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 3.10.3.2. Cu 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

3.10.3.2. Cu Kα1 laboratory X-ray powder diffraction (LXRPD)

| top | pdf |

Cu Kα1 powder patterns for exactly the same samples were recorded in reflection geometry (θ/2θ) on a X′Pert MPD PRO (PANalytical B.V.) diffractometer (240 mm radius) equipped with a Ge(111) primary monochromator, which gives monochromatic Cu radiation (λ = 1.54059 Å). The X-ray tube was operated at 45 kV and 40 mA. The optics configuration was a fixed divergence slit (0.5°), a fixed incident anti-scatter slit (1°), a fixed diffracted anti-scatter slit (0.5°) and an X′Celerator RTMS (real-time multiple strip) detector operating in scanning mode with the maximum active length. Using these conditions, the samples were measured between 6.5 and 81.5° 2θ with a step size of 0.0167° and a total measurement time of 2 h 36 min. The flat samples were prepared by rear charge of a flat sample holder in order to minimize preferred orientation and were rotated at a rate of 10 revolutions per minute.

The lowest analyte content samples, CGpQ_0.12A and GFL_0.12X, were measured three times using both radiations, Mo Kα1 and Cu Kα1, for a precision (reproducibility) assessment. Therefore, regrinding and reloading of the mixtures in the sample holder was carried out prior to every measurement.








































to end of page
to top of page