CHM207

Objective & Introduction

(1 mark)
Material & Methods
(1 mark)
Results (2 marks)
UNIVERSITI TEKNOLOGI MARA SARAWAK Discussion
(2 marks)
KAMPUS SAMARAHAN 2 Conclusion
(2 marks)
Q-A & Ref.
(2 marks)
Total

CHM207
ORGANIC CHEMISTRY

LABORATORY REPORT

EXPERIMENT TITLE : HEATING BY REFLUX AND FILTERING

kkkkkk.USING BUCHNER FUNNEL

EXPERIMENT NO. : 1A

STUDENT NAME : NABILAH BINTI BHARUDDIN

UiTM STUDENT ID : 2020835258

PARTNER / MEMBER NAME : - / INDIVIDU

GROUP NO. / MEMBERS NAME : NO GROUP (INDIVIDU)

DATE OF VIRTUAL EXPERIMENT (ODL): 28 October 2021

DATE OF REPORT SUBMISSION : 10 November 2021

LECTURER NAME : MS WONG MUI HUNG

 CHM207

EXPERIMENT 1
BASIC ORGANIC CHEMISTRY TECHNIQUES: REFLUX, DISTILLATION
AND EXTRACTION

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

OBJECTIVE
1. To understand how to set up a reflux apparatus.
2. To conduct virtually the setting up of the Buchner filtration system.
3. To understand the method to dissolve a solid using the reflux.
4. To know the importance of using reflux and Buchner filtration procedures.
5. To learn how to isolate the precipitate filtration under vacuum using a Buchner funnel.

INTRODUCTION
Reflux heating is beneficial for dissolving a solid material that can only be dissolved by
prolonged heating at boiling point in a suitable solvent. By using this method, the loss of the
solvent can be avoided which as the solvent is heated, the solvent vapour is cooled at the surface
of the condenser and condensed back to its liquid state again.
In addition, Buchner filtration or vacuum filtration is one of the methods used to separate
a solid product from a liquid. The mixture contains solid and liquid poured through a filter paper
in a Buchner funnel.

MATERIALS AND APPARATUS

Chemical(s) required:

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 or suitable apparatus for heating the round bottom flask
1 filter paper
 CHM207

1 Buchner funnel
1 250 ml Buchner flask
1 water aspirator or vacuum pump
*Oven for drying

DIAGRAM

Water outlet (continue to

rubber hose)

Liebig Condenser

Retort stand Condense solvent

Cold water inlet (continue to

rubber hose)
Clamp

Round bottom flask

Solvent and reactants
Heating mantle

Diagram 1

Large of solid that cannot fit through

tiny holes in filter paper and remain
here

Filter paper
Porous plate (plate with holes in)
Buchner funnel
Continue to vacuum pump

Rubber bung

Rubber tubing

Buchner flask

Filtrate (liquid that passes through

filter paper)

Diagram 2
 CHM207

PROCEDURE

1. 2 g of crude/impure acetanilide and 30 ml of distilled water, as a solvent, were added into

a round bottom flask. The solution was heated under reflux until the solid dissolved. Then
the solution was cooled at room temperature until the solid crystals of acetanilide formed.
2. A clean 250 ml Buchner flask was clamped to a retort stand and a Buchner funnel was
put with a filter paper to it. The filter paper was wetted to ensure it lies flat in order to
stop the crystals from passing through the edge and under the filter paper.
3. The Buchner filtration set was attached to a vacuum pump.
4. The solution containing the solid/crystals of acetanilide was poured into the Buchner
funnel. The vacuum was applied. The vacuum was stopped as soon as the liquid
disappeared.
5. The solid/crystals were rinsed with cold solvent (i.e. water), then the vacuum was
reapplied until the solvent disappeared.
6. The solid obtained was transferred into a suitable container and it was let to dry in an
oven.
7. The mass of solid obtained was reported after the drying process ended.
8. The percentage yield of the solid obtained was calculated.

RESULTS
A
Observation(s)
- Solid (2g of crude/impure acetanilide
During heating process dissolved in the solvent (30 ml of
distilled water))
- Solvent was boiled turns clear

- Vapour turns solvent (30 ml of distilled

During cooling process water) inside the condenser turn back
into liquid (condensed) dropping back
into the continuously boiling reaction
mixture.

Others - Volume of solvent (30 ml of distilled

water) remain the same.
 CHM207

After experiment (solid after cooling process) - Form white precipitate acetanilide in
solution.

B
Solid before heating
Weight (g)
Mass of the solid 2.0 g

C
Solid after heating
Weight (g)
Mass of filter paper 0.4 g
Mass of the solid + filter paper 1.3 g
Mass of the solid 1.3 g – 0.4 g = 0.9 g

Error (s) / Comment (s) Precaution

• The solution could spill when poured
into the Buchner funnel.
• Leaking may happen when doing the
filtration and cannot get the accurate
weight.
• Wet the filter paper first before to
avoid leakage.
• Fit the filter paper nicely in the
Buchner funnel to avoid crystal/solid
leakage into the flask.

CALCULATION

Percentage yield of the solid obtained:

=
 CHM207

DISCUSSION

From data A, observation during the heating process is that the solid of crude/impure
acetanilide is dissolved in the solvent and the solvent is boiled and turns clear. This means that
the compound was dissolved successfully in the suitable solvent when it was heated. Other than
that, the solvent chosen must be suitable for crystallization of a solid which is the solvent must
easily dissolve the solute (liquid) when heated, and insoluble as possible in the cold solvent. In
addition, the temperature at which the reaction is heated depends on the boiling points of the
solvents and also the reflux ring.
After that, during the cooling process vapour in the condenser turns back into liquid
(condensed) dropping back into the continuously boiling reaction mixture. This is because, in a
reflux setup, solvent vapour was trapped by the condenser, and the concentration of reactants
remains constant throughout the process. In this part, the loss of the solvent can be avoided which
as the solvent is heated, the solvent vapour is cooled at the surface of the condenser and
condensed back to its liquid state again.

Lastly, for the data B and C, the weight of the solid is obtained. The filter paper was
placed fit nicely on the porous plate (plate with holes in) and the filter paper was moistened with
a suitable solvent to prevent leakage. The liquid to be filtered is poured into the Buchner flask and
drawn through the perforated plate by the suction from vacuum pump. Large solids that cannot fit
through tiny holes in filter paper will remain in the Buchner funnel while the liquid that passes
through filter paper (filtrate) will remain in the Buchner flask. Buchner filtration or vacuum
filtration is suitable method at separating a solid product from a liquid.

CONCLUSION
As a conclusion, all objectives of this experiment were learned and hypothesis of this experiment
can be accepted which is reflux apparatus suitable to dissolve a solid material that can only be
dissolved by prolonged heating at a boiling point which is when heating consistently. Other than
that, the Buchner filtration apparatus are effective method to dry the crystal/solid from the solvent
using vacuum.

QUESTIONS

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

Answer: Reflux is a suitable method during prolonged heating because the method is
more suitable to dissolve a solid material that can only be dissolved by prolonged heating
 CHM207

at a boiling point which is when heating consistently. Other than that, reflux method
allows for facile heating of a solution without loss of solvent or reactant that would result
from heating in an open vessel.

2. The Buchner filtration process is well known, faster than gravity filtration, instead of this
reason why Buchner filtration chosen for filtration.
Answer: The Buchner filtration apparatus is the most effective method to dry the
crystal/solid with vacuum. Other than that, Buchner filtration is more efficient than
gravity filtration because it is much less efficient at removing residual liquid from the
solid on the filter paper.

3. Why the solid obtained need to be rinse with cold solvent during the filtration process?
Answer: The solid obtained need to be rinse with cold solvent because to remove
impurities for pure solid.

4. Give three 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)
Answer:
a) The solvent chosen should unreactive solvent and not react with the compound
that being crystallized.
b) The solvent should have a high solute solubility as well as a high potential
recovery means that when the solvent is heated, it should easily dissolve the
solute (liquid), and insoluble as possible in the cold solvent.
c) The solvent must low toxicity and inert to the compound, but some of them will
react with basic compounds such as acetic acid.

REFERENCES
1. Nichols, L. (2021, June 6). 1.4K: Reflux. Chemistry LibreTexts.
https://chem.libretexts.org/Bookshelves/Organic_Chemistry/Organic_Chemistry_Lab_Te
chniques_(Nichols)/01%3A_General_Techniques/1.04%3A_Heating_and_Cooling_Meth
ods/1.4K%3A_Reflux
2. Wikipedia contributors. (2021, June 16). Büchner funnel. Wikipedia.
https://en.wikipedia.org/wiki/B%C3%BCchner_funnel
 CHM207

3. (2021, November 6). Reflux. University of Toronto Scarborough.

https://www.utsc.utoronto.ca/webapps/chemistryonline/production/reflux.php
4. Nichols, L. (2021, August 4). 3.3C: Determining Which Solvent to Use. Libretexts.
https://chem.libretexts.org/Bookshelves/Organic_Chemistry/Organic_Chemistry_Lab_Te
chniques_(Nichols)/03%3A_Crystallization/3.03%3A_Choice_of_Solvent/3.3C%3A_De
termining_Which_Solvent_to_Use