I have a complex compound which is not soluble in any solvent, even dmso. It reacts with dmso, dmf and acetone when heating. I need it to be identified, but spectroscopic techniques don't work because of the poor solubility...
Does anyone know how I can crystallize it?
If you are trying to crystallize your compound to have a single crystal for X-ray, try to melt it and then cool it back. The size of the crystal depends on how quickly the molten compound solidifies. The more slowly it cools, the bigger the crystals.
You can identify it by crystal X-Ray analysis...
If you are trying to make crystallization to have a pure powder, you can think about by-products that you may have with your main product, then use a solvent that dissolves the unwanted compounds.
Crystallize Definition: crystallization is the slow precipitation of crystals from a solution of a substance. Crystallization can also refer to the solid-liquid separation and purification technique in which mass transfer occurs from the liquid solution to a pure solid crystalline phase (from http://chemistry.about.com/od/chemistryglossary/g/crystallizedef.htm)
If you can't dissolve, you can't crystallize.
A short list of purification methods in chemistry is in
http://www.wow.com/wiki/List_of_purification_methods_in_chemistry
If you are trying to crystallize your compound to have a single crystal for X-ray, try to melt it and then cool it back. The size of the crystal depends on how quickly the molten compound solidifies. The more slowly it cools, the bigger the crystals.
You can identify it by crystal X-Ray analysis...
If you are trying to make crystallization to have a pure powder, you can think about by-products that you may have with your main product, then use a solvent that dissolves the unwanted compounds.
Thank you Farah.
As I Know, complexes decompose at their melting point... Thanks again for your smart suggestion.
If you are willing to wait awhile, you don't need high solubility. Set up a horizontal tube filled with a solvent in which your material has some finite solubility and place a mass of your material at one end and the smallest bit you can separate out at the other end. Set the temperature of with the large mass of material above the temperature of the end with the small bit by a fixed small increment, say 5°C. Wait, probably a long time, for the material to dissolve at the hot end and crystalize out at the cold end. The smaller the temperature difference the better the crystal formed but the slower it is formed. The shorter the tube the better as the diffusion time increases as the square of the distance.
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