Abstract
Analysis of microcrystalline cellulose (MCC) PH-101, ciprofloxacin (CIP) and quantitative phase analysis of predetermined mixtures of CIP/MCC were performed by the Rietveld method with a physically based background. Correction factors for absorption and air scattering under a symmetrical reflection geometry with a given sample thickness, divergence and receiving slit width, scale factors, average temperature factors and specimen density of packing, were considered to model the background. By this way, the whole diffraction pattern was evaluated on a physical basis, considering the Bragg and the diffuse scattering (thermal diffuse scattering plus static disorder, Compton and air scattering) using a Python code. Compton scattering was also corrected for the bandpass function of the monochromator. Quantitative phase analysis is discussed on the scope of the results obtained. The maximum absolute difference in the weight% composition obtained was of 3.4% in the CIP/MCC mixtures.
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Acknowledgments
The authors acknowledge Prof. Xim Bokhimi, Antonio Morales Espino and Alejandro Herrera from LAREC laboratory at IF-UNAM for the XRD facilities as well as the financial support from the graduate program in Materials Science (PCeIM-UNAM) and DGAPA-PAPIIT project IN-110918. B. Ramírez acknowledges CONACYT for a PhD grant. The valuable collaboration of Prof. Sandra García Medina (ENCB-IPN), Octavio Graniel, Samuel Tehuacanero C., J. Eduardo L. Barriguete are gratefully appreciated. The authors thank Editor-in-Chief Alfred French and the anonymous reviewers for their helpful comments on this paper.
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Ramírez, B., Bucio, L. Microcrystalline cellulose (MCC) analysis and quantitative phase analysis of ciprofloxacin/MCC mixtures by Rietveld XRD refinement with physically based background. Cellulose 25, 2795–2815 (2018). https://doi.org/10.1007/s10570-018-1761-z
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DOI: https://doi.org/10.1007/s10570-018-1761-z