Polyhydroxy fullerenes |
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Authors: | Angelina T Georgieva Vijay Pappu Vijay Krishna Pando G Georgiev Ion Ghiviriga Paul Indeglia Xin Xu Z Hugh Fan Ben Koopman Panos M Pardalos Brij Moudgil |
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Institution: | 1. Department of Materials Science and Engineering, Particle Engineering Research Center, University of Florida, Gainesville, FL, USA 2. Center for Applied Optimization, University of Florida, Gainesville, FL, USA 3. NMR Facility, Department of Chemistry, University of Florida, Gainesville, FL, USA 6. Agency for Sustainable Systems in Science and Technology, Inc., P.O. Box 1636, Nashua, NH, 03061, USA 5. Department of Mechanical & Aerospace Engineering, University of Florida, Gainesville, FL, USA 4. Department of Environmental Engineering Sciences, University of Florida, Gainesville, FL, USA
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Abstract: | Characterization of C60 polyhydroxyfullerenes (PHF) prepared in alkaline media, preparation facilitated by phase-transfer catalyst, presents challenges in determining the chemical structure resulting from the possibility of multiple isomers or analogs with greater or fewer hydroxyl groups from a single reaction mixture. This paper presents the utilization of analytical methods employed in tandem, especially X-ray photoelectron spectroscopy, nuclear magnetic resonance spectroscopy, Fourier transform infrared spectroscopy for semi-quantitative analysis on the number of hydroxyl groups present in PHF. Capillary Electrophoresis was used for purity estimation of the material. Multiple spectra and electropherograms were analyzed using a new simultaneous curve fitting method. The most accurate estimate of hydroxyl groups for C60 polyhydroxy fullerenes obtained is between 16 and 18 allylic hydroxyl groups by combining analytical methods’ results with 5 % accuracy. High precision (reproducibility) of the experiments is observed. Purity of 98 % is estimated by capillary electrophoresis. The size of PHF nanoparticles or aggregates has been determined by atomic force microscopy to be 7.4–14.2 nm. According to the elemental analysis the average probable empirical formula for the most pure PHF at pH 7.1 is C60O17H12Na5(NaHCO3)3(H2O)13 and the average formula weight is 1,605.9 g/mol. This is the first thorough characterization of PHF in terms of purity. |
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