CHM 258

LABORATORY REPORT

EXPERIMENT 1 : RECRYSTALLIZATION OF VANILLIN

DATE OF EXPERIMENT : 17/09/2019

GROUP : AS1203D
NAME : DAYANG NOR EMELIA BINTI AWANG MUSTFA
STUDENT ID : 2018284036
PREPARED FOR : MADAM NURR MARIA ULFA SERUYI
Objectives
1. To purify the crude vanillin through recrystallization technique.
2. To determine the recovery percentage of recrystallized vanillin.

Questions

1. Define percent recovery.

Percent recovery is the percentage of an original substance that is recovered after a chemical
reaction is completed.

2. Vanillin solution is cooled in an ice bath before vacuum filtration. Briefly explain.

Vanillin solution is cooled in an ice bath before vacuum filtration to enable the vanillin crashed
out from the solution and form crystal. Ice-cooled distilled water is used to wash the crystal to
prevent the crystals back into solution. Thus, it can help to remove left impurities. After that,
the vanillin crystal are filtered using vacuum filtration to fully dry the crystals.

3. Discuss on how the recrystallization technique remove solvent soluble impurities.

The recrystallization technique remove solvent soluble impurities by dissolving both impurities
and desired compound into a hot appropriate solvent to fully dissolve the mixture. The
impurities are much soluble compare to the desired compound, so it will be evaporated and will
be removed. Let the solution cools down slowly to form the crystal and wash it with cool water
to remove the remaining impurities. The pure crystal can be obtained after the filtration.

4. Gravity and vacuum filtration separate insoluble solids from a liquid phase. The choice depends
on conditions. Suggest criteria you would apply to choose between them.

Gravity filtration is a general filtration where the mixture is filter by using the gravity. The
mixture is poured from above onto the filter paper, the liquid flows below it. The gravity will
pull down the liquid and solid left on the filter paper. Meanwhile, vacuum filtration use Büchner
flask and hose to create vacuum. The vacuum will suck the liquid from the filter paper. This
method is faster than gravity filtration and more efficient in removing residual liquid.
Results

Mass of crude vanillin + 167.76 g

container
Mass of container 165.76 g
Mass of crude vanillin 2.0000 g
Mass of filter paper 0.5081g
Mass of filter paper + 0.6225 g
recrystallized vanillin
Mass of recrystallized vanillin 0.1144 g

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑢𝑏𝑠𝑡𝑎𝑛𝑐𝑒 𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑

Recovery Percentage = × 100%
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑢𝑏𝑠𝑡𝑎𝑛𝑐𝑒 𝑢𝑠𝑒𝑑 𝑖𝑛𝑖𝑡𝑖𝑎𝑙𝑙𝑦

0.1144𝑔
= × 100%
2.00𝑔

= 5.72 %
Discussion

The difference between the mass of crude vanillin and recrystallization vanillin is due to
the impurities contained in the crude vanillin. The mass of recrystallized vanillin is lower than
the crude vanillin. During the experiment, the impurities was removed by the vacuum filtration
method. Distilled water was used in the experiment because it was a good solvent and does not
dissolve the vanillin at low temperature. The solubility of vanillin is increase when there is an
increase in the temperature. The vanillin solution was cooled in an ice bath before vacuum
filtration to enable crashed out from the solution and form into crystal. The solubility of the
impurities in cold solution is higher than the vanillin. Therefore, the mixture was able to
separate and crystal vanillin was obtained after the filtration. The result obtained is not really
accurate compared to the theoretical results. This maybe because of some errors occur during
conducting the experiment. Systematic errors can be included from the uncertainties in the
calibration of the laboratory equipment. Human errors also occur such as splitting some of the
crude vanillin and the residue of the recrystallized vanillin may be still attached on the filter
paper.

Conclusion

In conclusion, we were able to prove the principle behind the recrystallization and aim our
objectives which are to purify the crude vanillin through recrystallization technique and
determine the recovery percentage of recrystallized vanillin although there was some errors
occur during the experiment,
References
Bryant, S. (2015, March 12). What is the difference between gravity and vacuum filtration? Retrieved
from Cam Lab: https://camblab.info/wp/index.php/what-is-the-difference-between-gravity-
and-vacuum-filtration/

Helmenstine, A. M. (2019, September 08). Filtration Definition. Retrieved from thoughtco:

https://www.thoughtco.com/filtration-definition-4144961

Judge, M. (2018, April 30). How To Calculate The Percentage Recovery of a Product. Retrieved from
Sciencing: https://sciencing.com/calculate-percentage-recovery-product-8741204.html

Yoder, C. (n.d.). Recrystallization. Retrieved from Wired Chemist:

http://www.wiredchemist.com/chemistry/instructional/laboratory-tutorials/recrystallization