Hi everyone, I am trying to synthesize a crystalline material ( Metal-Organic Framework) by using NMP as solvent. After the reaction, I have carried out XRD analysis of a slurry sample that contains NMP and as-synthesized solid. The intensity of peaks below 10 theta was too low and broad.
I wanted to consult you to understand whether introducing my sample in the form of slurry with NMP can affect my analysis.
Best regards.
I do not well understand. The sample is solid? NMP was used as a solvent and removed? Usually the slurry for electrochemical measurements are prepared by using NMP as solvent, that is then removed by heating and drying in vacuum
I would rather suggest using the lyophilizer or freeze dryer to make powder of the sample.
It is possible that the presence of NMP in your sample could affect the quality of the X-ray diffraction (XRD) data. NMP is a solvent that can potentially interfere with the crystalline structure of your material, leading to broad and weak diffraction peaks.
One way to mitigate this issue is to try to remove as much of the solvent as possible before analyzing the sample. This can be done by drying the sample under reduced pressure or by evaporating the solvent at room temperature. After removing the solvent, you should be able to obtain more accurate and reliable XRD data.
Alternatively, you could try to analyze the sample in a different form, such as a dry powder or a thin film. This could help to minimize the impact of the solvent on the diffraction pattern.
It is also worth noting that the intensity and width of the diffraction peaks can be influenced by other factors as well, such as the size and shape of the crystallites in the sample, the degree of perfection of the crystal lattice, and the presence of defects or impurities. These factors should also be considered when interpreting the XRD data.
Thank you all for your explanations and suggestion. Dr. Marcella Bini my sample is solid but it is wet with NMP solvent and take the form of slurry. My solvent is NMP but it is not removed.This solid has a highly porous structure and removal of high boiling point solvent with vacuum and heat causes pore collapse. So, I need the XRD of wet sample.
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