UNIVERSITI KUALA LUMPUR

MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING

TECHNOLOGY
LABORATORY REPORT COVER PAGE

SECTION A – To be filled up by Student

Subject Code & Subject CPB21404 SEPARATION PROCESS
Title of Experiment Recrystallization of Benzoic Acid
Date of Experiment 10/4/2019 Date of Submission 17/4/2019
Name & ID No. 1)Ahmad Hafizzudin bin Jisfery
2) Ameera Arisya bt Abdul Halim
Group No: ( )
3) Aiman Afiq bin Fakarrudy
4)Salma Raimi Nazurah bt Rosli
Name of Lecturer DR. NOR SHAHIRAH MOHD NASIR
*Penalty:
 For any late of submission, the mark will be reduced by 5% per day to a maximum of 3 days, after which it
will NOT BE ACCEPTED.
 Plagiarism will not be tolerated and will be given ZERO.

SECTION B – To be filled up by Lecturer

Very Poor Poor Satisfactory Good Excellent Marks

Criteria
(1) (2) (3) (4) (5)
Report format (5%)
1 2 3 4 5
1.Organization of the report.
Summary (10%) – max 1 page
1.Brief review on the objectives of the experiment, major 2 4 6 8 10
findings and significant conclusions
Introduction & Theory (10%) – max 2 pages
1. State the background to the experiment conducted.
2 4 6 8 10
2. Summary of theories including formulations related to
the experimental work.
Data & Results (10%)
1. Data are presented as deemed suitable with complete 2 4 6 8 10
labels and units.
Analysis & Discussion (40%)
1. Explanations of the referred table and figure are
presented after the table and figure 8 16 24 32 40
2. Discuss on the findings and relations to the theory and
objective of experiment
Conclusion & Recommendation (10%)
1.Summary of the results to relate the findings or results
with the theory applicable to the experimental 2 4 6 8 10
2.Suggest improvements in apparatus or measurement
procedure, or experimental procedures for future
References & Appendices (5%)
1. Cite references in the text.
2. References taken from books, journals and articles. 1 2 3 4 5
References from website are not recommended.
3. Put raw data and sample calculation.
TOTAL (90%)

Laboratory Psychomotor Assessment (10%) Student 1 Student 3

Individual practical skills Student 2 Student 4
Student 1 Student 3
TOTAL (100%)
Student 2 Student 4

Date of Submission:
Received by:
Stamp
Student Slip Received
Date of Submission:
Student Name & ID.:
Experiment title:
Received by:

Summary
 UNIVERSITI KUALA LUMPUR
MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING
TECHNOLOGY
LABORATORY REPORT COVER PAGE

The objectives of this experiment are to purify benzoic acid by crystallization and to
determine the melting point of pure benzoic acid. Crystallization is the process of purifying
organic compounds that are solid at room temperature by using solvents. The solid used in this
experiment is benzoic acid. Crystallization of benzoic acid is done to remove by-products and
impurities present in the benzoic acid to get pure benzoic acid. Based on the result obtained the
weight of the recrystallized benzoic acid is less than the impure benzoic acid. The mass of
impure benzoic acid are decrease at the end of the experiment. Then, the %recovered is
calculated. The purity of the solid is verified using the melting point. The impure solid have
lower melting point than pure solid. The more amount of impure compound dissolved, the better
the recrystallization solvent. Overall, the objectives of the experiment are achievable.
 UNIVERSITI KUALA LUMPUR
MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING
TECHNOLOGY
LABORATORY REPORT COVER PAGE

Introduction and Theory

Producing pure substances is a very important process, especially in the pharmaceutical industry.
Separating insoluble solids from solvents is easily achieved using a simple technique
called filtration. Soluble solids again are easily separated from solvents by evaporation, and
chromatography is used to separate a mixture of liquids.  But what happens when we have two
soluble solids that we want to separate? In this lesson we will look at recrystallisation, a
commonly-used process in the pharmaceutical industry. 

Recrystallisation is a very important purification technique, purifying substances by removing

unwanted by-products. It is also used to manufacture the correct crystal size and shape of a
material. These factors can have a very significant impact on how a medicine acts when taken by
a patient. The same principles and techniques of recrystallisation can be applied both on a
laboratory and industry scale. 

The process depends on two principles; the fact that substances tend to be more soluble in a hot
solvent than in cold solvent, and that each solute tends to behave as though it were alone in the
solvent. Using the correct solvent is a very important part of the process. The solute must be
insoluble in the solvent at room temperature, and as the temperature of the solvent increases, the
solubility of the solute also increases. It is also important that the impurities present are soluble
in the solvent at room temperature and insoluble at higher temperatures.
 UNIVERSITI KUALA LUMPUR
MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING
TECHNOLOGY
LABORATORY REPORT COVER PAGE

Data and Result

Data on the impure Benzoic Acid

a. Mass of Benzoic acid + Weighing paper: 2.1 g

b. Mass of weighing paper: 1.06 g
c. Mass of impure benzoic acid: 1.04 g

Data for recrystallized benzoic acid

a. Mass of recrystallized benzoic acid + Weighing paper: 1.31 g

b. Mass of weighing paper: 1.06 g
c. Mass of recrystallized benzoic acid: 0.25 g
d. Calculation of percentage recovery:
%Recovered= Weight benzoic acid after recrystallization/weight of benzoic acid before x
100
= 0.25/1.04 x100
= 24.04%
e. Melting point of recrystallized benzoic acid: 116 degree C

Melting point of recrystallized benzoic acid (Theory): The melting point of the crude benzoic
acid was 118-122 degree C, while the melting point of the recrystallized benzoic acid was 121-
127 degree C.
 UNIVERSITI KUALA LUMPUR
MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING
TECHNOLOGY
LABORATORY REPORT COVER PAGE

Analysis and Discussion

The objectives of this experiment are to purify benzoic acid by crystallization and to
determine the melting point of pure benzoic acid. Crystallization is the process of purifying an
organic compounds that are solid at room temperature by using solvents. The solid used in this
experiment is benzoic acid. Crystallization of benzoic acid is done to remove by-products and
impurities present in the benzoic acid to get pure benzoic acid. Although crystallization is not a
perfect process, but it does increase the purity of the final product.

The experiment starts by weighing 1g of benzoic acid. 15 ml of water and anti bumping
granules are added. The mixture is heated on a hot plate until the solvent boils. The fluted filter
paper is put into the oven until it is ready to be used. Then, 20ml of water in a beaker is heated.
Once the solution boils, it is filtered through a fluted filter into the conical flask. Add minimum
amount of boiling water to dissolve any crystals formed on the filter paper. After that, small
volumes of solvent are added until all the crystals are dissolved. Next, the filtrate is boiled. The
solution is allowed to cool at room temperature until crystallization occurs. After it occurs, it is
placed in an ice bath. After some time, the crystals formed are filter through a Hirsch/buchner
funnel and the filter paper containing the crystals are left to dry for 4 hours. After 4 hours, the
weigh of pure benzoic acid recovered is weighed.

Based on the results recorded, it can be seen that the weight of recrystallized benzoic acid
is lesser than the impure benzoic acid. The impure benzoic acid at the start of the experiment is
1.04 g while the weight of recrystallized benzoic acid at the end of the experiment is 0.25g.
There is a huge difference between the both of them which is 0.79g. The percentage recovery of
the benzoic acid is 24.04%. Percentage recovery computes the percentage of an original
substance that is recovered after a chemical reaction is completed (Patkar, 2019). Percentage
recovery can determine the efficiency of the process (Patkar, 2019). It can be calculated by using

the formula

. There are two

types of percentage yield which are above 100% and below 100%. The percentage yield that is
above 100% is an inaccurate value which may be due to error in weighing or calculating.
 UNIVERSITI KUALA LUMPUR
MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING
TECHNOLOGY
LABORATORY REPORT COVER PAGE

Theoretically, the value below 100% is the desired value. Therefore, the experiment obeys the
theory.

The purity of the solid can be verified by taking the melting point. Based on theory, the
melting point of the crude benzoic acid is 118 ᵒC - 122 ᵒC while the melting point of
recrystallized benzoic acid is 121 ᵒC – 127 ᵒC. Impure solid usually have lower melting point
than pure solids. The method of purification is based on the principle that the solubility of most
solid increases when temperature increases. This means that the amount of benzoic acid that can
be dissolved in a solvent increases when the temperature is increased. A good (suitable)
recrystallization solvent will dissolve a large amount of the impure compound at temperatures
near the boiling point of the solvent (Libretexts, 2019).

In conclusion, the experiment was a success as the objectives which are to purify benzoic
acid by crystallization and to determine the melting point of pure benzoic acid, are achieved.
 UNIVERSITI KUALA LUMPUR
MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING
TECHNOLOGY
LABORATORY REPORT COVER PAGE

Conclusion and Recommendation

The recrystallization of benzoic acid experiment aims to purify benzoic acid by
crystallization and to determine the melting point of pure benzoic acid. This observation in this
experiment is based on the mass of impure benzoic acid and the recrystallized benzoic acid.
Based on the result, it can be conclude that mass of recrystallized benzoic acid is lesser
compared to the mass of impure benzoic acid with the difference of 0.79g. The percentage
recovery of the benzoic acid is 24.04% which abide the theory. Furthermore, based on theory the
melting point of the crude benzoic acid is 118 ᵒC - 122 ᵒC while the melting point of
recrystallized benzoic acid is 121 ᵒC – 127 ᵒC. Overall, the objectives of the experiment are
achievable.

It is known that the experiment conducted can have more accurate values if the errors in
the experiment are reduced. When weighing the mass of impure benzoic acid and recrystallized
benzoic acid, it is recommended to ensure that there is no vibration around the weighing balance
as the weighing balance is very sensitive. Another error that can be taken into account is when
filtrating the solution of benzoic acid, it is found that there are residue in the filter funnel. It is
recommended to ensure all the solid benzoic acid to filtrated so that there will be less errors in
weighing the mass of recrystallized benzoic acid.
 UNIVERSITI KUALA LUMPUR
MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING
TECHNOLOGY
LABORATORY REPORT COVER PAGE

References

Libretexts. (2019). Recrystallization. Available at

https://chem.libretexts.org/Bookshelves/Physical_and_Theoretical_Chemistry_Textbook_Maps/

Supplemental_Modules_(Physical_and_Theoretical_Chemistry)/Physical_Properties_of_Matter/

Solutions_and_Mixtures/Case_Studies/RECRYSTALLIZATION

Retrieved on 16 April 2019.

Patkar, P. (2019). How to Calculate Percent Recovery. Available at

https://sciencestruck.com/how-to-calculate-percent-recovery

Retrieved on 16 April 2019.