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Experiment 2 Liquid Liquid Extraction Theory
Experiment 2 Liquid Liquid Extraction Theory
When choosing the solvents for liquid-liquid extractions, what characteristics must they have?
1) First solvent would preferably completely dissolve both compounds in the mixture
When choosing the solvents for liquid-liquid extractions, what characteristics must they have?
When choosing the solvents for liquid-liquid extractions, what characteristics must they have?
3) Second solvent should preferentially dissolve only one component of the original mixture
Mixture is dissolved or suspended in the first solvent and then this solution is introduced to the
second solvent.
By shaking the solvent together in an apparatus called a separatory funnel, one component of the
mixture will be transferred into the second solvent
Final separation of two solvents is accomplished using separatory funnel - followed by evaporation
of solvents, produces the separated components
But if all we did was the following procedure, we would not have totally separated the two
compounds. How do we increase our success?
Compound that we are extracting with 2nd solvent, even though is more soluble in 2nd solvent than
1st but can still dissolve in 1st solvent
What is the extent of the compound dissolve in the less soluble 1st solvent governed by?
The partition coefficient of extraction. This forces us to repeat the extraction step many times
We add a fresh portion of the solvent to separatory funnel containing original solution of mixture, to
ensure that we get best possible separation
Solutions should never occupy more than what amount of volume of the separatory funnel?
Solutions should never occupy more than 2/3 of the volume of the funnel or else proper mixture will
be difficult
-One hand on the stopper, the other on the stopcock -Point stem away from yourself and neighbors
How do we properly shake the separatory funnel?
Gently shake the funnel and open the stopcock to release the initial pressure -Then shake more
vigorously and release
-Repeat until no more pressure develops -This is to enhance the separation of a compounds
Do not hit fragile step against edge. Since we use aqueous solutions, it is not necessary to dry it
before use
Aqueous phase and an immiscible organic phase. Compound isolated is extracted into organic phase
What organic solvents can we use for the solvents in liquid liquid extraction?
When doing liquid liquid solvents, what volume of 1st solvent should we use to dissolve original
mixture?
When doing liquid liquid solvents, how much of the second solvent volume should we use?
For a given amount of volume of extraction solvent, we should divide that volume up to do several
extractions
When doing liquid liquid solvents, how much of the second solvent volume should we use?
We get better results than if we were to use the entire amount for one extraction
When doing liquid liquid solvents, how much of the second solvent volume should we use?
Total volume of the extraction solvent used for the successive extractions usually approximates the
total volume of the other solvent
-Two solvents do not cleanly separate; an emulsion (foamy layer) forms between them
and happens when dissolved materials in the extraction cause the mutual solubility of the two layers
to increase
Wait 10-20 minutes and swirl the flask gently and the emulsion will disappear
If water is one of the solvents, we could add some saturated NaCl solution. This breaks up emulsion.
Because Saturated NaCl is less soluble in organic solvent than water and hence will pull the water
out of organic layer
leaving behind your solid compound. Drying agents are used to absorb this small amount of water
Magnesium Sulfate Sodium sulfate Calcium chloride for hydrocarbons or alkyl halides
-Swirl the corked flask, if all drying agent remains clumped on bottom and does not swirl freely, not
enough has been added
But as long as some of the agent will move freely as individual grains, you added enough. -Get to see
if its swirling again in 5 minutes
For at least 10 minutes with occasional swirling. We remove the salt by gravity filtration through
fluted filter paper
What methods do we use to remove the organic solvent from desired compound?
1) evaporation on a steam bath or hot water bath (in fumehood) 2) evaporation at reduced pressure
What methods do we use to remove the organic solvent from desired compound?
3) distillation (if solute is high boiling liquid or solid) 4)Evaporation by means of rotary evaporator
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