@mooka
I totally agree that we need to "
purify the product then check what's wrong."
That is why it was so disappointing and frustrating when Vash's associate lost the separated impurities that needed to be tested.
However, Vash and others have suggested that re-crystallization is not going to be enough to separate the impurities without running a column.
Which is why I am asking if anyone here can walk me through that process step by step. I have product here that has been acetone washed and re-crystallized and still is not right. Tell me what to do with it. The few instructions I have seen have started with a tremendous amount of product. I am never going to have that much product. I don't operate like that. How can I run a column on a small amount of product?
recrystallise more times, at least 4 or 5, using lab grade IPA.
Recrystallization is a laboratory technique used to purify solids based on their different solubilities. A small amount of solvent is added to a flask containing an impure solid. The contents of the flask are heated until the solid dissolves. Next, the solution is cooled. The more pure solid precipitates, leaving impurities dissolved in the solvent. Vacuum filtration is used to isolate the crystals. The waste solution is discarded.
Summary of Recrystallization Steps
- Add a small quantity of appropriate solvent to an impure solid.
- Apply heat to dissolve the solid.
- Cool the solution to crystallize the product.
- Use vacuum filtration to isolate and dry the purified solid.
Let's take a look at the details of the recrystallization process.
Add the Solvent
Choose a
solvent such that the impure compound has poor solubility at low temperatures, yet is completely soluble at higher temperatures. The point is to fully dissolve the impure substance when it is heated, yet have it crash out of solution upon cooling. Add as small a quantity as possible to fully dissolve the sample. It's better to add too little solvent than too much. More solvent can be added during the heating process, if necessary.
Heat the Suspension
After the solvent has been added to the impure solid, heat the suspension to fully dissolve the sample. Usually, a hot water bath or steam bath is used, since these are gentle, controlled heat sources. A hot plate or gas burner is used in some situations.
Once the sample is dissolved, the solution is cooled to force crystallization of the desired compound.
Cool the Solution for Recrystallization
Slower cooling may lead to a higher purity product, so it's common practice to allow the solution to cool to room temperature before setting the flask in an ice bath or refrigerator.
Crystals usually begin forming on the bottom of the flask. It's possible to aid crystallization by scratching the flask with a glass rod at the air-solvent junction (assuming you are willing to purposely scratch your glassware). The scratch increases the glass surface area, providing a roughened surface on which the solid can crystallize. Another technique is to 'seed' the solution by adding a small crystal of the desired pure solid to the cooled solution. Be sure the solution is cool, or else the crystal could dissolve. If no crystals fall out of solution, it's possible too much solvent was used. Allow some of the solvent to evaporate. If crystals do not spontaneously form, reheat/cool the solution.
Once crystals have formed, it's time to separate them from the solution.
Filter and Dry the Product
Crystals of purified solid are isolated by filtration. This is usually done with vacuum
filtration, sometimes washing the purified solid with chilled solvent. If you wash the product, be sure the solvent is cold, or else you run the risk of dissolving some of the sample.
The product may now be dried. Aspiring the product via vacuum filtration should remove much of the solvent. Open-air drying may be used as well. In some cases, the recrystallization may be repeated to further purify the sample.
a video here:
