis(3-dodecylthiophen-2-yl)thieno[3,2-b]thiophene] Oligomer Single-Crystal Nanowires from Supercritical Solution and Their Anisotropic Exciton Dynamics

Development of supercritical fluid chromatography coupled with mass spectrometry method for characterization of a nonionic surfactant and comparison with liquid chromatography coupled with mass spectrometry method

Novel behavior of the chromatographic separation of linear and cyclic polymers

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