RT Journal Article
T1 Accuracy in Rietveld quantitative phase analysis: a comparative study of strictly monochromatic Mo and Cu radiations
A1 León-Reina, Laura
A1 García-Maté, Marta
A1 Álvarez-Pinazo, Gema
A1 Santacruz-Cruz, María Isabel
A1 Vallcorba, Oriol
A1 Gómez-de-la-Torre, María de los  Ángeles
A1 García-Aranda, Miguel Ángel
K1 Rietveld, Método de
K1 Cristalografía
AB This study reports 78 Rietveld quantitative phase analyses using Cu K 1,Mo K 1 and synchrotron radiations. Synchrotron powder diffraction has beenused to validate the most challenging analyses. From the results for three serieswith increasing contents of an analyte (an inorganic crystalline phase, an organiccrystalline phase and a glass), it is inferred that Rietveld analyses from highenergyMo K 1 radiation have slightly better accuracies than those obtainedfrom Cu K 1 radiation. This behaviour has been established from the results ofthe calibration graphics obtained through the spiking method and also fromKullback–Leibler distance statistic studies. This outcome is explained, in spite ofthe lower diffraction power for Mo radiation when compared to Cu radiation, asarising because of the larger volume tested with Mo and also because higherenergy allows one to record patterns with fewer systematic errors. The limit ofdetection (LoD) and limit of quantification (LoQ) have also been establishedfor the studied series. For similar recording times, the LoDs in Cu patterns, 0.2 wt%, are slightly lower than those derived from Mo patterns,  0.3 wt%.The LoQ for a well crystallized inorganic phase using laboratory powderdiffraction was established to be close to 0.10 wt% in stable fits with goodprecision. However, the accuracy of these analyses was poor with relative errorsnear to 100%. Only contents higher than 1.0 wt% yielded analyses with relativeerrors lower than 20%.
PB Willey online Library
SN 1600-5767
YR 2016
FD 2016
LK http://hdl.handle.net/10630/13621
UL http://hdl.handle.net/10630/13621
LA eng
NO J. Appl. Cryst. (2016). 49, 722–735
NO This work has been supported by Spanish MINECO throughthe BIA2014-57658-C2-2-R, which is co-funded by  FEDER, and BIA2014-57658-C2-1-R research grants. Funding from Junta de Andalucı´a, grant P11-FQM-07517, is also acknowl- edged. We thank CELLS-ALBA (Barcelona, Spain) for providing synchrotron beam time at the  BL04-MSPD  beam- line. This work is part of the commissioning of the Mo Ka1 powder diffractometer that was installed in June 2014 at University of Malaga (Spain). We  thank  one  referee  for  his/ her enlightened comments which have improved the quality ofthe manuscript.
DS RIUMA. Repositorio Institucional de la Universidad de Málaga
RD 20 ene 2026