Purifying Compounds by Recrystallization

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Angela W. Herrera

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Feb 21, 2022, 6:11:51 AM2/21/22

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Recrystallization is a technique used to purify solid compounds.1 Solids are usually more soluble in hot liquids than in cold water. During recrystallization, an impure sound compound is dissolved in a hot liquid until the answer is saturated, and after that the liquid is permitted to cool.2 The combination should next make relatively pure crystals. Ideally, any impurities that are present will remain in the answer and will not be integrated into the growing crystals. The crystals might then be taken out of the solution by filtration. Not all the compound is recoverable - some will remain in the answer and also shall be lost. why is it good to use a stemless funnel for hot gravity filtration

Recrystallization isn't generally viewed as a separation technique; rather, it's a purification technique in which a small amount of an impurity is removed from a compound. But, if the solubility components of 2 elements are sufficiently different, recrystallization may be used to sort them, even if they're present in practically equal amounts. Recrystallization is most effective when most impurities have already been removed by another method, such as extraction or maybe column chromatography.

Procedure
Perform all steps in a fume hood to avoid contact with solvent fumes.

1. Selecting a Solvent

Place 50 mg of the test (N-bromosuccinimide) in an Erlenmeyer flask.
Add 0.5 mL of boiling solvent (water). If the sample dissolves completely, the solubility in the cold solvent is too high to be a good recrystallization solvent.

If the test doesn't dissolve in the chilly solvent, heat up the test tube until the solvent boils.
If the sample hasn't totally dissolved at this point, up the boiling solvent drop-wise, until all of the solid dissolves. If it takes more than three mL to dissolve the sample in the warm solvent, the solubility within this solvent is probably too small to make it an excellent recrystallization solvent.

If the first choice of solvent isn't an excellent recrystallization solvent, try others. If a single solvent that works can't be found, try a two solvent system.

If you can't find a suitable single solvent system, subsequently a solvent pair could be necessary. When identifying a solvent pair, there are a number of key considerations 1) The earliest solvent should readily dissolve the solid. 2) The next solvent must be miscible with the 1st solvent, but have a much smaller solubility for the solute.
As a broad rule "likes dissolve likes" which means that polar compounds tend to be soluble in polar solvents and non-polar elements are often more soluble non polar compounds.

Common solvent pairs

Make sure the solvent has a boiling point that is at least forty °C, so there is a reasonable environment difference between boiling solvent and room-temperature solvent.
Make sure that the solvent carries a boiling point below about 120 °C, for this reason it is easier to take away the final traces of solvent from the crystals.
Also ensure the boiling point of the solvent is less than the melting point of the combination, hence the compound forms as solid crystals as opposed to as an insoluble engine oil.
Check that the impurities are sometimes insoluble in the warm solvent (so they can be hot filtered out, after the compound is dissolved) and soluble in the cold solvent (so they stay dissolved during the whole process).

2. Dissolving the Sample in Hot Solvent

Place the combination to be recrystallized within an Erlenmeyer flask. This is a better choice than a beaker, since the sloping sides help trap solvent vapors and slow the rate of evaporation.
Place the solvent (water) in its own Erlenmeyer flask, and add boiling chips or a flurry bar to keep it boiling smoothly. High temperature it to boiling on a hotplate.
Add hot solvent to a flask at room temperature containing the combination in portions which are modest, swirling after every addition, until the compound is totally dissolved.
During the dissolution procedure, maintain the answer hot always by resting it on the hotplate, too. Don't increase the hot solvent than needed - just adequate to dissolve the sample.
If a part of the good does not seem to dissolve, even after much more hot solvent has become added, it is likely due to the presence of extremely insoluble impurities. If this happens, stop adding solvent and do a favorite filtration before proceeding.
To do a hot filtration, fold a piece of air filter paper straight into a fluted cone shape and set it into a glass stemless funnel.
Add a 10 20 % excess of warm solvent to the hot answer to allow for evaporation in the action.
Pour the formula through the paper. If crystals start off to form at any time during the procedure, include a small portion of warm solvent to liquefy them.