LIQUID

SEPARATING A
SOLID MIXTURE

EXTRACTION BASED ON
DIFFERENTIAL
SOLUBILITIES
 1. Weigh the quantity of unknown mixture to be separated.

a) Place an empty beaker on the b) Remove the beaker from the balance and
balance and push the T to add mixture by carefully tapping the vial with your forefinger
electronically zero the balance
 1. Weigh the quantity of unknown mixture to be separated.

c) Weigh a preliminary amount d) Remove the beaker from the e) Reweigh: anything between
and estimate how much more pan and add more mixture 1.7 and 2.2 g will work.
you need to add.
 2. Transfer the mixture to a conical tube.

a) Label the tube with the b) Hold the tube and beaker in c) Carefully transfer all the solid
unknown #. one hand to the tube.
2. Transfer the mixture to a conical tube.

d) Use ether to rinse the solid residue from the beaker e) Transfer the ether wash into
the conical tube.
. Prepare the extraction.

a) label 3 clean, dry, regular test tubes:

c) Weigh Et2O #2 and record the
aq. NaHCO3
weight in your lab notebook.
Et2O
Et2O #2
b) line them up in the test tube rack
Extraction requires two immiscible solvents

meniscus

and a conical tube

Use a pipette to mix layers vigorously

Then allow the layers to

separate
 To transfer a layer, hold both
test tubes in the same hand

Transfer the bottom transferred

Pipet layer aqueous layer
touches the bottom
Repeat with aqueous washes, then transfer ether
layer to a dry test tube
Drying the Organic Layer 1

add 5 or 6 CaCl2 pellets to the ether layer

rotate the test tube gently
Drying the organic layer 2

Too wet!
Water droplets on side of test tube

Drying pellets have dissolved!

 Better,
but not dry enough

Drying pellets

float freely in dry organic solvent

 Recovering the component from ether 2 immiscible liquids

Insert
the tip in
the top
of the
ether
test tube

Turn on a very gentle stream of compressed air

Recovering the Acid

Transfer the aq. NaHCO3

layer to a beaker
Recovering the Acid Component

Add HCl dropwise to precipitate organic acid

Test pH - If paper turns red,
youve added enough HCl
Set up vacuum filtration Filter paper

To collect the product Buchner funnel

neoprene
adaptor vacuum hose

vacuum flask
filter
trap
Wet the filter paper so it
will stick to the funnel
Transfer the solid
 Completely transfer the solid

Then draw air through the funnel for 5 more minutes

 2. Transfer the
filtered solid to
the watchglass

1. Tare a clean, dry

watchglass

3. Weigh and record the

mass of the solid
When all the ether is gone, weigh the neutral component
 Testing for Phenolic -OH

1. Add a few mLs water 2. Add 2 drops FeCl3

Mix well by knocking the test tube

against your hand