Characterization of Polyalkylvinyl Ether Phases by Solid-State and Suspended-State Nuclear Magnetic Resonance Investigations

Bachmann, Stefan; Hellriegel, Christine; Wegmann, Jürgen; Händel, Heidi; Albert, Klaus

doi:10.1006/snmr.2000.0004

Cited by 21 publications

(8 citation statements)

References 25 publications

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“…These measurements were performed using the same solvent as HPLC and allowed details about the polymer structure and mobility to be evaluated; these properties are expected to impact the chromatographic process. [39] Interactions between solution molecules and the polymer component of HPLC stationary phases (C18, C30 and PEAA) [40] or the interaction with molecularly imprinted polymers [41] have also been investigated using HR-MAS NMR. These studies used saturation transfer difference pulse sequences to identify those molecules that were involved in binding to the larger stationary phase.…”

Section: Polymersmentioning

confidence: 99%

HR-MAS NMR Spectroscopy in Material Science

Alam¹,

Jenkins²

2012

Advanced Aspects of Spectroscopy

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Section: Polymersmentioning

confidence: 99%

HR-MAS NMR Spectroscopy in Material Science

Alam¹,

Jenkins²

2012

Advanced Aspects of Spectroscopy

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“…Our study also connects to characterization of silica‐based chromatography media with solid‐state NMR, a field that has been active for many years. Besides investigating the molecular dynamics of components immobilized on silica or on polymeric resins and the interactions between bound ligands and analytes in the mobile phase, a few MAS NMR studies concerned the ligand concentration in stationary phases such as chromatography media or resins for solid‐phase organic synthesis . Here, we present for the first time quantitative MAS NMR to measure ligand concentration in a chromatography medium based on a soft polysaccharide hydrogel resin.…”

Section: Introductionmentioning

confidence: 99%

¹³C SPE MAS measurement of ligand concentration in compressible chromatographic beads

Elwinger

Dvinskikh

Furó

2015

Magnetic Reson in Chemistry

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A method for measuring the ligand concentration in heterogeneous materials like chromatography media is described. In this method, 13C single pulse excitation magic angle spinning NMR experiment with broadband 1H decoupling is used to determine the peak integrals for a butyl ligand in the spectrum of a dried chromatography medium. Within a carefully controlled protocol, those integrals compared with that of the internal reference compound dimethyl sulfone provide the required volume concentration with an accuracy of ca 2%. The effects of temperature, degree of hydration, and other experimental parameters are discussed. Copyright © 2015 The Authors. Magnetic Resonance in Chemistry published by John Wiley & Sons Ltd.

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“…[32±36] Solid-state NMR spectroscopy ( 29 Si and 13 C cross polarization magic angle spinning (CP/MAS)) proved its great importance, wide range of application, and its meaningfulness in the demanding, detailed structure elucidation. [32,37,38] The existence of alkyl chains of different mobilities and their alignment influences the separation process. This shows that the separation can be improved if the molecular recognition sites have similar structures.…”

Section: Introductionmentioning

confidence: 99%

New Inorganic-Organic Hybrid Materials for HPLC Separation Obtained by Direct Synthesis in the Presence of a Surfactant

et al. 2002

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Nanostructured, mesoporous inorganic–organic hybrid xerogels were reproducibly synthesized by a sol–gel procedure. For the introduction of long alkyl chains into inorganic polymers, trifunctional n‐alkyltrialkoxysilanes of the type CH3(CH2)nSi(OR)3 (n = 7, 11, 17; R = CH3, C2H5) were co‐condensed with Si(OEt)4 (TEOS). The synthetic pathway involves the employment of n‐hexadecylamine as template and catalyst. The xerogels obtained by the present procedure consist of uniform spherical particles with a diameter of about 1 μm. The composition of the new materials was determined by 13C and 29Si cross polarization magic angle spinning (CP/MAS) NMR spectroscopy. In addition, the degree of organization was investigated by small angle X‐ray and electron diffraction. In accordance with 13C CP/MAS NMR spectroscopic measurements, the alkyl chains form a crystalline arrangement within the silica polymer. Brunauer–Emmett–Teller (BET) adsorption measurements confirm specific surface areas of up to 1400 m2/g. The material properties prove the xerogels to be suitable as stationary phases in high‐performance liquid chromatography (HPLC). These novel mesoporous, nanostructured materials have been successfully employed in HPLC for the first time. Different standard reference materials (SRMs) containing polycyclic aromatic hydrocarbons have been separated with the xerogels described in the present work.

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Characterization of Polyalkylvinyl Ether Phases by Solid-State and Suspended-State Nuclear Magnetic Resonance Investigations

Cited by 21 publications

References 25 publications

HR-MAS NMR Spectroscopy in Material Science

HR-MAS NMR Spectroscopy in Material Science

¹³C SPE MAS measurement of ligand concentration in compressible chromatographic beads

New Inorganic-Organic Hybrid Materials for HPLC Separation Obtained by Direct Synthesis in the Presence of a Surfactant

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Characterization of Polyalkylvinyl Ether Phases by Solid-State and Suspended-State Nuclear Magnetic Resonance Investigations

Cited by 21 publications

References 25 publications

HR-MAS NMR Spectroscopy in Material Science

HR-MAS NMR Spectroscopy in Material Science

13C SPE MAS measurement of ligand concentration in compressible chromatographic beads

New Inorganic-Organic Hybrid Materials for HPLC Separation Obtained by Direct Synthesis in the Presence of a Surfactant

Contact Info

Product

Resources

About

¹³C SPE MAS measurement of ligand concentration in compressible chromatographic beads