Lab Report c1

SIC 1011
LAB REPORT C1- RECRYSTALLIZATION
PREPARED FOR: DR. LIM SIEW HUAH
NAME SUMAYYAH BINTI LOKMAN
MATRIX NO. 22003285/1
SEMESTER 1
OCCURANCE 1
DATE OF 22nd NOVEMBER 2022

EXPERIMENT
TITLE
Recrystallisation
OBJECTIVES
1. To purify the benzoic acid by recrystallisation
2. To measure the melting point of pure benzoic acid
METHODOLOGY
1. About 1.0g benzoic acid is weighed and transferred into 100-ml conical flask. 15 ml
of water and 2-4 pieces of anti-bumping granules is added. The mixture is heated on
a hot plate until the solvent boils. 2-3 ml of water is added and boiling process is
continued until all benzoic acid has dissolved
2. Fluted filter paper is prepared and placed in a funnel. The funnel is then put in a
conical flask. A little water and anti-bumping granules are added into the conical flask
and heated on a hot plate.
3. The mixture of benzoic acid is filtered through a fluted filter paper into the heated
conical flask. Add a minimum volume of boiling water to re-dissolve the crystals
formed on the filter paper. After filtration, the filtrate is boiled until a more
concentrated solution is produced.
4. The conical flask is covered with a watch glass and the solution is allowed to cool to
room temperature, then in an ice bath after the crystallization occurred.
5. When all the benzoic acid crystals have crystallized out, filter the crystals through a
Buchner funnel at suction pump. All the crystals are transferred in the flask into the
funnel by rinsing the flask with some of the filtrate. Wash the crystals with minimum
volume of cold water and air dry.
6. The crystals are placed in a watch glass to air dry. Let the crystals dry completely
before taking the melting point. The weight of pure benzoic acid recover is recorded
and percentage yield is calculated.
RESULTS
Table 1: Recrystallisation of benzoic acid
Mass of impure benzoic acid (g) 1.0

Mass of plastic bag (g) 1.3
Mass of pure benzoic acid + plastic (g) 1.9
Mass of pure benzoic acid (g) 0.6
Table 2: Melting point of pure benzoic acid crystals

Initial temperature (℃) 34
First drop of liquid (℃) 123
Liquid form (℃) 125
Melting point of pure benzoic acid range (℃) 123 - 125
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑏𝑒𝑛𝑧𝑜𝑖𝑐 𝑎𝑐𝑖𝑑 𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑

Percentage yield of pure benzoic acid = 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑖𝑚𝑝𝑢𝑟𝑒 𝑏𝑒𝑛𝑧𝑜𝑖𝑐 𝑎𝑐𝑖𝑑
× 100%
0.6
= 1.0 × 100%
= 60%
ANALYSIS AND DISCUSSION
According to Fletcher, B. (n.d.), the most crucial process for removing impurities from
nonvolatile organic solids is recrystallisation. The solute, which need to be purified is dissolved
in appropriate hot solvent in order to be purified. When the solvent cools down, the solution
becomes saturated with the solute and the solute reforms a solid by forming crystals. The
purification process is completed when the impurities are removed from the crystal lattice as
the crystal develops. The crystals can afterwards be gathered, cleaned and dried.
In this experiment, attention must be given to the melting point of recovered benzoic acid. The
melting point, or more precisely, the melting point range, of a pure substance is one of its
physical characteristics. The small range of temperatures between a substance's melting
point and the point at which all of the material has melted and the temperature at which melting
starts. Within this narrow temperature range, the substance changes between its solid and
liquid states (Recrystallisation of Benzoic Acid and Determination of Its Melting Point (A)
Recrystallisation Theory, n.d.). The standard melting point of benzoic acid is 122.3⁰C.
From this experiment, the melting point of pure benzoic acid range obtained is 123 - 125⁰C
and the experimental melting point is 125⁰C. The experimental range of melting point is slightly
higher than the theoretical range may be caused by the heat source temperature is too high,
causing the melting point to overshoot. The percentage yield of pure benzoic acid is 60%
which is quite low. This low percentage yield may result from the crystallization that occur on
the fluted filter paper during the filtration of benzoic acid mixture into the conical flask. Thus,
the pure benzoic acid mass retrieved from the experiment is only 0.6 g. This error can be
prevented by adding boiling water to dissolve the crystals formed on the fluted filter paper.
The precaution steps for this experiment include putting some anti-bumping granules into the
mixture to make it boil smoothly. Secondly, avoid using too much water to dissolve the mixture
as it will affect the recrystallisation process. Other than that, fold the filter paper as much as
possible so that it will stick to the filter funnel wall when wet. Furthermore, transfer the mixture
of benzoic acid quickly as soon as the benzoic acid dissolve completely to avoid the mixture
vaporized. Lastly, use rubber stopper during the suction filtration to prevent air flow.
CONCLUSION
Recrystallization is a common method for product purification in the large chemical and
pharmaceutical industries. For instance, to obtain sugar crystals, recrystallization is utilised in
the manufacturing of sugar from syrupy sugar mixtures. To accelerate the process, seeding
is done. Sea water is converted into salt by allowing it to evaporate in big pools. When this is
carried out, the salt crystallizes (Recrystallisation of Benzoic Acid and Determination of Its
Melting Point (A) Recrystallisation Theory, n.d.). The range of melting point of benzoic acid
recovered is 123-125⁰C meanwhile the melting point of benzoic acid recovered is 125⁰C which
is slightly higher than the theoretical melting point of pure benzoic acid which is 122.3⁰C. The
p e r c e n t a g e y i e l d o f b e n z o i c a c i d r e c o v e r e d f r o m t h i s e xp e r i m e n t i s 6 0 % .
QUESTIONS
1. Anti-bumping granules offer nucleation sites, allowing the liquid to boil easily and
smoothly without overheating (Boiling_chip, n.d.).
2. Recrystallisation is a purification technique that uses variations in solubility and

temperature to separate a desired product from a mixture of contaminants. The
product is dissolved in a heated solvent and then allowed to cool in the
recrystallization process. The product's crystals will reform as a purer final result
(Study.com, n.d.).
3. With solid seals and a reliable vacuum source, suction filtration can be completed
much more quickly than gravity filtration. Purer solids are produced through suction
filtering, which is more effective at eliminating leftover liquid. Since the liquid may
contain soluble contaminants that could reabsorb back onto the solid surface after
the solvent evaporates, this is particularly crucial when crystallization occurs
(Nichols, 2020).
4. To wash the crystals, add minimum amount of cold solvent (distilled water) and dry is
using Buchner funnel and suction pump.
5. The solvent need to be removed because a compound's melting point will be low
and/or wide if it contains the solvent for recrystallization (Kilway & Clevenger, 2006).
6. A good recrystallization solvent has the ability to quickly dissolve compounds when it
is warm, but is less soluble when cooled in an ice bath or at room temperature. The
solvent should have a low boiling point (typically below 100⁰C). Water is a poor
recrystallization solvent for the majority of organic molecules (Lprecrystal, n.d.)
REFERENCE
1. Recrystallization. (n.d.). https://sites.pitt.edu/%7Eceder/add_info/recrystallization.html
2. Recrystallisation of benzoic acid and determination of its melting point (a)

Recrystallisation Theory. (n.d.). Retrieved November 26, 2022, from
https://mccscience.yolasite.com/resources/EXP%207.1.pdf
3. Study.com. (n.d.). Take online courses. earn college credit. Research Schools,
Degrees & Careers. Study.com | Take Online Courses. Earn College Credit.
Research Schools, Degrees & Careers. Retrieved November 27, 2022, from
https://study.com/academy/lesson/recrystallization-procedure-purpose.html
4. Nichols, L. (2020, August 11). 1.5D: Suction Filtration. Chemistry LibreTexts.

https://chem.libretexts.org/Courses/SUNY_Oneonta/Chem_221%3A_Organic_Chemi
stry_I_(Bennett)/2%3ALab_Textbook_(Nichols)/01%3A_General_Techniques/1.05%
3A_Filtering_Methods/1.5D%3A_Suction_Filtration
5. Kilway, K. V., & Clevenger, R. (2006). Recrystallization [Review of Recrystallization].

Department of Chemistry, University of Missouri.
http://d.web.umkc.edu/drewa/chem321l/Handouts/Lab01HandoutCrystallization321L.
pdf
6. lprecrystal. (n.d.). Organicchem.org.

http://organicchem.org/oc2web/lab/exp/lp/lprecrystal.html

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SIC 1011

LAB REPORT C1- RECRYSTALLIZATION

PREPARED FOR: DR. LIM SIEW HUAH

NAME SUMAYYAH BINTI LOKMAN

MATRIX NO. 22003285/1

DATE OF 22nd NOVEMBER 2022

Mass of impure benzoic acid (g) 1.0

Table 2: Melting point of pure benzoic acid crystals

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑏𝑒𝑛𝑧𝑜𝑖𝑐 𝑎𝑐𝑖𝑑 𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑

2. Recrystallisation is a purification technique that uses variations in solubility and

1. Recrystallization. (n.d.). https://sites.pitt.edu/%7Eceder/add_info/recrystallization.html

2. Recrystallisation of benzoic acid and determination of its melting point (a)

4. Nichols, L. (2020, August 11). 1.5D: Suction Filtration. Chemistry LibreTexts.

5. Kilway, K. V., & Clevenger, R. (2006). Recrystallization [Review of Recrystallization].

6. lprecrystal. (n.d.). Organicchem.org.

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