‘Click’ Functionalization of Cryogels Conveniently Verified and Quantified Using High‐Resolution MAS NMR Spectroscopy

Camp, Wim Van; Dışpınar, Tuğba; Dervaux, Bart; Prez, Filip Du; Martins, José; Fritzinger, Bernd

doi:10.1002/marc.200900087

Cited by 20 publications

(18 citation statements)

References 34 publications

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“…As a complementary method to IR, Raman spectroscopy can reveal other functional groups (such as C-Cl and C≡N) that can be difficult to detect by IR [302][303]. Moreover, solid state [304][305], gel phase [306][307] and high-resolution magic angle spinning (HRMAS) NMR [308][309][310][311] techniques can be quite successfully applied to detect the functional groups and monitor reactions on particles. Availability of probes, operator experience and need of a suitable solvent for the analysis can be the parameters to tackle.…”

Section: Chemical Analysismentioning

confidence: 99%

Porous polymer particles—A comprehensive guide to synthesis, characterization, functionalization and applications

Gökmen

Prez

2012

Progress in Polymer Science

446

309

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Section: Chemical Analysismentioning

confidence: 99%

Porous polymer particles—A comprehensive guide to synthesis, characterization, functionalization and applications

Gökmen

Prez

2012

Progress in Polymer Science

446

309

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“…NMR spectroscopy has been more frequently catalysed azide-alkyne "click" cycloaddition reactions using high-resolution magic angle spinning (MAS) NMR spectroscopy. The authors observed complete conversion when benzylazide molecules reacted with the grafted alkyne functions, but only partial conversion was observed when they used azide-modified poly(ethylene glycol) [164]. Subsequent addition of benzylazide consumed all remaining alkyne groups.…”

Section: Low-temperature 1 H Nmr Spectroscopy Tsdc and Quantum Chemimentioning

confidence: 99%

“…All chemical modifications were easily monitored at each stage using the MAS NMR spectroscopy. The alkyne functionality and the resulting triazole ring gave well resolved 1 H resonances to monitor and quantify the progress of such "click" reactions in general [164]. However, the authors did not use the NMR method to study the textural characteristics of the synthesised cryogels.…”

Section: Low-temperature 1 H Nmr Spectroscopy Tsdc and Quantum Chemimentioning

confidence: 99%

Cryogels: Morphological, structural and adsorption characterisation

Gun'ko

Savina

Mikhalovsky

2013

Advances in Colloid and Interface Science

281

205

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*Graphical Abstract (for review)Cryotripic gelation technique allows the synthesis of solid and soft macroporous gels Textural characterisation of cryogel in native superhydrated state with noninvasive methods Adsorption and diffusion characteristics of macroporous cryogels with respect to macromolecules and cells Theoretical modelling of adsorption from aqueous media *Highlights (for review) Please find the revised manuscript entitled "Cryogels: morphological, structural and adsorption characterisation" by Vladimir M. Gun'ko, Irina N. Savina, Sergey V. Mikhalovsky to re-consider for publication in the "Advances in Colloid and Interface Science"The paper was completely edited and changed according to reviewers comments.Sincerely yours, Prof. V. M. Gun'koCover Letter ABSTRACTExperimental results on polymer, protein, and composite cryogels and data treatment methods used for morphological, textural, structural, adsorption and diffusion characterisation of the materials are analysed and compared. Treatment of microscopic images with specific software gives quantitative structural information on both native cryogels and freeze-dried materials that is useful to analyse the drying effects on their structure. A combination of cryoporometry, relaxometry, thermoporometry, small angle X-ray scattering (SAXS), equilibrium and kinetic adsorption of low and high-molecular weight compounds, diffusion breakthrough of macromolecules within macroporous cryogel membranes, studying interactions of cells with cryogels provides a consistent and comprehensive picture of textural, structural and adsorption properties of a variety of cryogels. This analysis allows us to establish certain regularities in the cryogel properties related to narrow (diameter 0.4 < d < 2 nm), middle (2 < d < 50 nm) and broad (50 < d < 100 nm) nanopores, micropores (100 nm < d < 100 m) and macropores (d > 100 m) with boundary sizes within modified life science pore classification. Particular attention is paid to water bound in cryogels in native superhydrated or freeze-dried states. At least, five states of water -free unbound, weakly bound (changes in the Gibbs free energy G < 0.5-0.8 kJ/mol) and strongly bound (G > 0.8 kJ/mol), and weakly associated (chemical shift of the proton resonance  H = 1-2 ppm) and strongly associated ( H = 3-6 ppm) waters can be distinguished in hydrated cryogels using 1 H NMR, DSC, TSDC, TG and other methods. Different software for image treatment or developed to analyse the data obtained with the adsorption, diffusion, SAXS, cryoporometry and thermoporometry methods and based on regularisation algorithms is analysed and used for the quantitative morphological, structural and adsorption characterisation of individual and composite cryogels, including polymers filled with solid nano-or microparticles.

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“…[30,31] Other HR-MAS studies observed the impact of cross-linking in solvent swollen poly(amidoamine) polymers, the nature of water interactions in these same class of polymers, [32,33] or the cross-linking performance in silicon-containing soybean-oil copolymers. [34] HR-MAS NMR has also been used to study the functionalization of poly hydroxyethyl methacrylate (HEMA) cryogels, [35] cyclomaltoheptaose polymers, [36] the synthesis of hyper-branched bis (hydroxymethyl) propionic acid (bis-MPA) polymers as a function of catalysts, [37] and polymers for nanoparticle stabilization. [38] HR-MAS NMR has found use in investigation of porous polyalkylvinyl ether polymer particles being used for stationary phases in chromatographic applications.…”

Section: Polymersmentioning

confidence: 99%