Semi-quantitative phase identification using Whole Pattern Fitting (WPF) is a sophisticated technique derived from Rietveld Refinement. It aims to determine the relative quantities of [[Crystalline phases]] in a material by comparing the measured diffraction pattern to calculated patterns of known phases. Here's a more detailed explanation:
1. Methodology:
WPF takes into account variations in crystal structure, including:
a) Lattice parameters, which can shift peak positions
b) Orientation factors, which can alter peak intensity relations
2. Process:
- The software (in this case, Smartlab Studio 2) uses known crystal structures from the ICSD (Inorganic Crystal Structure Database) to generate theoretical diffraction patterns for each identified phase.
- It then attempts to minimize the difference between the measured diffraction pattern and a weighted sum of these theoretical patterns.
- The weightings of these theoretical patterns correspond to the relative abundances of each phase.
3. Quality of Fit:
- The quality of this fitting is quantified by the Rwp value (weighted profile R-factor).
- In this analysis, an Rwp of 13.15% was achieved, indicating a moderate agreement between observed and calculated patterns.
4. Limitations:
- The report notes a critical limitation: differences in X-ray absorptivity between phases.
- Iron silicon, being less likely to absorb X-rays than the other phases, is probably overestimated in quantity.
- This overestimation consequently affects the reported percentages of other phases.
5. Accuracy:
- The concentrations are reported with an uncertainty of ±5 wt%.
- This uncertainty reflects both the inherent limitations of the technique and the specific challenges of this sample.
6. Interpretation:
- Despite the limitations, WPF provides valuable insights into the relative abundances of crystalline phases.
- It's particularly useful for comparing similar samples or tracking changes in phase composition.
In this specific analysis, the semi-quantitative results suggest a predominance of iron silicon $(\text{Fe}_4\text{Si})_{0.4}$ at 75%, followed by silicon oxide $\text{SiO}_2$ at 18.7%, biotite at 5.3%, and a complex potassium-sodium-barium-magnesium-iron-aluminum-titanium-silicon oxide hydroxide compound at 1%. However, these percentages should be interpreted cautiously due to the noted absorptivity issues.
This semi-quantitative approach, while not providing absolute quantification, offers a robust method for characterizing the crystalline composition of complex materials like the "golden mica ore" analyzed in this report.
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