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15444360726
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note
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2 precipitates at pH = 8.0 and when dried in air is brown. After calcination, the color changed to black. After addition of CTAB aqueous solution of pH 7.0, the pH of the mixture was 6.0.
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26
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15444350869
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note
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6 groups due to changes in mixed valency during calcination of MOMS-2 may lead to the observed enhanced ordering. The XRD baselines were flat, and there were no sharp peaks in the XRD patterns of MOMS-1 or MOMS-2 from impure dense-phase crystalline manganese oxides. The HRTEM data [Philips CM 200 FEG (Super Twin-α Objective lens) operated at 200 kV; images were taken at a magnification of 580,000 and enlarged 2.87 times] were collected on calcined samples dispersed in acetone, which were supported on a holy carbon grid. A Bruker Electron Spin Resonance ESP 300 spectrometer was used to obtain EPR spectra, which show a hyperfine splitting of six lines centered at 3300 G that are separated by 92.8 G for calcined samples at 4.2 K, indicative of octahedral symmetry.
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27
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15444351096
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note
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-1. Omnisorp 100 CX and Cahn 2000 Microbalance instruments were used to determine surface areas and pore-size distributions. A static sorption vacuum system with a homemade quartz in situ cell with KBr windows was used for pyridine adsorption experiments on calcined samples. A Nicolet 750 FTIR spectrometer was used for diffusereflectance FTIR experiments.
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A Fell four-probe head combined with a Keithley 224 Programmable Current Source and a voltmeter were used to measure the conductivities of pressed sample pellets [L. Van der Pauw, J. Phillips Res. Rep. 13, 1 (1958)]. The band gaps were calculated from powder UV-Vis spectra [A. R. West, Solid State Chemistry and Its Applications (Wiley, New York, 1984), pp. 75-78] collected on a Hewlett-Packard 8452A Diode Array Spectrophotometer equipped with a Labshere RSA-HP-84 Reflectance Spectroscopy Accessory.
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A Fell four-probe head combined with a Keithley 224 Programmable Current Source and a voltmeter were used to measure the conductivities of pressed sample pellets [L. Van der Pauw, J. Phillips Res. Rep. 13, 1 (1958)]. The band gaps were calculated from powder UV-Vis spectra [A. R. West, Solid State Chemistry and Its Applications (Wiley, New York, 1984), pp. 75-78] collected on a Hewlett-Packard 8452A Diode Array Spectrophotometer equipped with a Labshere RSA-HP-84 Reflectance Spectroscopy Accessory.
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15444353553
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note
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The reactions were carried out under reflux for 40 hours in aqueous solutions with stirring at 75°C. The reaction mixture contained 1.8 g of cyclohexane or n-hexane, 2.0 g of tert-butyl hydrogen peroxide (70% aqueous solution), 2.5 g of tert-butyl alcohol, 70 mg of calcined mesoporous material, and 0.1 g of acetophenone. The acetophenone (1.0 g, internal standard) was mixed with 25.0 g of tert-butyl alcohol before it was added to the reactants. The reaction mixtures were analyzed by gas chromatography (GC) [HP-5890 GC equipped with a Supelcowax 10 fused silica column].
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15444351838
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note
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We acknowledge helpful discussions with M. E. Davis, A. Clearfield, C. T. Kresge, T. J. Pinnavaia, and G. D. Stucky. V. Chynwat is acknowledged for assistance with EPR experiments. We thank Y. Feng of Philips Electronic Instruments for help with HRTEM experiments. We acknowledge the U.S. Department of Energy, Office of Basic Energy Sciences, Division of Chemical Sciences, for support of this research.
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