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Diffusion NMR as a New Method for the Determination of the Gel Point of Gelatin

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Institute of Analytical Chemistry, University of Leipzig, Linnéstrasse 3, D-04103 Leipzig, Germany, and Physical Chemistry of Polymers, Dresden University of Technology, Mommsenstrasse 13, D-01062 Dresden, Germany
Cite this: J. Phys. Chem. B 2006, 110, 32, 15853–15857
Publication Date (Web):July 26, 2006
https://doi.org/10.1021/jp062960z
Copyright © 2006 American Chemical Society
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    Abstract

    The gelation of gelatin has been investigated using pulsed field gradient (PFG) NMR. For the first time, diffusion results have been used to determine the gelation point, which is indicated by a minimum in the self-diffusion coefficient of the free polymer fraction vs temperature. Biexponential analysis of the diffusion decay data allowing the diffusion of free and network-bound gelatin to be determined separately has been applied to provide an extended insight into the gelation process. Low-amplitude oscillatory shear rheology and time-resolved dynamic light scattering (DLS) as classical polymer characterization methods were applied as control experiments. All three methods yielded a gelation temperature of 24−25 °C for the cooling regime. Hysteresis effects could also be observed.

    †

     University of Leipzig.

    *

     To whom correspondence should be addressed. Phone:  (+49) 341-9736101. Fax:  (+49) 341-9736115. E-mail:  [email protected] (S.B.). Phone:  (+49) 351-46332492. Fax:  (+49) 351-46337122. E-mail:  [email protected] (S.R.).

    ‡

     Dresden University of Technology.

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    Figure S1 containing seven TCFs measured for the gelatin sample during the cooling regime in the temperature range from 35 to 23 °C. Figure S2 showing an example data set visualizing the diffusional decay as well as the integral regions used. Figure S3 displaying the temperature dependent diffusion behavior of the fast component according to eq 6. Figure S4 visualizing the relative signal contributions of the slow and fast components (see eq 6) for the cooling experiment. This material is available free of charge via the Internet at http://pubs.acs.org.

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