Abstract
Nuclear magnetic resonance (NMR) relaxometry of liquids is a widely used tool to characterize porous media. In particular, 23Na NMR is an especially suitable method when applied to gels and biological tissues. In this work we investigated the thermoreversible melting and gelation processes of supramolecular hydrogels formed by succinamic acid-based amphiphiles (SAn) in a saturated aqueous NaHCO3 solution (sat. aq. NaHCO3 sol.). We could show that it is not only possible to determine the melting points and to monitor the gelation process with 23Na relaxometry, but also to estimate the effective pore size based on the expanded Brownstein-Tarr model. Our findings are in good agreement with data from differential scanning calorimetry (DSC) and transmission electron microscopy (TEM) experiments.
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- aq.:
-
Aqueous
- CPMG:
-
Carr-Purcell-Meiboom-Gill
- DSC:
-
Differential scanning calorimetry
- ff:
-
Freeze-fracture replica
- NMR:
-
Nuclear magnetic resonance
- RT:
-
Room temperature
- SAn:
-
Succinamic acid-based amphiphiles (n: number of carbon atoms in linear alkyl chain)
- sat.:
-
Saturated
- SEM:
-
Scanning electron microscopy
- sol.:
-
Solution
- TEM:
-
Transmission electron microscopy
References
Tromp RH, van der Maarel JR, de Bleijser J, Leyte JC (1991) Counter-ion dynamics in crosslinked poly(styrene sulfonate) systems studied by NMR. Biophys Chem 41:81–100
Gustavsson H, Lindman B, Bull T (1978) Sodium-23 nuclear magnetic resonance in polyanion solution. Correlation times and quadrupole coupling constants of sodium(+) bound to poly(methacrylic acid). J Am Chem Soc 100:4655–4661
Levij M, de Bleijser J, Leyte JC (1981) Long-range electric field gradients in charged polymer solutions as probed by sodium-23 relaxation. Chem Phys Lett 83:183–191
Woessner DE (2001) NMR relaxation of spin-3/2 nuclei: effects of structure, order, and dynamics in aqueous heterogeous systems. Concepts Magn Reson 13:294–325
Rijniers LA, Magusin PCMM, Huinink HP, Pel L, Kopinga K (2004) Sodium NMR in porous materials. J Magn Reson 167:25–30
Brownstein KR, Tarr CE (1979) Importance of classical diffusion in NMR studies of water in biological cells. Phys Rev A 19:2446–2453
Valckenborg EMW, Pel L, Hazrati K, Kopinga K, Marchand J (2001) Pore water distribution in mortar during drying as determined by NMR. Mater Struct 34:599–604
de Loos M, Feringa BL, van Esch JH (2005) Design and application of self-assembled low molecular weight hydrogels. Eur J Org Chem 17:3615–3631
Dastidar P (2008) Supramolecular gelling agents: can they be designed? Chem Soc Rev 37:2699–2715
Sangeetha NM, Matira U (2005) Supramolecular gels: functions and uses. Chem Soc Rev 34:821–836
Estroff LA, Hamilton AD (2004) Water gelation by small organic molecules. Chem Rev 104:1201–1217
The self-assembly behavior and hydrogel formation potential of the succinamic acid-based class of amphiphiles will be reported in detail elsewhere.
Turco G, Donati I, Grassi M, Marchioli G, Lapasin R, Paoletti S (2011) Mechanical spectroscopy and relaxometry on alginate hydrogels: a comparative analysis for structural characterization and network mesh size determination. Biomacromolecules 12:1272–1282
Wallace M, Adams DJ, Iggo JA (2013) Analyses of the mesh size in a supramolecular hydrogel by PFG-NMR spectroscopy. Soft Matter 9:5483–5491
Höhne G, Hemminger W, Flammersheim HJ (1996) Differential scanning calorimetry. Springer, Berlin
Roy S, Dasgupta A, Das PK (2007) Alkyl chain length dependent hydrogelation of L-Tryptophan-based amphiphile. Langmuir 23:11769–11776
Wang D, Hao J (2011) Self-assembly fibrillar network gels of simple surfactants in organic solvents. Langmuir 27:1713–1717
Hao J, Liu W, Yuan Z (2008) Gel phase originating from molecular quasi-crystallization and nanofiber growth of sodium laurate-water system. Soft Matter 4:1639–1644
Acknowledgments
The authors wish to thank the German Research Foundation (DFG) for financial support in the frame of Programme SPP 1259 “Intelligente Hydrogele”. We are indebted to Dr. M. Krekhova for the preparation of the ff-TEM images and M. Behr for fruitful discussions.
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© 2013 Springer International Publishing Switzerland
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Raue, M. et al. (2013). Sodium NMR Relaxation: A Versatile Non-invasive Tool for the Monitoring of Phase Transitions and the Estimation of Effective Pore Sizes of Supramolecular Hydrogels. In: Sadowski, G., Richtering, W. (eds) Intelligent Hydrogels. Progress in Colloid and Polymer Science, vol 140. Springer, Cham. https://doi.org/10.1007/978-3-319-01683-2_4
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DOI: https://doi.org/10.1007/978-3-319-01683-2_4
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