scholarly journals Quantitative phase analysis by X-ray diffraction – Simple routes

2015 ◽  
Vol 34 (1) ◽  
pp. 33 ◽  
Author(s):  
Stanko Popović
Keyword(s):  
Phase Analysis ◽  
Great Difficulty ◽  
Quantitative Phase Analysis ◽  
Spectroscopic Techniques ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multiphase Material ◽  
Ideal Technique

<p>        The elemental composition of a multiphase material can be obtained by means of chemical and spectroscopic techniques. However, these techniques face a great difficulty in distinguishing the chemical identity of the phases present in the material and in derivation of the fractions of particular phases. X-ray powder diffraction seems to be an ideal technique for the analysis of a multiphase material. Each crystalline phase of the material gives its characteristic diffraction pattern independently of the other phases; this fact makes it possible to identify the phase of interest and to determine its fraction. The intensities of diffraction lines of a given phase are proportional to its fraction and an appropriate quantitative analysis can be performed after the application of the correction for the absorption of X-rays in the material.</p><p class="IUCrfigurecaption">        The principles of quantitative X-ray diffraction phase analysis of a multiphase material are presented, with a special attention paid to the doping methods. The following methods are described: (<em>i</em>) determination of the fraction of a phase using repeated dopings, (<em>ii</em>) determination of the fraction of a phase using a single doping, (<em>iii</em>) simultaneous determination of the fractions of several phases using a single doping; (<em>iv</em>) determination of the fraction of the dominant phase. The applicability of the doping methods is stated and the optimum conditions to minimize systematic errors are discussed. Recent approaches in quantitative X-ray diffraction phase analysis are also mentioned in short.</p>

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 Electronic Excitations and Radiation Damage in Macromolecular Crystallography

Crystals ◽  
2018 ◽  
Vol 8 (7) ◽  
pp. 273 ◽  
Author(s):  
José Brandão-Neto ◽  
Leonardo Bernasconi
Keyword(s):  
Chemical Information ◽  
X Rays ◽  
Electronic Excitations ◽  
Macromolecular Crystallography ◽  
X Ray Diffraction ◽  
X Ray ◽  
Atomic Structures ◽  
Successful Approach ◽  
Structural Research

Macromolecular crystallography at cryogenic temperatures has so far provided the majority of the experimental evidence that underpins the determination of the atomic structures of proteins and other biomolecular assemblies by means of single crystal X-ray diffraction experiments. One of the core limitations of the current methods is that crystal samples degrade as they are subject to X-rays, and two broad groups of effects are observed: global and specific damage. While the currently successful approach is to operate outside the range where global damage is observed, specific damage is not well understood and may lead to poor interpretation of the chemistry and biology of the system under study. In this work, we present a phenomenological model in which specific damage is understood as the result of a single process, the steady excitation of crystal electrons caused by X-ray absorption, which acts as a trigger for the bulk effects that manifest themselves in the form of global damage and obscure the interpretation of chemical information from XFEL and synchrotron structural research.

A Method for Quantitative Phase Analysis of Silicon Nitride by X-Ray Diffraction

1990 ◽  
Vol 5 (3) ◽  
pp. 121-124 ◽  
Author(s):  
David J. Devlin ◽  
Kamal E. Amin
Keyword(s):  
Silicon Nitride ◽  
Iterative Method ◽  
Calibration Curve ◽  
Quantitative Measurement ◽  
Quantitative Phase Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pure Phases ◽  
Yttrium Disilicate

AbstractThe relative intensities ratios for the determination of the relative amounts of alpha and beta phases in silicon nitride and the relative amounts of delta yttrium disilicate (Y2Si2O7) and nitrogen apatite [Y5(SiO4)3N] are reported. These constants were determined using an iterative method applicable when the pure phases are not easily prepared. In addition, a calibration curve was obtained for the quantitative measurement of free silicon in silicon nitride over the range 0 to 0.3% by weight of Si.

scholarly journals Electronic Excitations and Radiation Damage in Macromolecular Crystallography

2018 ◽  
Author(s):  
José Brandão-Neto ◽  
Leonardo Bernasconi
Keyword(s):  
Chemical Information ◽  
X Rays ◽  
Electronic Excitations ◽  
Macromolecular Crystallography ◽  
X Ray Diffraction ◽  
X Ray ◽  
Atomic Structures ◽  
Successful Approach ◽  
Structural Research

Macromolecular crystallography at cryogenic temperatures has so far provided the majority of the experimental evidence that underpins the determination of the atomic structures of proteins and other biomolecular assemblies by means of single crystal X-ray diffraction experiments. One of the core limitations of the current methods is that crystal samples degrade as they are subject to X-rays, and two broad groups of effects are observed: global and specific damage. While the currently successful approach is to operate outside the range where global damage is observed, specific damage is not well understood and may lead to poor interpretation of the chemistry and biology of the system under study. In this work, we present a phenomenological model in which specific damage is understood as the result of a single process, the steady excitation of crystal electrons caused by X-ray absorption, which acts as a trigger for the bulk effects that manifest themselves in the form of global damage and obscure the interpretation of chemical information from XFEL and synchrotron structural research.

Quantitative Phase Analysis by X-Ray Diffraction.

1966 ◽  
Vol 38 (12) ◽  
pp. 1741-1745 ◽  
Author(s):  
R. F. Karlak ◽  
D. S. Burnett
Keyword(s):  
Phase Analysis ◽  
Quantitative Phase Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Quantitative Phase

Quantitative Phase Analysis in Titanium by X-Ray Diffraction

1957 ◽  
Vol 1 ◽  
pp. 39-58
Author(s):  
Ralph H. Hiltz ◽  
Stanley L. Lopata
Keyword(s):  
Phase Analysis ◽  
Quantitative Phase Analysis ◽  
Metallographic Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Quantitative Phase ◽  
Method Of Measurement ◽  
Graphic Methods

AbstractIn view of present difficulties encountered in met alio graphic methods of phase analysis of titanium and its alloys, the possibility of utilizing integrated X-ray intensities for phase analysis was investigated. Power Formula variables were calculated for titanium, and relative areas of three alpha and one beta peak were determined. Recorded X-ray intensities were obtained from a large number of titanium specimens. The recorded intensities were analyzed and the results compared with those from metallographic analysis. The errors in the method arising from the nature of titanium, texture and peak overlapping, were studied and where possible, compensated for by adjusting the method of measurement and calculation.

X-Ray Diffraction Intensity of Oxife Soild Soultions: Application to Qualitative and Quantitative Phase Analysis

1982 ◽  
Vol 26 ◽  
pp. 119-128 ◽  
Author(s):  
Ronald C. Gehringer ◽  
Gregory J. McCarthy ◽  
R.G. Garvey ◽  
Deane K. Smith
Keyword(s):  
Phase Analysis ◽  
Solid Solutions ◽  
Inorganic Materials ◽  
Quantitative Phase Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Qualitative And Quantitative ◽  
Quantitative Analyses ◽  
End Members

Solid solutions are pervasive in minerals and in industrial inorganic materials. The analyst is often called upon to provide qualitative and quantitative X-ray phase analysis for specimens containing solid solutions when all that is available are Powder Diffraction File (PDF) data or commercial standards for the end members. In an earlier paper (1) we presented several examples of substantial errors in accuracy of quantitative analysis that can arise when the crystallinity and composition of the analyte standard do not match those of the analyte in the sample of interest. We recommended that to obtain more accurate quantitative analyses, one should determine the analyte composition (e.g., from XRF on grains seen in a SEM or from comparison of cell parameters with those of the end members) and synthesize an analyte standard with this composition and with a crystallinity approximating that of the analyte (e.g., as determined from peak breadth or α1/ α2 splitting).

Effects of Internal Standards and Peak Profile Functions on Quantitative XRD Phase Analysis of Cement and its Hydrates

2011 ◽  
Vol 492 ◽  
pp. 424-428
Author(s):  
Yong Qi Wei ◽  
Wu Yao ◽  
Wei Wang
Keyword(s):  
Phase Analysis ◽  
Internal Standard ◽  
Direct Determination ◽  
Quantitative Phase Analysis ◽  
X Ray Diffraction ◽  
Profile Function ◽  
Internal Standards ◽  
Refinement Method ◽  
Xrd Phase Analysis

Quantitative X-Ray diffraction (QXRD) combined with the Rietveld refinement method allows direct determination of crystalline phase content of cement and its hydrates. However, relatively precise results need the correction of proper internal standards and the use of matched peak profile functions with masterly refinement strategies. The aim of this paper is to research and discuss effects of these factors on the quantitative phase analysis results. For this purpose, different internal standards and peak profile functions with corresponding refinement strategies were attempted in experiments and refinements. The results indicate that Al2O3as internal standard is more suitable for cement and its hydrates than ZnO, and the better peak profile function is CW function 2 rather than function 3 in GSAS.

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