Abstract
The gelation of an aqueous (aq) solution of the sodium salt of carboxyethylcellulose (NaCEC: total degree of substitution <<F>>=0.39) by contacting several aqueous metal chloride solutions was investigated visually and by 13C NMR analysis. Diffusion of acidic Ti3+ and Al3+ into aq NaCEC solution was found to produce CEC gel with high dimensional stability, slightly loosing the original transparency of aq NaCEC solution. Purple Ti3+ ion was proved to diffuse slower than proton ion. Ca2+ was also found to produce CEC gel having a little weaker dimensional stability than those obtained by Ti3+ and Al3+. It was also affirmed that deuterated hydrogen chloride solution was significantly opaque. Any diffusion of Na+ and K+ into NaCEC solution produced no gel and aq NaCEC solution remained as solution phase. Analysis on the chemical shift and the half value width of 13C NMR peaks obtained for the CEC gel phases in comparison with those of the peaks for the original NaCEC solution revealed that only Al3+ and Ti3+ produced considerable broadening and splitting of the peaks responsible for the carboxyethyl substituent, but DCl only resulted in a peak shift towards a higher magnetic field with no peak broadening. Chemical shift of C1 carbon, constituting backbone of NaCEC, of the CEC gels gave different values from gel to gel, showing some difference in configuration of β-glucoside linkage of these CEC gels. Several possible gelation mechanisms were proposed to explain the roles of the cation species and pH value of their solutions used for contacting the aqueous NaCEC solution.
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Kamide, K., Yasuda, K. & Okajima, K. 13C NMR Study on Gelation of Aqueous Carboxyethylcellulose with Total Degree of Substitution of 0.39 Solution Induced by Metal Cations. Polym J 20, 259–268 (1988). https://doi.org/10.1295/polymj.20.259
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DOI: https://doi.org/10.1295/polymj.20.259
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