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dc.contributor.authorLeón-Reina, Laura
dc.contributor.authorGarcía-Maté, Marta
dc.contributor.authorÁlvarez-Pinazo, Gema
dc.contributor.authorSantacruz-Cruz, Maria Isabel 
dc.contributor.authorVallcorba, Oriol
dc.contributor.authorDe la Torre, Angeles G.
dc.contributor.authorAranda, Miguel A. G.
dc.date.accessioned2017-05-11T11:22:20Z
dc.date.available2017-05-11T11:22:20Z
dc.date.issued2016
dc.identifier.citationJ. Appl. Cryst. (2016). 49, 722–735es_ES
dc.identifier.issn1600-5767
dc.identifier.urihttp://hdl.handle.net/10630/13621
dc.description.abstractThis study reports 78 Rietveld quantitative phase analyses using Cu K 1, Mo K 1 and synchrotron radiations. Synchrotron powder diffraction has been used to validate the most challenging analyses. From the results for three series with increasing contents of an analyte (an inorganic crystalline phase, an organic crystalline phase and a glass), it is inferred that Rietveld analyses from highenergy Mo K 1 radiation have slightly better accuracies than those obtained from Cu K 1 radiation. This behaviour has been established from the results of the calibration graphics obtained through the spiking method and also from Kullback–Leibler distance statistic studies. This outcome is explained, in spite of the lower diffraction power for Mo radiation when compared to Cu radiation, as arising because of the larger volume tested with Mo and also because higher energy allows one to record patterns with fewer systematic errors. The limit of detection (LoD) and limit of quantification (LoQ) have also been established for 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 powder diffraction was established to be close to 0.10 wt% in stable fits with good precision. However, the accuracy of these analyses was poor with relative errors near to 100%. Only contents higher than 1.0 wt% yielded analyses with relative errors lower than 20%.es_ES
dc.description.sponsorshipThis work has been supported by Spanish MINECO through the 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 of the manuscript.es_ES
dc.language.isoenges_ES
dc.publisherWilley online Libraryes_ES
dc.rightsinfo:eu-repo/semantics/openAccesses_ES
dc.subjectRietveld, Método dees_ES
dc.subjectCristalografíaes_ES
dc.subject.otherLimit of quantificationes_ES
dc.subject.otherSpiking methodes_ES
dc.subject.otherHigh-energy laboratory X-ray powder diffractiones_ES
dc.titleAccuracy in Rietveld quantitative phase analysis: a comparative study of strictly monochromatic Mo and Cu radiationses_ES
dc.typeinfo:eu-repo/semantics/articlees_ES
dc.centroFacultad de Cienciases_ES
dc.cclicenseby-nc-ndes_ES


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