A new method for quantitative phase analysis using X-ray powder diffraction: direct derivation of weight fractions from observed integrated intensities and chemical compositions of individual phases

2016 ◽  
Vol 49 (5) ◽  
pp. 1508-1516 ◽  
Author(s):  
Hideo Toraya
Keyword(s):  
Phase Analysis ◽  
Powder Diffraction ◽  
Volume Fraction ◽  
Quantitative Phase Analysis ◽  
Chemical Compositions ◽  
Chemical Formula ◽  
X Ray ◽  
Quantitative Phase ◽  
Integrated Intensity ◽  
The Individual

A new method for the quantitative phase analysis of multi-component polycrystalline materials using the X-ray powder diffraction technique is proposed. A formula for calculating weight fractions of individual crystalline phases has been derived from the intensity formula for powder diffraction in Bragg–Brentano geometry. The integrated intensity of a diffraction line is proportional to the volume fraction of a relevant crystalline phase in an irradiated sample, and the volume fraction, when it is multiplied with the chemical formula weight, can be related to the weight fraction. The structure-factor-related quantity in the intensity formula, when it is summed in an adequate 2θ range, can be replaced with the sum of squared numbers of electrons belonging to composing atoms in the chemical formula. Unit-cell volumes and the number of chemical formula units are all cancelled out in the formula. Therefore, the formula requires only single-measurement integrated intensity datasets for the individual phases and their chemical compositions. No standard reference material, reference intensity ratio or crystal structure parameter is required. A new procedure for partitioning the intensities of unresolved overlapped diffraction lines has also been proposed. It is an iterative procedure which starts from derived weight fractions, converts the weight fractions to volume fractions by utilizing additional information on material densities, and then partitions the intensities in proportion to the volume fractions. Use of the Pawley pattern decomposition method provides more accurate intensity datasets than the individual profile fitting technique, and it expands the applicability of the present method to more complex powder diffraction patterns. Test results using weighed mixture samples showed that the accuracy, evaluated by the root-mean-square error, is comparable to that obtained by Rietveld quantitative phase analysis.

scholarly journals Quantitative Phase Analysis by X-ray Diffraction—Doping Methods and Applications

Crystals ◽  
2020 ◽  
Vol 10 (1) ◽  
pp. 27 ◽  
Author(s):  
Stanko Popović
Keyword(s):  
Quantitative Analysis ◽  
Phase Analysis ◽  
Powder Diffraction ◽  
Phase Fraction ◽  
Quantitative Phase Analysis ◽  
Intermetallic Alloys ◽  
X Ray Diffraction ◽  
X Ray ◽  
Quantitative Phase

X-ray powder diffraction is an ideal technique for the quantitative analysis of a multiphase sample. The intensities of diffraction lines of a phase in a multiphase sample are proportional to the phase fraction and the quantitative analysis can be obtained if the correction for the absorption of X-rays in the sample is performed. Simple procedures of quantitative X-ray diffraction phase analysis of a multiphase sample are presented. The matrix-flushing method, with the application of reference intensities, yields the relationship between the intensity and phase fraction free from the absorption effect, thus, shunting calibration curves or internal standard procedures. Special attention is paid to the doping methods: (i) simultaneous determination of the fractions of several phases using a single doping and (ii) determination of the fraction of the dominant phase. The conditions to minimize systematic errors are discussed. The problem of overlapping of diffraction lines can be overcome by combining the doping method (i) and the individual profile fitting method, thus performing the quantitative phase analysis without the reference to structural models of particular phases. Recent suggestions in quantitative phase analysis are quoted, e.g., in study of the decomposition of supersaturated solid solutions—intermetallic alloys. Round Robin on Quantitative Phase Analysis, organized by the IUCr Commission on Powder Diffraction, is discussed shortly. The doping methods have been applied in various studies, e.g., phase transitions in titanium dioxide, biomineralization processes, and phases in intermetallic oxide systems and intermetallic alloys.

scholarly journals Evaluation via multivariate techniques of scale factor variability in the rietveld method applied to quantitative phase analysis with X ray powder diffraction

2006 ◽  
Vol 9 (4) ◽  
pp. 369-374 ◽  
Author(s):  
Terezinha Ferreira de Oliveira ◽  
Roberto Ribeiro de Avillez ◽  
Eugenio Kahn Epprecht ◽  
Joaquim Carlos Barbosa Queiroz
Keyword(s):  
Phase Analysis ◽  
Powder Diffraction ◽  
Rietveld Method ◽  
Scale Factor ◽  
Quantitative Phase Analysis ◽  
Multivariate Techniques ◽  
X Ray ◽  
Quantitative Phase

scholarly journals Method of calculating the coherent scattering power of crystals with unknown atomic arrangements and its application in the quantitative phase analysis

2022 ◽  
pp. 1-6
Author(s):  
Hui Li ◽  
Meng He ◽  
Ze Zhang
Keyword(s):  
Phase Analysis ◽  
Powder Diffraction ◽  
Coherent Scattering ◽  
Unit Cell ◽  
Quantitative Phase Analysis ◽  
X Ray ◽  
Cell Parameters ◽  
Quantitative Phase ◽  
Structure Factors ◽  
Component Phase

Quantitative phase analysis is one of the major applications of X-ray powder diffraction. The essential principle of quantitative phase analysis is that the diffraction intensity of a component phase in a mixture is proportional to its abundance. Nevertheless, the diffraction intensities of the component phases cannot be compared with each other directly since the coherent scattering power per unit cell (or chemical formula) of each component phase is usually different. The coherent scattering power per unit cell of a crystal is well represented by the sum of the squared structure factors, which cannot be calculated directly when the crystal structure data is unavailable. Presented here is a way to approximate the coherent scattering power per unit cell based solely on the unit cell parameters and the chemical contents. This approximation is useful when the atomic coordinates for one or more of the phases in a sample are unavailable. An assessment of the accuracy of the approximation is presented. This assessment indicates that the approximation will likely be within 10% when X-ray powder diffraction data is collected over a sufficient portion of the measurable pattern.

Quantitative Phase Analyses of a Slag Using X-Ray Powder Diffraction

2014 ◽  
Vol 881-883 ◽  
pp. 1241-1244
Author(s):  
Wei Jin Zeng ◽  
Chao Zeng ◽  
Wei He
Keyword(s):  
Quantitative Analysis ◽  
Phase Analysis ◽  
Powder Diffraction ◽  
Rietveld Method ◽  
Quantitative Phase Analysis ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Quantitative Phase ◽  
Full Profile ◽  
Qualitative Phase

The quantitative phase analyses of a slag have been successfully carried out by using both of the full-profile Rietveld and RIR methods from X-ray powder diffraction data. The qualitative phase analysis indicates that the slag contains mayenite (CaO)12(Al2O3)7, olivine Ca2(SiO4), gehlenite Ca2Al (AlSiO7), lemite Ca2(SiO4) and hibonite CaO(Al2O3)6. The quantitative analysis from Rietveld refinement shows that the weight concentrations of mayenite, olivine, gehlenite, lemite and hibonite for the slag are 48.8(4) wt.%, 32.2(5) wt.%, 11.0(9) wt.%, 6.2(1.1) wt.% and 1.8 (1.2) wt.%, respectively. The quantitative phase analysis results obtained by Rietveld method are more precise then those by RIR method.

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