Explain the Recrystallization Operating Procedure Flashcards

Experiment 3 Recrystallization Operating Procedure

29 cards   |   Total Attempts: 189
  

Cards In This Set

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What glassware are recrystallizations usually done in?
Erlenmeyer flasks and the size of the flask is determined by the volume used
Why Erlenmeyer flasks?
Good crystal growth, accompanied by expulsion of impurities requires space (depth) in solution -This is achieved by Erlenmeyer flasks
Why Erlenmeyer flasks?
-Erlenmeyer flasks must contain much solution as possible (0.5 to 2/3 full) which is done by turning flask to 45 degree angle
List 4 Reasons why Erlenmeyer flasks are idea
1) Narrow neck allows some refluxing of the solvent so that surface evaporation is minimized (can put condenser on top of flask)
List 4 Reasons why Erlenmeyer flasks are idea
2) They can be corked or stoppered so that during crystallization vapour and liquid can equilbriate,
List 4 Reasons why Erlenmeyer flasks are idea
2)Thus the amount of solvent will not be changed through evaporation
List 4 Reasons why Erlenmeyer flasks are idea
3) They can be swirled to facilitate dissolving of the solid
List 4 Reasons why Erlenmeyer flasks are idea
4) It is easy to remove crystals from an erlenmeyer flask
When setting up apparatus, the condenser is clamped to a bar. How tightly should the clamp hold the condenser
Very loosely, as this is done to allow free swirling of the flask on top of the hotplate
Why is swirling important in recrystallizations?
It helps facilitate the dissolving of the solid and also prevents bumping which occurs during heating
What do we place in the erlenmeyer flask initially?
The pure solid, together with a boiling chip and a small amount of solvent is added at room temp to begin reflux, (not to fully dissolve)
Once the mixture is heated to boiling what do we do?
We add small amounts of solvent (via top of condenser) until the solid just dissolves
Why do we add a minimum amount of solvent so that the compound just barely dissolves?
This results in a solution that is saturated with the solid and when cooled should return the maximum amount of solute in the form of crystals
When do we perform hot gravity filtrations?
If either or both are present 1) Insoluble impurities remaining in the solution 2) Coloured, soluble impurities which necessitates the use of Norit
How do we prepare for a hot filtration?
Once desired compound has been dissolved in hot solvent, add an addition amount of solvent (1/4 of original volume to produce saturated solution)