## July 18, 2024
Explanation of the [[X-Ray Diffraction (XRD)]] Analysis Report for the sample submitted by Carbonatik. This report was prepared by NSL Analytical Services, Inc.
1. Project Scope:
The goal was to use X-ray diffraction to study the crystalline phases present in the sample and develop a [[Semi-quantitative phase identification]] using whole pattern fitting (WPF).
2. Sample Identification:
- The sample was submitted by Carbonatik and described as "golden mica ore".
- NSL Analytical assigned it the sample number S-240710-176.
[[S-240710-176 Gold-Mica]]
3. Methodology:
- The sample was packed into a holder and pressed with a glass slide.
- XRD was performed using a Rigaku Miniflex with Cu Kα radiation, a Ni Kβ filter, and a D/teX Ultra high-speed detector.
- Two scans were performed:
a) Scan 1: 5° to 100° 2θ, at 8.0°/min, with 0.4° step size
b) Scan 2: 7° to 94° 2θ, at 0.5°/min, with 0.1° step size
![[Pasted image 20240817144421.png]]
This image contains two X-ray diffraction (XRD) plots from the analysis of the "golden mica ore" sample (S-240710-176).
Figure 1 (Top Plot):
This is labeled as "Original scan data" and shows the raw XRD pattern.
- X-axis: Represents the diffraction angle (2θ) in degrees, ranging from about 7° to 94°.
- Y-axis: Shows the intensity of diffracted X-rays in counts, scaled up to 1.1 x 10^6.
- The red line represents the diffraction pattern of the sample.
- Major peaks are visible at approximately 9°, 27°, and 45° 2θ, with the highest intensity at 9°.
- Smaller peaks are also visible at higher angles.
Figure 2 (Bottom Plot):
This shows the fitted Whole Pattern Fitting (WPF) results.
- The X and Y axes are the same as in Figure 1.
- The plot contains multiple elements:
1. Blue line: Calculated (fitted) diffraction pattern based on the identified phases.
2. Red line: The original experimental data (same as in Figure 1).
3. Yellow line: Estimated background signal.
4. Colored vertical lines below the main plot: These represent the theoretical peak positions for each identified crystalline phase:
- Blue: Complex K-Na-Ba-Mg-Fe-Al-Ti-Si oxide hydroxide compound
- Red: Biotite
- Green: Silicon Oxide (Alpha form, likely quartz)
- Purple: Iron Silicon
5. Bottom section: Shows the difference plot (pink line) between the calculated and observed patterns. This helps visualize the quality of the fit.
Key Observations:
1. The calculated pattern (blue) closely follows the experimental data (red), indicating a good fit.
2. The major peaks are well accounted for by the identified phases.
3. The difference plot shows some discrepancies, especially at lower angles, which is common in XRD analysis.
4. The background is relatively flat, suggesting good sample preparation and data collection.
This XRD analysis provides crucial information about the crystalline composition of the sample, allowing for the identification and semi-quantitative analysis of the mineral phases present in the "golden mica ore".
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4. Results:
The analysis identified four main phases in the sample:
![[Pasted image 20240817144518.png]]
a) $\text{SiO}_2$ (Silicon Oxide):
- Concentration: 18.7% (±5%)
- Crystal structure: Triclinic, Space Group 1
b) Biotite $\text{K}(\text{Mg},\text{Fe})_3\text{AlSi}_3\text{O}_{10}(\text{F},\text{OH})_2$:
- Concentration: 5.3% (±5%)
- Crystal structure: Monoclinic, Space Group 12
c) $(\text{Fe}_4\text{Si})_{0.4}$ (Iron silicon):
- Concentration: 75% (±5%)
- Crystal structure: Cubic, Space Group 229
d) $(\text{K}_{1.78}\text{Na}_{0.14}\text{Ba}_{0.08})(\text{Mg}_{2.21}\text{Fe}_{1.65}\text{Al}_{1.86}\text{Ti}_{0.28})(\text{Al}_{2.64}\text{Si}_{5.36}\text{O}_{20})\text{O}_{2.7}(\text{OH})_{1.3}$:
- Concentration: 1% (±5%)
- Crystal structure: Monoclinic, Space Group 12
5. Important Notes:
- The report emphasizes that due to differences in X-ray absorptivity between these phases, the proportion of iron silicon is likely overestimated. This affects the reported percentages of other phases as well.
- The analysis achieved a moderate fit between the observed data and calculated phase presence, with an Rwp value of 13.15%.
6. Additional Information:
The report provides explanations of key concepts:
- Phase Identification: How crystalline phases are identified by their unique 2θ peak locations and intensities.
- Semi-quantitative Phase ID: The use of Whole Pattern Fitting (WPF) to determine relative quantities of phases.
- Rachinger Correction: A mathematical method to reduce or eliminate Kα2 peaks in diffraction patterns.
7. Figures:
The report includes two figures:
- Figure 1 shows the original scan data.
- Figure 2 displays the fitted Whole Pattern Fitting (WPF) for Scan 1.
8. Limitations and Considerations:
- The quantitative results are subject to variability due to the nature of testing.
- The analysis is focused on crystalline structures and may not fully represent amorphous phases if present.
- The report is specific to this sample and cannot be used to generalize about all "golden mica ore".
In conclusion, this XRD analysis provides detailed information about the crystalline structure and composition of the submitted sample. However, it's important to note that this analysis alone cannot determine the economic value or potential applications of the material. For a complete assessment, additional geological, mineralogical, and market-based evaluations would be necessary.
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