Untitled - Technische Universiteit Eindhoven

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2.4. Results and discussion 290.0950 mT/m100 mT/m200 mT/m0.080.07T 2[s]0.060.050.042 4 6 8time [h]Fig. 2.13: Detail of the dominant T 2 component in the aqueous phase as a function of timefor the experiment with initial TMOS fraction 0.4 and temperature 25 ◦ C. The T 2was measured using three different read-out gradient strengths as indicated in thelegend. The lines in the graph indicate the construction used to find the time atwhich the T 2 reaches a plateau.400350300test tube 40 vol%test tube 20 vol%NMR 40 vol%NMR 20 vol%gel time [min]25020015010050025 30 35 40 45 50T [°C]Fig. 2.14: Gel times for the bulk experiments obtained from the NMR and tilting test tubemeasurements. The initial TMOS concentration in the n-hexadecane is shown inthe legend. The error bars shown hold for all data sets.
30 2. Coupled mass transfer and sol-gel reaction in a two-phase bulk systemto find the points at which the minima occur. The resulting transition time (with anaccuracy of about 30 minutes) was subsequently compared to the gel times obtained fromthe tilting test tube experiments (as demonstrated in Figure 2.14). A good agreement isfound between the gel times and the times at which the minimum T 2 (or plateau) occurs.The leveling-off time in T 2 therefore appears to be an adequate indication for the geltransition time in these experiments.2.5 ConclusionIn binary mixtures of TMOS and n-hexadecane the longitudinal relaxation time T 1 increasesmonotonically with the concentration of TMOS and with temperature. The measurementof T 1 proves to be a robust method to determine concentrations in a non-intrusivemanner. The prepared gels showed a significant decrease in the transverse relaxation timeT 2 compared to either water, TMOS or methanol. The short T 2 component is related tothe water hydrogen nuclei, whereas the longer components can be attributed to methanol.The shortening of the water T 2 component is due to the interaction of water with methanol.An additional decrease of the relaxation times is caused by the geometrical confinementin the gel structure, and the interaction of the fluid with the silica surface.Through the measurement of T 1 the concentration of TMOS in n-hexadecane wasdetermined dynamically during the experiments with an accuracy of about 2 vol%. Boththe T 1 -weighed 2D images as the T 1 profiles revealed that the oleic and the aqueousphase were uniform in terms of T 1 at each time step measured during the reactive masstransfer. Significant concentration gradients were therefore not observed, which meansthat the mass transfer within each phase is enhanced by convective mixing, and is notdue to diffusion only. After the phases are brought in contact the average concentrationof TMOS in the oleic phase decreases exponentially. The rate is rather insensitive totemperature (within the range of 25–45 ◦ C), but is sensitive to the initial concentrationof TMOS. In case of an initial concentration of TMOS of 40 vol% the rate is at leasttwo times higher compared to the lower initial concentration of 20 vol%. The gel pointof the aqueous phase is indicated by the minimum (or plateau) in T 2 , which appearsafter several hours when the fluids are brought in contact. The gel time decreases withincreasing temperature and with increasing initial TMOS concentration.
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146 Appendix AThe 0.95 Tesla scanne
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148 Appendix B
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150 Appendix CwhereΩ A (θ) = −2
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152 Appendix C
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154 Appendix D
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156 Appendix Eand equal to zero in
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158 Appendix EAs the saturations, d
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160 Bibliography[12] B. Vinot, R. S
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162 Bibliography[40] M. D. Mantle a
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164 Bibliography[70] F. J. M. van d
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166 Bibliography[97] K. Yoshida, A.
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168 Bibliography[127] G. W. Scherer
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170 Bibliography
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172 Summaryand gelation rates. The
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174 Samenvattingwaterfase. De T 1 v
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176 List of publications
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178 Dankwoordimmer opgewekte stemmi
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Prior to the speech, Harald Cramér
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Untitled - Technische Universiteit Eindhoven

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