2026-06-01T19:49:10Zhttps://riuma.uma.es/rest/oai/request

oai:riuma.uma.es:10630/136212026-02-03T11:10:06Zcom_10630_2254col_10630_37953

Accuracy in Rietveld quantitative phase analysis: a comparative study of strictly monochromatic Mo and Cu radiations León-Reina, Laura García-Maté, Marta Álvarez-Pinazo, Gema Santacruz-Cruz, María Isabel Vallcorba, Oriol Gómez-de-la-Torre, María de los Ángeles García-Aranda, Miguel Ángel Rietveld, Método de Cristalografía This 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%. 2017-05-11T11:22:20Z 2017-05-11T11:22:20Z 2016 journal article J. Appl. Cryst. (2016). 49, 722–735 1600-5767 http://hdl.handle.net/10630/13621 eng open access by-nc-nd Willey online Library