CHEM 235 - EXP. 3 - RECRYSTALLIZATION

Crude solid compounds are purified via Recrystallization

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WHAT PROPERTIES OF THE SOLIDS ALLOWS IT TO UNDERGO RECRYSTALLIZATION?
A difference in solubility of the solids. A compound increases its solubility with increased temperature, therefore, by elevating the temperature and allowing it to cool, the compound can be recovered.
WHY DO SOLUBLE IMPURITIES NOT AFFECT THE PURIFICATION PROCESS DURING RECRYSTALLIZATION?
The impurities are in smaller concentrations than the desired compound (isolated from extraction) and will remain in solution under both hot and cold conditions.
If there are is large quantities of impurities, the main chief component reject them during recrystallization because they do not meet its geometry.
WHAT ARE THE BASIC REQUIREMENTS OF A GOOD SOLVENT FOR RECRYSTALLIZATION?
1) It must dissolve the compound only sparingly at room temperature or not at all. It must dissolve the compound readily at its boiling point.
2) It cannot react chemically with the compound to be purified.
3) It must have a bp lower than the melting point of the solid to be purified.
4) It should dissolve impurities well, or not at all.
WHAT IS THE OPTIMUM VOLUME OF SOLVENT TO USE FOR MAXIMUM YIELD OF CRYSTALS?
Varies.
Method: add small amount continuously via the top of the condenser while the compound is being boiled until the compound just dissolves.
WHAT ARE THE ADVANTAGES OF USING A FLASK FOR RECRYSTALLIZATION?
- Narrow neck allows for minimal evaporation.
- Contents can be swirled without spilling.
- Can be corked or stoppered so that vapor and liquid can equilibrate during crystallization.
- Ease of removal
WHEN SHOULD HOT FILTRATION BE CARRIED OUT?
During a recrystallization when one or both of the following are present:
a) There are insoluble impurities remaining in the solution.
b) There are coloured, soluble impurities which require use of Norit as well.
WHY DO YOU ADD EXCESS SOLVENT AND PREWARM THE FUNNEL AND FLASK FOR HOT GRAVITY FILTRATION?
This is to prevent premature precipitation of the solid on the funnel or flask.
WHY CAN NORIT BE USED TO REMOVE IMPURITIES?
It is not soluble in any solvent and coloured substances adsorb onto the Norit. It can be filtered off, along with the impurities.
SOMETIMES, WHEN FILTERING OFF NORIT, SOME TINY CHARCOAL PARTICLES MAY GO THROUGH THE FILTER PAPER, HOW MAY YOU AVOID THIS?
Addition of Celite (twice the amount of Norit) with the Norit. The Norit absorb onto the Celite surfaces thus not falling through the filter paper.