BASIC ORGANIC CHEMISTRY TECHNIQUES: REFLUX,DISTILLATION AND EXTRACTION

Experiment 1A: Heating by Reflux and Filtering using Buchner Funnel

Objectives :
1) To know how to use the apparatus of Buchner filtration and set up the reflux
2) To know the reflux techniques to dissolving a solid
3) To learn the importance of Buchner filtration techniques

Chemical(s) :
2 g of crude/impure acetanilide
Apparatus :
An ice-bath
A bottle of distilled water
1 retort stand
1 50 ml or 100 ml round bottom flask
1 condenser
2 rubber hoses
1 adapter
1 heating mantle
1 Buchner funnel
1 250 volumetric flask
1 vacuum pump

Procedure :
Data :
A.

Observation
During heating process -The solution started to boil after a few minutes.
-Solution in round bottom flask is having the
condensation process, water droplets drop back into the
round bottom flask.

During cooling process -Crystal was formed.

Others -White crystal.

B.

Solid before heating

Weight(g)

Mass of the solid 2.01

C.

Solid after heating

Weight(g)

Mass of filter paper 0.80

Mass of the solid + filter paper 2.81

Mass of the solid 2.01

Error(s)/Comment(s) Precaution

-Not all the crystal compound is filtered due -Let the water keep flowing in the
to some crystal sticks to the wall of round condenser.
bottom flask. -Switch off the vacuum pump when wet the
filter to avoid paper from tearing.

Discussion :
The experiment was expected easy to do because it is only dissolved a solid by reflux
techniques. It just need to add a impure acetanilide and 30ml of distilled water to it into a
round bottom flask. Then the solution heated under reflux until the solid dissolved and let
the solution cool at room temperature until the solid crystals of acetanilide form. Once the
solution cooled , attach the Buchner filtration and filtered the solution into a Buchner flask
through the Buchner funnel with filter paper to it . The solid obtained transferred into a
suitable container and let it dry in an oven. Weigh and record the mass of the solid after
drying process end. Overall , during the experiment conduct , there is not too much error
happened unless when the filtering process , not all the crystal compound is filtered
because of some crystal sticks to the wall of round bottom flask.

Conclusion :
Based on the experiment , a solid can be dissolved by using a reflux techniques .

Reference :
https://chemistry.stackexchange.com
 Experiment 1B : Distillation techniques and to determine the boiling point of a liquid.

Objectives :
To learn the techniques of distillation and boiling point determination

Chemicals :
30% of ethanol
Boiling chips (5-6 pieces)

Apparatus :
2 retort stands
1 50-100 ml round bottom flask
1 Condenser
1 still head
1 thermometer
1 filter paper
2 rubber hoses
1 adapter
1 pocket thermometer
1 heating mantle

Procedure :
 Data :
A : Record a stable temperature as the boiling point of the liquid to be distilled

Range of stable temperature (° C ¿

Start : 76
End : 85

Boiling point range of ethanol : 78℃

B : Calculation of percentage of ethanol recovered

Volume(ml)
Initial volume of ethanol in 25 ml
7.5ml

Volume of ethanol collected after

distillation 4ml

Calculation of percentage recovery

4/7.5 X 100 =53.33%

Discussion :
This experiment is about the distillation techniques and determine the boiling point. For the
distillation and boiling process , the round bottom flask was filled with 25 ml solution of 30%
ethanol and add a few boiling chips. When boiling , the liquid was heated until the
distillation rate is about 2-3 drops per second which is a constant rate. A stable temperature
as the boiling point of the liquid distilled recorded which is 78℃ . After the following
process is done , we got the volume of ethanol collected after distillation is 4ml. For the
percentage yield is 53.33%. When conduct this experiment , there is a little bit problem to
set up the apparatus because involved a lot of apparatus . However , not much error
happened .
 Conclusion :
The boiling point of ethanol can be determine through this experiment which is 78℃.

Reference :
https://orgchemboulder.com
 Experiment 1C : Extraction and Drying of an Aqueous Solution.

Objectives :
1. To learn the techniques of separating toluene from water ( and other inorganic
compounds) by extraction.
2. To learn the techniques of drying a dehydrated solution.

Chemicals :
Toluene solution
Diethyl ether
Anhydrous magnesium sulphate

Apparatus:
1 separating funnel
1 retort stand
1 100ml round bottom flask
1 condenser
1 still head
1 thermometer
1 filter paper
1 heating mantle
1 adapter
1 pocket thermometer
Procedure :

Data :
Volume of toluene used : 20ml
Volume of diethyl ether used : 40ml
Volume of toluene after distillation : 13ml
Volume of diethyl ether after distillation : 30ml
Boiling point range of diethyl ether : 33 to 36 ml
Boiling point of toluene : 110℃
Percentage yield of toluene recovered : 65%

13 × 100 = 65%
20

Percentage yield of diethyl ether recovered : 65%

30 × 100 = 75 %
40
Discussion :
This experiment is about extraction and drying of an aqueous solution. However , there are
several mistake that accidently happened when conduct the experiment . Based on the
experiment , we need to drain the diethyl ether containing toluene into a dry conical flask .
But we accidentally drained the wrong solution which is aqueous layer into a conical flask
due we cant identified which one is the organic layer and aqueous layer since there is two
layers appear .So that there is organic layer in separating funnel left . Then we add another
20ml diethyl ether into the separating funnel so that its not split into two layers . Beside , we
added one spatula of anhydrous magnesium sulphate into a aqueous solution . So that the
second extraction did not work . Due this error we could not get the full data and make a
decisions to take a data from another group for our report .

Conclusion :
Based on the experiment , the toluene cannot be separate from water by extraction
because of an error happened . The dehydrated solution also cannot be dry due the second
extraction did not work.

Reference :
Royal Society of Chemistry page .