22 September 1999 Synchrotron x-ray microtomography and solid state NMR of environmental wastes in cement
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Synchrotron X-ray microtomography shows vesicular structures for toluene/cement mixtures prepared with 1.22 to 3.58 wt% toluene. Three-dimensional imaging of the cured samples shows spherical vesicles with diameters ranging from 20 to 250 microns; a search with electron microscopy for vesicles in the range of 1 - 20 microns proved negative. However, the total vesicle volume, as computed from the microtomography images, accounts for less than 10% of initial toluene. Evidence for toluene in the cement matrix comes from 29Si MAS NMR spectroscopy, which shows a reduction in chain silicates with added toluene. Also, 2H NMR of d8-toluene/cement samples shows high mobility for all toluene and thus no toluene/cement binding. A model that accounts for all observations follows: For loadings below about 3 wt%, most toluene is dispersed in the cement matrix, with a small fraction of the initial toluene phase separating from the cement paste and forming vesicular structures that are preserved in the cured cement. Furthermore, at loadings above 3 wt%, the abundance of vesicles formed during toluene/cement paste mixing leads to macroscopic phase separation.
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Leslie G. Butler, Frank K. Cartledge, John W. Owens, Betsy A. Dowd, "Synchrotron x-ray microtomography and solid state NMR of environmental wastes in cement", Proc. SPIE 3772, Developments in X-Ray Tomography II, (22 September 1999); doi: 10.1117/12.363711; https://doi.org/10.1117/12.363711

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