Experiment 2: Heating by Reflux and Filtering using Buchner

Funnel
Course Code: CHM 207

Group Members:

Name Matrix no.

AZMIR NURHAKIM MOHD ZAWAWI 2017256812

MUHAMMAD DARWIN BIN MOHMAD ROSDI 2017256596

RAJA MUHAMMAD ARASHRIFQI BIN RAJA ADNAN 2017256794

NUR AFIQAH BINTI JAFRI 2015804574

Date of experiment: 16 March 2018

Date of submission: 30 March 2018

Lectures’ Name: En. Muhd Hafiz Yaakub

 EXPERIMENT 1
BASIC ORGANIC CHEMISTRY TECHNIQUES: REFLUX, DISTILLATIONAN AND EXTRACTION
EXPERIMENT 1A: Heating by Reflux and filtering using Buchner Funnel
Objective:
1. To learn how to set up a reflux and Buchner filtering apparatus
2. To learn the technique of dissolving a solid by reflux.
3. To learn the importance of using reflux and Buchner filtration technique.
Introduction:
Heating by reflux is useful for dissolving a solid that only can be dissolved by prolonged
heating in a suitable solvent at boiling point. The loss of the solvent can be avoided by using
this method whereby as a solvent heated, the solvent vapour would be cooled at the
surface of the condensed back to its liquid form again,
Chemical(s):
2g of crude/impure acetanilide
Apparatus:

• An iced-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 or suitable apparatus for heating the round bottom flask
• 1 filter paper
• 1 Buchner funnel
• 1 250 ml Buchner flask
• 1 vacuum pump
• Oven for drying (optional)
Procedures:
1. 2g of crude/impure acetanilide and 30 ml of distilled water, as a solvent was added
into a round bottom flask. The solution under reflux was heated until the solid
dissolved. Then the solution been cooled at room temperature until the solid crystals
of acetanilide.
2. A clean 250 ml Buchner was clamped to a retort stand and put a Buchner funnel with
a Filter to it. Filter paper are been wet to ensure it lies flat in order to stop the
crystals not to pass through the edge and under the filter paper.
3. The Buchner filtration was attached to a vacuum pump
 4. The solution that contained the solid/crystals of acetanilide was poured into the
Buchner funnel. The vacuum applied. The c=vacuum was stopped as soon as the
liquid disappears.
5. The solid/crystals with cold solvent was rinsed, then the vacuum reapplied until the
solvent disappears.
6. The solid obtained was transferred into a suitable container and let it dry in an oven.
7. The mass of solid obtained was reported after drying process end.
8. The percentage yield of the solid obtained was calculated.

QUESTION

1. In a process in which require prolong heating, why reflux is a suitable method?

Reflux is a suitable method during a prolong heating experiment because the
technique more suitable to dissolve a solid when heating with consistent.

2. The Buchner filtration process is well known, faster than gravity filtration, instead
of this reason why Buchner filtration chosen for filtration?
It is because the apparatus of Buchner filtration are most effective to dry the
crystal/solid with vacuum.

3. Why the solid obtained need to be rinse with cold solvent during the filtration
process?
The solid obtained need to be rinse with cold solvent because the solid must form
with the crystal formed.

4. Give 3 characters of a solvent that can make the solvent chosen suitable for
crystallization of a solid. (Note: think about the process of dissolving solid and
cooling the solution until the solid appear)
i. The solvent should not react with the compound that being crystallized.
ii. The solvent should be readily dissolves the liquid (solute) when the solvent is hot
but not when it is cold.
iii. The solvent should be inert but few are for example acetic acid is sometimes
used as a solvent although it will react with basic compounds.
 DATASHEET EXPERIMENT 1A
Heating by Reflux and Filtering using a Buchner Funnel

Name: 1) Muhammad Darwin Bin Mohmad Rosdi (2017256596)

2) Azmir Nurhakim Mohd Zawawi (2017256812)
3) Nur Afiqah Binti Jafri (2015804574)
4) Raja Muhammad Arashrifqi Bin Raja Adnan (2017256794)
Date : 16/03/2018
Group: RAS 113 2A
A

Observation(s)
1) During heating process After 2 minutes of heating , the water
vapour start to wrap up around the round
bottom flask .The solid (impure acetanilide)
start to dissolved into the water. The
solution turned to clear.

2) During cooling process The cooling process takes 10 minutes in

order to cool down the solution .After 10
minutes, the solution turn into the solid
crystals of acetanilide form.

3) Others

No changes
B

Solid before heating

Weight (g)

Mass of solid 2.078

Solid after heating

Weight (g)

Mass of filter paper 0.412

Mass of the solid + filter paper 2.816

Mass of the solid 2.816-0.412 = 2.404

Errors / comments Precaution

• They may be a leakage of filter
paper when filtration.
• The solution could spill out when
transfer it from the bottom flask to
the funnel.
• The filter paper had been moistened
to avoid the leakage.
• We must transfer the solution
slowly and carefully to avoid any
error to happen.

Assessment of crystal – by lecturer Scale 1-10 : (10 is the full mark)

Lecturer’s signature and date:

DISCUSSION

Based on the observation and result, the impure acetanilide dissolved in water and
the solution turned to clear due to the rate of reaction was increase towards its boiling point
during heating process. In order to become solution, acetanilide will dissolve when at high
temperature and it cannot be dissolved at low temperature. It is necessary to heat because it
will readily dissolve in hot condition. During cooling process, the solution form white
precipitate. Then, the solution was filter by Buchner filtration with vacuum to dry completely
the solid crystal and isolated from its impurities. The solid precipitates occur when the
solution cools and leaves impurities within solvent solution. Thus, it will produce the crystal
form in term of impurities in solvent solutions.
Furthermore, the errors may happen in this experiment that can affect the result of
the experiment. In order to avoid it, a few steps must be taken such as the solution must be
transfer with very carefully and slowly to avoid the solution spill out during the transfer
process from bottom flask to funnel. Then, the filter paper also must be moistened to prevent
the leakage of filter paper during filtration.
Finally, the solid crystal that obtained was transferred into a suitable container and was
put it in an oven until a couple days to make sure the solid dry completely. After a couple days,
the solid crystal mass was reported that is 20.816g.

Conclusion:
The objective of this experiment was learned that is how to set up a reflux and Buchner
filtration technique apparatus, the technique of dissolving a solid by reflux and the
importance of using reflux and Buchner filtration technique.