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Quantitative Compound Analysis

General XRD - Quantitative Compound Analysis

AMIA Laboratories specializes in the investigation and characterization of materials using the latest advances in x-ray diffraction. We can help you determie if or which x-ray analysis will help in your materials characterization. The quantification of  an XRD pattern can produce percentages of crystallographic phases. Quantitative Analysis (Semi-Quant and Reitveld) are the two major quantification for crystallographic phases. Percent crystallinity, latice parameters and crystallite size are other quanitative measurments of a crystallographic phase.

General XRD: Semi-Quant Analysis

Semi-quantitative analysis (sometimes called Easy-Quant) does not require external standard calibration curves as does complete quantitative analysis, but the accuracy is not as high as with complete quantitative analysis. Semi-quantitative analysis does yield good relative values however, and in most cases is accurate to within + 5% for multiphase samples. Semi-quantitative analysis uses the RIR (Reference Intensity Ratio) associated with the phases in question in order to estimate the wt % of the individual phases. Although it does not require standards and calibration curves, it does require that all phases are identified correctly and that RIR values are available from the literature for all of the phases in the sample. AMIA Labs provides complete quantitative analysis via the external calibration method, quantitative analysis via the Rietveld method, and semi-quantitative analysis via the RIR method. Please call for recommendation on analysis type and quotation.

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General XRD: Rietveld Analysis

Rietveld Analysis may be considered a Fundamental Parameters program for XRD, providing accurate Quantitative results (usually to within ±1%), Unit Cell dimensions (phase chemistry and solid solutions), Crystallite Size and Crystal Structure (atomic site occupancy factors). Rietveld modeling does require models for atomic coordinates for all phases present in the sample, as well as a professional diffractionist capable of setting variables such as preferred orientation and accurate background modeling. AMIA Laboratories has significant experience in Rietveld analysis, and is available to do the complete analysis, or set up models to automate procedures at the customer site. Please call for a quotation.

More Rietveld Analysis

Rietveld Analysis may be considered a Fundamental Parameters program for XRD. It refines various parameters including lattice parameters, peak width and shape, and preferred orientation to derive a new diffraction pattern. Once the derived pattern is nearly identical to the original data, various properties pertaining to the sample can be obtained including:

  • Accurate Quantitative Results (usually to within ±1%)
  • Crystallite Size
  • Site Occupancy Factors

There are many methods for conventional quantitative analysis. Most need standards to achieve reasonable accuracy. The standardless or RIR method is usually accurate to within ±3%. For better accuracy a standards method is used. There is a considerable time investment involved in preparing and measuring standards. It is an accurate technique, but inflexible. If a new component enters the method, additional standards must be prepared.

Rietveld Analysis doesn't use standards. Instead, it calculates how the diffraction profiles are affected by the different crystal properties previously mentioned. It continues to refine its estimates of the new diffraction profiles and computes a difference pattern. As this difference becomes smaller, the derived pattern begins to look more like the original data. At some point there is no improvement, and the refined pattern's parameters are used to calculate results. The process of refining the pattern is compute-intensive, but with the advent of modern powerful PC's it takes approximately 20 minutes to calculate results for a 12-component mixture, a task nearly impossible using conventional methods.

The main advantage of Rietveld Analysis over conventional quantitative methods is that no standards are required to achieve accurate results to within ±1%.

 

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