1.

0 OBJECTIVES
1)
2)
3)
4)
5)

To compare the yield of crystals with the yield of crystals obtained theoretically.
To explain how the crystallization occurs in this experiment.
To perform batch crystallization process utilizing the evaporation method.
To examine the rate of evaporation and crystallization in a batch process.
To discuss the factors that influenced the yield of crystals.

2.0 Abstract

Crystallisation is the slow precipitation of crystals from a solution of a substance. This

experiment is carry out to perform batch crystallization process utilizing the evaporation
method, to compare the yield of crystals with the yield of crystals obtained theoretically and
to discuss the factors that influenced the yield of crystal. The experiment started with
obtaining the mass of crystal by evaporating the concentrated benzoic acid, C7H6O2. After the
crystal has been formed, the material balance of this experiment was calculated. Throughout
the experiment, the theoretical value of percentage of yield of crystal (%) is 49%, while the
experimentally value is 58%. There are several factors that cause the difference between the
experimental and theoretical values, such as excess of used solvent and did not dissolve
completely.

Material balance:
Result theoretically:

W kg H2o

Cooler and Crystallizer

S kg C6H5COOH

1 g of
C6H5COOH +
15 ml H20
60% mole C6H5COOH
C kg crystals,
C6H5COOH. H2O

40% mole sulphur

Material balance
We assume W=0
15 = 100/106.8 (S) + 18.02/140.14 (C) + 0 eq. 1
0.6 = 6.8/106.8 (S) + 122.12/140.14 (C) + 0 eq. 2
Solve the equation simultaneously:
S= 2.72 g
C= 0.49 g
Thus the mass of the crystal theoretically = 0.49 g
Percentage yield of crystal= 0.49/1 x 100%
= 49%

3.0 RESULT/DATA:
Before crystallization:

Mass of benzoic acid: 1.02 g

Mass of distilled water: 15 ml = 15 g
After crystallization:
Mass of filter paper: 0.32 g
Mass of crystals + filter paper: 1.45 g
Mass of crystals: 0.58 g

Mole fraction of benzoic acid: 0.4 mole

Mole fraction of sulphur: 0.6 mole

Mass of benzoic acid: 0.4 x 1.02 g = 0.408 g

Mass of sulphur: 1.02 g - 0.408 g = 0.612 g
Solubility of benzoic acid in water (20C): 0.29 g/100 mL
Molecular weight of benzoic acid: 122.12 g/mole

Equation:
We assume the mole of H2O = 1
C6H5COOH (aq) + H2O (l)

C6H5COOH (aq). H2O (l)

Result experimentally:
% yield of crystal = 0.58/1 x 100%
= 58%

4.0 DISCUSSION

The purpose of conducting this experiment is to compare the yield of crystals with the
yield of crystals obtained from the calculation by doing the material balance. Secondly, is to
explain how the crystallization occurs in this experiment. Thirdly is to perform batch
crystallization process utilizing the evaporation method. Next, is to examine the rate of
evaporation and crystallization in a batch process. Last but not least, is to discuss the factors
which influenced the factors which will influences by the yield of crystals.
The most commonly used technique for purifying a solid compound is crystallization.
Crystallization is a process where solid particles are formed from a homogenous phase.
(Geankoplis C. J. (2014). Transport Process and Separation Process Principle. UK. Pearson
Education Limited.). In the most basic form of this process, the solid compound is dissolved
in a minimal amount of a hot solvent, and then the solution is allowed to cool until the
compound precipitates, or crystallize, from a super-saturated solution. Impurities, which often
are soluble in the solvent, stay dissolved, and these impurities are removed, along with the
solvent by filtration. The success of this technique depends heavily on the solvent being
used. The solid compound (solute) must be only slightly soluble in the solvent at room
temperature, while being virtually completely soluble in the solvent at higher temperatures. In
addition, it is vital that the solvent not react with the compound which is being purified.
(Separation of Solids: Recrystallization and Melting Points. 14 th November 2012. Retrieved
from https://www.miracosta.edu/home/dlr/210exp1b.htm)
From the material balances that have been calculated, the percentage yield of crystals
theoretically is 49% while the percentage yield of crystals experimentally is 58%. So, it can
be concluded that the percentage yield of crystals experimentally is quite differ from the
theoretical. Thus, the percentage yield of crystal experimentally is higher than the percentage
yield of crystal theoretically. However, it is supposedly the value of the percentage yield of
crystal theoretically should be higher than the value of experimentally. This is because when
heating the benzoic acid the temperature was set higher than 100C.

There are several factors that can influence the yield of crystals. Firstly, is solvent.
Solvent with moderate solubility is the best choice in order to avoid super-saturation. Supersaturation may leads to sudden precipitation and will cause the crystal's size smaller. Other

than that, hydrogen bonding can help the crystallization as well as the presence of benzene
can helps the crystal's growth. The second factor is nucleation. In a solution at a given
temperature, the thermodynamics difference between small and large particles or crystals is
that the small crystals has a significant amount of surface energy per unit mass, whereas the
large particle does not. As a result, the solubility of a small crystal of less than micrometer
size is greater than that of a larger size crystal. In simple words, the less number of nucleation
are better. The third factor is time. The faster crystallization is as not good as a slower
crystallization because usually the faster crystallization will results with low quality of
crystals. (McCabe W. L., Smith J. C. and Harriot P.. (1993). Unit Operation of Chemical
Engineering

[Kindle

Version].

Retrieved

from

http://www.eng.unideb.hu/userdir/deak.krisztian/UNIT%20OPERATION
%20HANDBOOK_red_6.pdf

5.0 CONCLUSIONS AND RECOMMENDATION

In this experiment, the comparison made have state that the percentage yield of
crystals experimentally is higher compared to the percentage yield of crystals theoretically.

Furthermore, the process of the crystallization has been explained. While batch crystallization
process has been performed by utilizing the evaporation method, the rate of evaporation and
crystallization in a batch process has been examined. There are several factors that affects the
yield of crystal obtained which are solubility of the solvent used, nucleation, the time taken
for crystallization, and last but not least hydrogen bonding with the presence of benzene.
There are some recommendations to achieve the objectives of this experiment
successfully. Firstly, hot water must be used to rinse the benzoic acid solution after filtration
takes place in order to avoid further crystallization to occur. Secondly, minimum usage of
solvent to dissolve the benzoic acid must be used to allow crystallization to happen easily.
Thirdly, the filter paper and filter funnel must be very dry to avoid any moist that will affect
the result. Last but not least, the mass of the impure benzoic acid solute must be weigh
precisely and accurately.

6.0 REFERENCE

i.

Geankoplis C. J.2014. Transport Process and Separation Process Principle. UK.

ii.

Pearson Education Limited. 818-825.

Separation of Solids: Recrystallization and Melting Points. 14 th November 2012.
Retrieved from https://www.miracosta.edu/home/dlr/210exp1b.htm. Accessed on 20th

iii.

February 2016.
McCabe W. L., Smith J. C. and HarriotP.. (1993). Unit Operation of Chemical
Engineering. Library of Congress Cataloging-in-Publication Data Retrieved from
http://www.eng.unideb.hu/userdir/deak.krisztian/UNIT%20OPERATION
%20HANDBOOK_red_6.pdf. Accessed on 20th February 2016.