XRD Sample Prep: Pulverization w/o Affecting Crystallinity?

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SUMMARY

The discussion centers on the challenge of preparing precipitate samples for X-ray diffraction (XRD) analysis without compromising their crystallinity. The user collected samples via filtration, resulting in a cemented form unsuitable for XRD. Suggestions include using a mortar and pestle for pulverization, with concerns raised about potential crystallinity loss. Alternative methods, such as evaporating the carrier fluid instead of filtering, were considered impractical due to the sample volume and the need for filtrate collection.

PREREQUISITES
  • Understanding of X-ray diffraction (XRD) analysis techniques
  • Familiarity with sample preparation methods for crystallinity preservation
  • Knowledge of mortar and pestle usage for material pulverization
  • Basic principles of filtration and solvent evaporation in sample processing
NEXT STEPS
  • Research methods to minimize crystallinity loss during sample pulverization
  • Explore alternative sample preparation techniques for XRD analysis
  • Investigate the effects of different solvents on crystallinity during evaporation
  • Learn about advanced filtration techniques suitable for precipitate samples
USEFUL FOR

Researchers and laboratory technicians involved in materials science, particularly those focused on XRD analysis and sample preparation techniques for preserving crystallinity in precipitate samples.

Baho Ilok
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I have some precipitate samples that I wish to analyze for XRD. I collected them by filtration of a slurry. Through the filtration, the precipitates "cemented" on the surface of the filter pad so the samples I collected are not exactly in powdered form, which I believe is the ideal form to do XRD analysis.

I have read that in such cases, pulverization can be achieved using mortar and pestle. However, I worry that this might affect the crystallinity of the precipitates, which is the most important characteristic that I wish to analyze.

Can somebody suggest a method to achieve pulverization without affecting (or at least minimizing) the effect on crystallinity? Or if I am to use mortar and pestle, is there an additional step that should be taken to avoid errors?

Thank you so much!
 
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Can you evaporate off the carrier fluid instead of using filtering for separation ?
 
Nidum said:
Can you evaporate off the carrier fluid instead of using filtering for separation ?
I have thought of that but my slurry volume is 1 L so it may be a bit impractical to evaporate off the solvent. And I also have to collect the filtrate for analysis.