XRD Sample Prep: Pulverization w/o Affecting Crystallinity?

AI Thread Summary
The discussion centers on the challenge of analyzing precipitate samples for XRD after they have cemented on a filter pad, making them unsuitable for direct analysis. The user is concerned that using a mortar and pestle for pulverization may compromise the crystallinity of the samples, which is crucial for accurate results. Suggestions include exploring alternative methods for pulverization that minimize crystallinity loss or discussing the potential use of a mortar and pestle with additional precautions. The practicality of evaporating the carrier fluid instead of filtering is also considered, but the user finds it impractical due to the volume of slurry and the need to collect the filtrate. Overall, the focus is on finding a method to prepare the samples without compromising their structural integrity.
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.
 

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