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Accuracy in Rietveld quantitative phase analysis with strictly monochromatic Mo and Cu radiations
International Tables for Crystallography (2018). Vol. H, ch. 3.10, pp. 374-384 [ doi:10.1107/97809553602060000955 ]
... based on an article Accuracy in Rietveld quantitative phase analysis: a comparative study of strictly monochromatic Mo and Cu radiations by ... of an analyte (inorganic crystalline phases, organic crystalline phases and a glass), it is inferred that Rietveld analyses from high-energy ... those derived from Mo patterns (~0.3wt%). The LoQ for a well crystallized inorganic phase using laboratory powder diffraction was ...
Increasing amorphous content series within an inorganic crystalline phase matrix
International Tables for Crystallography (2018). Vol. H, Section 3.10.9, pp. 382-383 [ doi:10.1107/97809553602060000955 ]
... employed phases. Hence, we used the SXRPD data to calculate a correction factor for quartz to yield zero amorphous content for ... powder patterns for the amorphous-material-containing series composed of a constant matrix of calcite and zincite, and increasing amounts of ground glass. Quartz was added as internal standard. (a) MoK[alpha]1, (b) CuK[alpha]1 and (c) ...
Increasing crystalline organic phase content series
International Tables for Crystallography (2018). Vol. H, Section 3.10.8, pp. 381-382 [ doi:10.1107/97809553602060000955 ]
... Table 3.10.3 shows RQPA results for six mixtures prepared with G, F, L and an increasing amount of X measured with ... wt% Mo trm Cu rfl wt% Mo trm Cu rfl G 33.4 33.8 (1) 33.5 (3) 33.3 33.6 (1) 33.1 (2 ... wt% Mo trm Cu rfl wt% Mo trm Cu rfl G 33.0 34.7 (1) 33.6 (2) 32.7 32.2 (1) 31.5 ( ...
Increasing inorganic crystalline phase content series
International Tables for Crystallography (2018). Vol. H, Section 3.10.7, p. 381 [ doi:10.1107/97809553602060000955 ]
... results for six inorganic mixtures with increasing amounts of i-A measured with MoK[alpha]1 (transmission) and CuK[alpha]1 ... . The Rietveld plots of the mixture with 4wt% i-A are shown in Fig. 3.10.6 . For most of the ... 33.9 (1) 33.0 (1) 34.0 34.6 (1) 34.2 (1) s-A 0.8 0.66 (3) 0.76 (5) 0.8 0.77 (4) 0.78 ( ...
Limits of detection and quantification
International Tables for Crystallography (2018). Vol. H, Section 3.10.6, pp. 379-381 [ doi:10.1107/97809553602060000955 ]
... In techniques such as Rietveld analysis, the approach of having a powder pattern with its strongest (not overlapped) diffraction peak with ... and Fig. 3.10.4 shows the strongest diffraction peak for i-A in the mixtures containing 0.123wt% anhydrite (CGpQ_0.12A) and 0.25wt ... . For CGpQ_0.25A, the CuK[alpha]1 pattern yielded a clear peak with S/N = 4.1; therefore, it can ...
Crystalline single phases
International Tables for Crystallography (2018). Vol. H, Section 3.10.5, pp. 377-379 [ doi:10.1107/97809553602060000955 ]
... using CuK[alpha]1 radiation in reflection mode. As expected, a transparency effect was observed in the CuK[alpha]1 patterns ... Buhrke, V. E., Jenkins, R. & Smith, D. K. (1998). A Practical Guide for the Preparation of Specimens for X-ray ... Diffraction Analysis. New York: Wiley.GoogleScholar León-Reina, L., García-Maté, M., Álvarez-Pinazo, G., Santacruz, I., Vallcorba, O., ...
Powder-diffraction data analysis
International Tables for Crystallography (2018). Vol. H, Section 3.10.4, p. 377 [ doi:10.1107/97809553602060000955 ]
... are reported in Table 3.10.1 . In order to provide a single numerical assessment of the performance of each analysis, a statistic based on the KLD distance was used (Kullback, 1968 ... internal standard methodology approach (De la Torre et al., 2001 ; Aranda et al., 2012 ) with quartz as an internal standard [ ...
Transmission synchrotron X-ray powder diffraction (SXRPD)
International Tables for Crystallography (2018). Vol. H, Section 3.10.3.3, pp. 376-377 [ doi:10.1107/97809553602060000955 ]
... 2013 ). The wavelength, [lambda] = 0.77439(2)Å, was selected with a double-crystal Si(111) monochromator and was determined using the NIST SRM640d Si standard (a = 5.43123Å). The diffractometer is equipped with a MYTHEN-II detector system. The samples were loaded into ...
[more results from section 3.10.3 in volume H]
Variable amorphous content series
International Tables for Crystallography (2018). Vol. H, Section 3.10.2.4, pp. 375-376 [ doi:10.1107/97809553602060000955 ]
Variable amorphous content series 3.10.2.4. Variable amorphous content series A constant matrix of calcite (C) and zincite (Z) was prepared. ... elemental composition of the ground glass is given in García-Maté et al. (2014) . The mixtures were labelled CZQ ... adding ~20wt% quartz (Q) as an internal standard. References García-Maté, M., Santacruz, I., Cuesta, A., León-Reina, ...
[more results from section 3.10.2 in volume H]
Introduction
International Tables for Crystallography (2018). Vol. H, Section 3.10.1, pp. 374-375 [ doi:10.1107/97809553602060000955 ]
... iii) data-analysis protocol(s). The Rietveld method is a standardless methodology which uses the crystal-structure descriptions of each ... minimize absorption and microabsorption effects, (ii) to the measurement of a higher number of Bragg peaks and (iii) to increase the irradiated volume of the specimen. Figs. 3.10.1 (a) and 3.10.1 (b) show the irradiated volumes bathed by ...
International Tables for Crystallography (2018). Vol. H, ch. 3.10, pp. 374-384 [ doi:10.1107/97809553602060000955 ]
... based on an article Accuracy in Rietveld quantitative phase analysis: a comparative study of strictly monochromatic Mo and Cu radiations by ... of an analyte (inorganic crystalline phases, organic crystalline phases and a glass), it is inferred that Rietveld analyses from high-energy ... those derived from Mo patterns (~0.3wt%). The LoQ for a well crystallized inorganic phase using laboratory powder diffraction was ...
Increasing amorphous content series within an inorganic crystalline phase matrix
International Tables for Crystallography (2018). Vol. H, Section 3.10.9, pp. 382-383 [ doi:10.1107/97809553602060000955 ]
... employed phases. Hence, we used the SXRPD data to calculate a correction factor for quartz to yield zero amorphous content for ... powder patterns for the amorphous-material-containing series composed of a constant matrix of calcite and zincite, and increasing amounts of ground glass. Quartz was added as internal standard. (a) MoK[alpha]1, (b) CuK[alpha]1 and (c) ...
Increasing crystalline organic phase content series
International Tables for Crystallography (2018). Vol. H, Section 3.10.8, pp. 381-382 [ doi:10.1107/97809553602060000955 ]
... Table 3.10.3 shows RQPA results for six mixtures prepared with G, F, L and an increasing amount of X measured with ... wt% Mo trm Cu rfl wt% Mo trm Cu rfl G 33.4 33.8 (1) 33.5 (3) 33.3 33.6 (1) 33.1 (2 ... wt% Mo trm Cu rfl wt% Mo trm Cu rfl G 33.0 34.7 (1) 33.6 (2) 32.7 32.2 (1) 31.5 ( ...
Increasing inorganic crystalline phase content series
International Tables for Crystallography (2018). Vol. H, Section 3.10.7, p. 381 [ doi:10.1107/97809553602060000955 ]
... results for six inorganic mixtures with increasing amounts of i-A measured with MoK[alpha]1 (transmission) and CuK[alpha]1 ... . The Rietveld plots of the mixture with 4wt% i-A are shown in Fig. 3.10.6 . For most of the ... 33.9 (1) 33.0 (1) 34.0 34.6 (1) 34.2 (1) s-A 0.8 0.66 (3) 0.76 (5) 0.8 0.77 (4) 0.78 ( ...
Limits of detection and quantification
International Tables for Crystallography (2018). Vol. H, Section 3.10.6, pp. 379-381 [ doi:10.1107/97809553602060000955 ]
... In techniques such as Rietveld analysis, the approach of having a powder pattern with its strongest (not overlapped) diffraction peak with ... and Fig. 3.10.4 shows the strongest diffraction peak for i-A in the mixtures containing 0.123wt% anhydrite (CGpQ_0.12A) and 0.25wt ... . For CGpQ_0.25A, the CuK[alpha]1 pattern yielded a clear peak with S/N = 4.1; therefore, it can ...
Crystalline single phases
International Tables for Crystallography (2018). Vol. H, Section 3.10.5, pp. 377-379 [ doi:10.1107/97809553602060000955 ]
... using CuK[alpha]1 radiation in reflection mode. As expected, a transparency effect was observed in the CuK[alpha]1 patterns ... Buhrke, V. E., Jenkins, R. & Smith, D. K. (1998). A Practical Guide for the Preparation of Specimens for X-ray ... Diffraction Analysis. New York: Wiley.GoogleScholar León-Reina, L., García-Maté, M., Álvarez-Pinazo, G., Santacruz, I., Vallcorba, O., ...
Powder-diffraction data analysis
International Tables for Crystallography (2018). Vol. H, Section 3.10.4, p. 377 [ doi:10.1107/97809553602060000955 ]
... are reported in Table 3.10.1 . In order to provide a single numerical assessment of the performance of each analysis, a statistic based on the KLD distance was used (Kullback, 1968 ... internal standard methodology approach (De la Torre et al., 2001 ; Aranda et al., 2012 ) with quartz as an internal standard [ ...
Transmission synchrotron X-ray powder diffraction (SXRPD)
International Tables for Crystallography (2018). Vol. H, Section 3.10.3.3, pp. 376-377 [ doi:10.1107/97809553602060000955 ]
... 2013 ). The wavelength, [lambda] = 0.77439(2)Å, was selected with a double-crystal Si(111) monochromator and was determined using the NIST SRM640d Si standard (a = 5.43123Å). The diffractometer is equipped with a MYTHEN-II detector system. The samples were loaded into ...
[more results from section 3.10.3 in volume H]
Variable amorphous content series
International Tables for Crystallography (2018). Vol. H, Section 3.10.2.4, pp. 375-376 [ doi:10.1107/97809553602060000955 ]
Variable amorphous content series 3.10.2.4. Variable amorphous content series A constant matrix of calcite (C) and zincite (Z) was prepared. ... elemental composition of the ground glass is given in García-Maté et al. (2014) . The mixtures were labelled CZQ ... adding ~20wt% quartz (Q) as an internal standard. References García-Maté, M., Santacruz, I., Cuesta, A., León-Reina, ...
[more results from section 3.10.2 in volume H]
Introduction
International Tables for Crystallography (2018). Vol. H, Section 3.10.1, pp. 374-375 [ doi:10.1107/97809553602060000955 ]
... iii) data-analysis protocol(s). The Rietveld method is a standardless methodology which uses the crystal-structure descriptions of each ... minimize absorption and microabsorption effects, (ii) to the measurement of a higher number of Bragg peaks and (iii) to increase the irradiated volume of the specimen. Figs. 3.10.1 (a) and 3.10.1 (b) show the irradiated volumes bathed by ...
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