OBJECTIVE

To perform batch crystallization process utilizing the evaporation method.

To examine the rate of evaporation and crystallization in a batch process.

SUMMARY

The products of chemical reactions can be impure. Purification of products must be performed to
remove by-products and impurities. Crystallization is a method of purifying a solid. There are
two types of impurities which are more soluble in a given solvent than the main component and
those less soluble. The main objectives in this experiment are to perform batch crystallization
process utilizing the evaporation method and to examine the rate of evaporation and
crystallization in a batch process. First of all, the mass used for benzoic acid is 1 gram. The
benzoic acid has been mixed with 15 mL of water and heated on a hot plate, while stirring the
mixture and boiling gently to dissolve the benzoic acid. After it boiled, the mixture was filtered
with filter paper and poured into new conical flask. The filtered benzoic acid plus water
precipitate was heated once again until it dissolved like clear water. It has been cooled for a few
minutes and the conical flask was put into the ice bath for the crystallization to occur. In
crystallization, the solution is concentrated and usually cooled until the solute concentration
becomes greater than its solubility at that temperature. Then the solute comes out of the solution
forming crystals of approximately. Based on the results, the yield of the crystal from experiment
is 29%. On the other hand, the yield of crystal obtained from the material balances calculation is
0.45 gram or 45%. Thus, the yield of material balance is higher than yield of crystal from the
experiment. Plus, the yield was smaller than the theoretical yield because of some impurities
might occur in the process. Not only that, this crystallization is not that efficient enough due to
some less amount of percentage of crystal achieved compared to the crystal achieved via
theoretical. After that, there might have some error where when solution is placed on the hot
plate that cause the heating with open of the beaker causes the loss of certain amount in air by
diffuse due to not uniformly stirred the mixture. The recommendation on this experiment was
avoid all the present of such impurities that effect the result thus gain lower result value than the
theoretical amount. When the collected moist crystals should be placed in a vacuum dryer instead
of drying it in open space.

RESULTS

Before Crystallization
Mass of Benzoic Acid = 1.0 g
Mass of Distilled Water = 15 ml

After Crystallization
Mass of Filter Paper = 0.81 g
Benzoic Acid = 1.05 g
Mass of Crystal + Filter Paper = 1.10 g
Mass of Crystal = 0.29 g

Mass of Benzoic Acid obtained after crystallization

% Yield of Crystal = Mass of Benzoic Acid before cyrstallization 100%

0.29 g
= 100
1.0 g

= 29%
 Mass of Water

3
1000 kg 1m 1L 1000 g
15 ml 3

m 1000 L 1000 mL 1 kg

= 15 g of Water

Overall Material Balance

B+W=M+C+W
1.05 g of Benzoic Acid +15.0 g of Water = M + C + 15.0 g of Water
S = - C 1.0 g (1)

Mass Balance of Sulfur

60 wt
S= 1.0 g
100

S = 0.6 g (2)
Mass Balance of Crystal
Substitute 2 into 1

S = - C 1.05 g
C = 1.0 g 0.6 g
C = 0.45 g of Crystal

DISCUSSION

The main objectives of this experiment are to perform batch crystallization process utilizing
the evaporation method. Moreover, it is to examine the rate of evaporation and crystallization in
a batch process. Based on the result calculated, the yield of the crystal from experiment is 29%.
On the other hand, the yield of crystal obtained from the material balances calculation is 0.45
gram or 45%. Thus, the yield of material balance is higher than yield of crystal from the
experiment. The experiment yield percentage does not similar with the theoretical yield. The
yield results shown the crystallization process in the experiment only achieved 29% from the
45%. It shown the reaction of crystallization was not efficient. In addition, the yield was smaller
than the theoretical yield because of some impurities might occur in the process.

Crystallization is a separation process where solid particles form within a homogenous liquid
phase due to supersaturation induced either through cooling or evaporation. It is essentially a
solid-liquid separation techniques and a very important one at that. An important example is the
production of sucrose from sugar beet, where the sucrose is crystallized out from aqueous
solution. This process can occur in the freezing of water to form ice, in the formation of snow
particle from a vapor, in the formation of solid particle from liquid melt, or in the formation of
solid crystals from a liquid solution. (Gupta, B. & Ibrahim, S., 2000)

Based on the objectives, the experiment was conducted started with weighting the filter paper
and benzoic acid. The mass used for benzoic acid is 1 gram. The benzoic acid has been mixed
with 15 mL of water and heated on a hot plate, while stirring the mixture and boiling gently to
dissolve the benzoic acid. After it boiled, the mixture was filtered with filter paper and poured
into new conical flask. The filtered benzoic acid plus water precipitate was heated once again
until it dissolved like clear water. It has been cooled for a few minutes and the conical flask was
put into the ice bath for the crystallization to occur.

When the crystals have formed completely, the solid chemical was collected by setting up a
vacuum (suction) filtration on a properly fitted filter paper in a clean Bchner funnel apparatus.
The chilled mixture was poured into the Buchner funnel. The water was filtered quickly. The
aspirator run for a few minutes to start air-drying the crystals. A spatula was used to lift the filter
paper and crystals out of the Buchner funnel. The crystal was dry completed at the room
temperature and weight to collect the result. (Slund, B. & Rasmuson, ., 1992)

The crystallization occur in this experiment during the heating of the benzoic acid plus water
that make seed of crystallization to appeared. Benzoic acid is a colourless crystalline solid. It is
highly soluble in hot water, but poorly soluble in cold water. It can be recrystallised by
dissolving it in hot water. The hot solution obtained is filtered and cooled. Upon cooling, white
crystals of benzoic acid was crystalize. The factors that influenced the yield of crystals is lack of
solvent added when the benzoic acid was dissolved. Besides that, some of the solutions was
spilled a little and reduce the yield of experiment. Given that the original sample is a mixture
containing the substance that wish to be isolate and other substances, extra solvent added could
cause other substances in the mixture to dissolve along with the substance that need to
recrystallize. This could result in low purity. Moreover, presence of another substance in the
mother liquor also can affect the yield. The rate of cooling are another factors of the influenced.
(Sthl, M., slund, B., & Rasmuson, ., 2001)

CONCLUSION AND RECOMMENDATION

This experiment can be concluding as per the objectives of this experiment which is to
perform batch crystallization process utilizing the evaporation method. However, it is to examine
the rate of evaporation and crystallization in a batch process. Based on the result of the
experiment it is known that the yield of material balance is higher than yield of crystal from the
experiment. Crystallization is a separation process where solid particles are separated from the
liquid phase due to super saturation induced either through cooling or evaporation. This
crystallization is not that efficient enough due to some less amount of percentage of crystal
achieved compared to the crystal achieved via theoretical. In this experiment the crystallization
occurs during the heating of the benzoic acid plus water that make seed of crystallization to form
in small solid pieces. The level of the purity of the crystal might be affected by the extra solvent
added could cause other substances in the mixture to dissolve along with the substance that need
to recrystallized. In this experiment there some mistakes that might happen which causes the low
reading of crystallization where as the it might occur when the measurement of benzoic acid of 1
gram is weight, when solution is placed on the hot plate that cause the heating with open of the
beaker causes the lost of certain amount in air by diffuse and when the stirring process might
occur slight error due to not uniformly stirred the mixture. In recommend it is also can be
recommended that the experiment should been taken with high concern to avoid all the present
of such impurities that effect the result thus gain lower result value than the theoretical amount.
When the collected moist crystals should be placed in a vacuum dryer instead of drying it in
open space where the temperature and the surrounding organism can reaction with open filter
paper which consists of moist crystal form.

REFERENCES
Gupta, B. & Ibrahim, S. (2000). Mixing and Crystallization (1st ed.). Dordrecht: Springer
Netherlands.
Slund, B. & Rasmuson, . (1992). Semibatch reaction crystallization of benzoic
acid. Aiche Journal, 38(3), 328-342. http://dx.doi.org/10.1002/aic.690380303
Sthl, M., slund, B., & Rasmuson, . (2001). Reaction crystallization kinetics of
benzoic acid. Aiche Journal, 47(7), 1544-1560. http://dx.doi.org/10.1002/aic.690470708