From theory of spectra to standardless analysis of molecular objects

2012 ◽  
Vol 67 (5) ◽  
pp. 414-422 ◽  
Author(s):  
L. A. Gribov ◽  
V. A. Dement’ev
Author(s):  
John J. Friel

Committee E-04 on Metallography of the American Society for Testing and Materials (ASTM) conducted an interlaboratory round robin test program on quantitative energy dispersive spectroscopy (EDS). The test program was designed to produce data on which to base a precision and bias statement for quantitative analysis by EDS. Nine laboratories were sent specimens of two well characterized materials, a type 308 stainless steel, and a complex mechanical alloy from Inco Alloys International, Inconel® MA 6000. The stainless steel was chosen as an example of a straightforward analysis with no special problems. The mechanical alloy was selected because elements were present in a wide range of concentrations; K, L, and M lines were involved; and Ta was severely overlapped with W. The test aimed to establish limits of precision that could be routinely achieved by capable laboratories operating under real world conditions. The participants were first allowed to use their own best procedures, but later were instructed to repeat the analysis using specified conditions: 20 kV accelerating voltage, 200s live time, ∼25% dead time and ∼40° takeoff angle. They were also asked to run a standardless analysis.


1991 ◽  
Vol 35 (B) ◽  
pp. 1035-1046
Author(s):  
Y. Kataoka ◽  
N. Masukawa ◽  
K. Toda

The semi-quantitative analysis, which is called ‘Standardless Analysis’, plays a major role in X-ray fluorescent analysis, especially in the field of research and development. The main feature of the semi-quantitative analysis is the fact that the composition of a sample can be obtained directly from a qualitative scan without any prior knowledge of the sample.


Author(s):  
János L. Lábár ◽  
Charles E. Fiori ◽  
Robert L. Myklebust

Relative intensities of the non-analytical lines of an element (as compared to the analytical X-ray line of the same element) directly affect the accuracy of quantitative X-ray microanalysis. Correct spectral deconvolution can only be based on the knowledge of these relative intensities. Not even wavelength dispersive spectrometry (WDS) is free from spectral overlaps, making deconvolution of the X-ray lines necessary. A typical example for such a serious overlap can be the L line series of different rare-earth elements simultaneously present in the same sample. Energy dispersive spectrometry (EDS) is even more affected. Many EDS systems are equipped on scanning electron microscopes (SEM). Quick standardless analysis is frequently in use in these systems. Starting approximation of the elemental concentrations are based on computed "standard intensities" in contrast to measured ones in full quantitative analysis. Computation of the generated standard intensities directly contain the relative intensities of other lines too.


Author(s):  
Martin Völkerer ◽  
Michael Andrae ◽  
Kurt Röhrbacher ◽  
Johann Wernisch

1998 ◽  
Vol 361 (5) ◽  
pp. 504-506 ◽  
Author(s):  
F. N. Rossi ◽  
D. Melucci ◽  
C. Locatelli ◽  
P. Reschiglian ◽  
A. Millemaggi ◽  
...  

1997 ◽  
Vol 3 (S2) ◽  
pp. 899-900
Author(s):  
J.M. Dijkstra ◽  
R.B Shen

In the last 10 years the development of new polymer type detector window materials has dramatically increased the opportunities for light element analysis with Energy Dispersive Spectrometers (EDS). With the introduction of light-element analysis the need also arises to accurately quantify X-ray spectra. Traditional quantification techniques, using a probe current measuring device and pure elemental standards, have been introduced into the field of EDS, but these techniques prevented much of the conveniences of the EDS techniques with respect to speed and ease of use. Many users are therefore willing to sacrifice part of the maximum achievable accuracy in return for a method that is more convenient: standardless analysis.With EDS analysis the widely published ZAF and φ(ρz) models can be used to convert relative intensities into weight percentages, but for standardless analysis the inaccuracy of the result is mainly caused by the reference intensities.


1992 ◽  
Vol 7 (4) ◽  
pp. 186-193 ◽  
Author(s):  
Robert L. Snyder

AbstractEach of the RIR based methods for carrying out quantitative X-ray powder diffraction analysis are described and a consistent set of notation is developed. The so called “standardless” analysis procedures are shown to be a special case of the internal-standard method of analysis where the normalizing assumption is used. All analytical methods, other than the Rietveld whole pattern matching procedure, require the use of explicitly measured standards, typically in the form of RIR values. However, if only semi-quantitative results can be tolerated, the standards may be obtained by using published RIR and relative intensity values. The exciting new techniques of whole pattern fitting and Rietveld constrained quantitative analysis are also described in RIR notation and shown also to be forms of the internal-standard method with the normalization assumption. The quantitative results obtained from Rietveld quantitative analysis are derived from computed standards in the form of computed, normalized, RIRN values. The normalization assumption in Rietveld analysis allows the exclusive use of computed standards and comes as close to a “standardless” analysis as one can achieve: relying on the absence of amorphous material and on the validity of the structural models. Relationships are given for obtaining quantitative analysis from these RIRN values obtainable from the least-squares scale factors.


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