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SEM image of a representative crystal used for WDS and X-ray diffraction analysis showing the location and results for the WDS analysis. The 10 μm sized analysis spots are represented by the white dots. Adapted from B. D. Fahlman, Ph.D. Thesis, Rice University, 2000.

Comparison of the methods

Method 1

Since Method 1 does not refine the %Cr and relies on an input for the Al and Cr percent composition of the "bulk" material, i.e., the %Cr in the total mass of the material ( [link] , Column 1), as opposed to the analysis of the single crystal on which X-ray diffraction was performed, ( [link] , Column 2), the closer these values were to the "actual" value determined by WDS for the crystal on which X-ray diffraction was performed ( [link] , Column 1 versus 2) then the closer the overall refinement of the structure to those of Methods 2 - 4.

While this assumption is obviously invalid for many of the samples, it is one often used when bulk data (for example, from NMR) is available. However, as there is no reason to assume that one crystal is completely representative of the bulk sample, it is unwise to rely only on such data.

Method 2

This method always produced final, refined, occupancy values that were close to those obtained from WDS ( [link] ). This approach assumes that the motion of the central metal atoms is identical. While this is obviously not strictly true as they are of different size, the results obtained herein imply that this is a reasonable approximation where simple connectivity data is required. For samples where the amount of one of the elements (i.e., Cr) is very low so low a good refinement can not often be obtained. In theses cases, when refining the occupancy values, that for Al would exceed 1 while that of Cr would be less than 1!

Method 3

In some cases, despite the interrelationship between the occupancy and the displacement parameters, convergence was obtained successfully. In these cases the refined occupancies were both slightly closer to those observed from WDS than the occupancy values obtained using Method 2. However, for some samples with higher Cr content the refinement was unstable and would not converge. Whether this observation was due to the increased percentage of Cr or simply lower data quality is not certain.

While this method does allow refinement of any differences in atomic motion between the two metals, it requires extremely high quality data for this difference to be determined reliably.

Method 4

This approach adds little to the final results.

Correlation between analyzed composition and refined composition

[link] shows the relationship between the chromium concentration (%Cr) determined from WDS and the refinement of X-ray diffraction data using Methods 2 or 3 (labeled in [link] ). Clearly there exists a good correlation, with only a slight divergence at high Cr concentration. This is undoubtedly a consequence of trying to refine a low fraction of a light atom (Al) in the presence of a large fraction of a heavier atom (Cr). X-ray diffraction is, therefore, an accurate method of determining the M:M' ratios in crystalline solid solution.

Comparison of the chromium concentration determined from WDS (with error) and refinement of X-ray diffraction data (with error) using Methods 2 or 3. Adapted from S. G. Bott, B. D. Fahlman, M. L. Pierson, and A. R. Barron, J. Chem. Soc., Dalton Trans. , 2001, 2148.

Bibliography

  • S. G. Bott, B. D. Fahlman, M. L. Pierson, and A. R. Barron, J. Chem. Soc., Dalton Trans. , 2001, 2148.
  • K. R. Dunbar and S. C. Haefner, Inorg. Chem., 1992, 31 , 3676.
  • J. Glusker, M. Lewis, and M., Rossi, Crystal Structure Analysis for Chemists and Biologists VCH: New York (1994).
  • K. Yoon and G. Parkin, Inorg. Chem. , 1992, 114 , 31.

Questions & Answers

how do you translate this in Algebraic Expressions
linda Reply
Need to simplify the expresin. 3/7 (x+y)-1/7 (x-1)=
Crystal Reply
. After 3 months on a diet, Lisa had lost 12% of her original weight. She lost 21 pounds. What was Lisa's original weight?
Chris Reply
what's the easiest and fastest way to the synthesize AgNP?
Damian Reply
China
Cied
types of nano material
abeetha Reply
I start with an easy one. carbon nanotubes woven into a long filament like a string
Porter
many many of nanotubes
Porter
what is the k.e before it land
Yasmin
what is the function of carbon nanotubes?
Cesar
what is nanomaterials​ and their applications of sensors.
Ramkumar Reply
what is nano technology
Sravani Reply
what is system testing?
AMJAD
preparation of nanomaterial
Victor Reply
Yes, Nanotechnology has a very fast field of applications and their is always something new to do with it...
Himanshu Reply
good afternoon madam
AMJAD
what is system testing
AMJAD
what is the application of nanotechnology?
Stotaw
In this morden time nanotechnology used in many field . 1-Electronics-manufacturad IC ,RAM,MRAM,solar panel etc 2-Helth and Medical-Nanomedicine,Drug Dilivery for cancer treatment etc 3- Atomobile -MEMS, Coating on car etc. and may other field for details you can check at Google
Azam
anybody can imagine what will be happen after 100 years from now in nano tech world
Prasenjit
after 100 year this will be not nanotechnology maybe this technology name will be change . maybe aftet 100 year . we work on electron lable practically about its properties and behaviour by the different instruments
Azam
name doesn't matter , whatever it will be change... I'm taking about effect on circumstances of the microscopic world
Prasenjit
how hard could it be to apply nanotechnology against viral infections such HIV or Ebola?
Damian
silver nanoparticles could handle the job?
Damian
not now but maybe in future only AgNP maybe any other nanomaterials
Azam
can nanotechnology change the direction of the face of the world
Prasenjit Reply
At high concentrations (>0.01 M), the relation between absorptivity coefficient and absorbance is no longer linear. This is due to the electrostatic interactions between the quantum dots in close proximity. If the concentration of the solution is high, another effect that is seen is the scattering of light from the large number of quantum dots. This assumption only works at low concentrations of the analyte. Presence of stray light.
Ali Reply
the Beer law works very well for dilute solutions but fails for very high concentrations. why?
bamidele Reply
how did you get the value of 2000N.What calculations are needed to arrive at it
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advantages of NAA
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Source:  OpenStax, Physical methods in chemistry and nano science. OpenStax CNX. May 05, 2015 Download for free at http://legacy.cnx.org/content/col10699/1.21
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