EXPERIMENT 4

TITLE: Acid Base Extraction

OBJECTIVE: To analyze and identify the unknown compound.
PROCEDURE:

A) Extraction
1. Place 0.24g of unknown sample and 0.12g benzoic acid in a test tube.

test tube

benzoic acid

unknown sample

2. Add 10 ml of ether of the mixture and shake to dissolve the mixture.

conical flask

ether “ “
3. Transfer the solution to separatory funnel and add 5 ml of 1 M NaOH.
Relieve the pressure build up as soon as mix the liquids.

solution

1 M NaOH

Swirl and shake the mixture for 30 second. Relieve the pressure occasionally. (
do this step in fume hood)

“ “
4. Allow the layers of mixture to separate. Drain the aqueous solution into
conical flask and label as first extraction NaOH. (flask 1)

flask 1

5. Add 5 ml of the 1 M NaOH solution to the ether layer in the funnel and
repeat step 1 to 5 and label as second extraction NaOH. (flask 2)

Commented [su1]:

flask 2
6. Proceed part 5.2 for aqueous solution in both flasks. Leave the ether in
separation funnel for part 5.3.

B) Filtration

1. In the fume hood, add 6 M of HCI (drop by drop) into each flask and slowly
stirring with glass rod until the solution is acidic by using blue litmus paper.
(16-17 drops)

glass rod

dropper

litmus paper
flask 2
flask 1 flask 1 and flask 2

2. Cool each flask in an ice bath for 15 minutes or until throughly chilled.

ice bath
3. Collect the solid benzoic acid using Buchner funnel and filter flask.

filter paper

buncher
funnel

filter flask

benzoic acid

4. Wash the solution with 2-3 ml of cool water and allow the suction for 5
minutes to get the dry solid possible. Further air dry the solid.

5. Weight the solid and obtain melting point.

5.3 Removal NaOH

1) Add 5 ml of saturated solution NaCI to the ether layer in separatory funnel.

5 ml NaCI

2. Cap, mix and vent and the layers separate as before.

Swirl mixture for 30 seconds. Discard the aqueous layer.

3. Transfer the ether layer into conical flask and 1 g of anhydrous Na₂SO₄
(drying agent) to remove the moisture contains in this flask.

1 g Na₂SO₄
Cap (cover) the flask, swirl and let stand for 10 minutes.

4. While the ether layer is drying, weight of empty small conical flask.
Transfer the dry ether layer using Pasteur pipet into
conical flask.

Pasteur pipet

ether layer

5. In the fume hood, place the conical flask into steam water bath to
evaporate.

fume hood

water bath
Precaution Steps:
1) Wear safety goggles and lab coat during the experiment.
2) Rinse conical flask with deionized water.
3) Avoid contact of acid with skin and clothing.

Potential Hazard:

1. Health Hazard

May cause or suspected of

causing serious health
effects.

2. Chemical Hazard

May cause your skin burn.