International
Tables for
Crystallography
Volume H
Powder diffraction
Edited by C. J. Gilmore, J. A. Kaduk and H. Schenk

International Tables for Crystallography (2018). Vol. H, ch. 3.10, p. 376

Section 3.10.3.1. Mo Kα1 laboratory X-ray powder diffraction (LXRPD)

L. León-Reina,a A. Cuesta,b M. García-Maté,c,d G. Álvarez-Pinazo,c,d I. Santacruz,c O. Vallcorba,b A. G. De la Torrec and M. A. G. Arandab,c*

aServicios Centrales de Apoyo a la Investigación, Universidad de Málaga, 29071 Málaga, Spain,bALBA Synchrotron, Carrer de la Llum 2–26, Cerdanyola, 08290 Barcelona, Spain,cDepartamento de Química Inorgánica, Cristalografía y Mineralogía, Universidad de Málaga, 29071 Málaga, Spain, and dX-Ray Data Services S.L., Edificio de institutos universitarios, c/ Severo Ochoa 4, Parque tecnológico de Andalucía, 29590 Málaga, Spain
Correspondence e-mail:  g_aranda@uma.es

3.10.3.1. Mo Kα1 laboratory X-ray powder diffraction (LXRPD)

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Mo Kα1 powder patterns were collected in transmission geometry in constant irradiated volume mode, in order to avoid any correction of the measured intensities, on a D8 ADVANCE (Bruker AXS) diffractometer (188.5 mm radius) equipped with a Ge(111) primary monochromator, which gives monochromatic Mo radiation (λ = 0.7093 Å). The X-ray tube operated at 50 kV and 50 mA. The optics configuration was a fixed divergence slit (2°) and a fixed diffracted anti-scatter slit (9°). A LYNXEYE XE 500 µm energy-dispersive linear detector, optimized for high-energy radiation, was used with the maximum opening angle. Using these conditions, the samples were measured between 3 and 35° 2θ with a step size of 0.006° and with a total measurement time of 3 h 5 min. The flat samples were placed into cylindrical holders between two Kapton foils (Cuesta et al., 2015[link]) and rotated at a rate of 10 revolutions per minute during data collection. Moreover, the absorption factor of each sample was experimentally measured by comparing the direct beam with and without the sample (Cuesta et al., 2015[link]). The amount of sample loaded (which determines the height of the cylinder) in the holders was adjusted to obtain a total absorption (μt) of ∼1, which corresponds to an absorption factor of ∼2.7 or 63% of direct-beam attenuation. For the organic samples this criterion was not followed as it would lead to very thick specimens. In this case, the maximum holder thickness was used (1.7 mm).

References

Cuesta, A., Álvarez-Pinazo, G., García-Maté, M., Santacruz, I., Aranda, M. A. G., De la Torre, Á. G. & León-Reina, L. (2015). Rietveld quantitative phase analysis with molybdenum radiation. Powder Diffr. 30, 25–35.Google Scholar








































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