UNIVERSITI TEKNOLOGI MARA

CAWANGAN PERAK
KAMPUS TAPAH
Faculty of Applied Sciences
Diploma in Science

CHM 258
Introduction To Organic Chemistry
LABORATORY REPORT

EXPERIMENT 2:
MELTING POINT DETERMINATION

CLASS : A4AS1203_4

NO NAME STUDENT ID
1. NUR ALIAH NATASHA BINTI NAZRI 2017441596
2. NUR HEZRIN ALIA BT ZAMAN HURI 2017802754
3. UMUL JASRINA BT SIED ABD JALIL 2017635534
4. NUR AQILAH AINAA BT SAHROL 2017644738
5. SITI ZULAIKHA BT ZULKEFLI 2017680442
6. NUR KESUMA BT ISHAK 2017403804

LECTURER : PN. NAZRIZAWATI AHMAD TAJUDDIN

DATE OF SUBMISSION : 4 October 2018

PROCEDURE

1. The capillary tube was filled by pressing the open end onto the powdered sample until
there is a 1cm length of sample in tube.
2. The capillary tube was dropped, sealed down through a 1m piece of 6mm glass tubing
that is being held on a hard surface.
3. The dropping procedure was repeated until the sample was packed in the bottom of
the tube.
4. The capillary tube was placed in the sample holder of the melting point apparatus.
5. ON button was pressed and the plateau light was observed. The set button was
pressed until the heat light turned on when the plateau light is on.
6. The melting point of sample was recorded when the heat light is on.
7. The sample was observed through magnifying eyepiece part.

Figure 1.1: the melting point apparatus

(http://www.writeopinions.com/melting-point-apparatus)

RESULTS

SAMPLE MELTING POINT (°C)

START COMPLETE
A 50 88
B 50 85
C 50 79
QUESTIONS

1. Discuss the importance to identify melting point of recrystallized compound.

The importance to identify melting point of recrystallized compound is for
verification purposes because they are quickly measured and involve relatively an
inexpensive instrumentation and accurate procedures. Besides, melting points also
provide a simple method of obtaining an indication of purity of a compound.

2. Briefly explain the effect of phenyl carbonate in Sample C.

The effect of phenyl carbonate in Sample C is the mix of 50% recrystallized
vanillin and 50% phenyl carbonate have the lowest melting point than crude vanillin
and recrystallized vanillin.

DISCUSSION

The first goal of this experiment is to determine the melting point of recrystallized vanillin
and crude vanillin. The melting point of a substance means the temperature at which
the liquid and solid phases exist in equilibrium with one another without change
of temperature. However, if impurities present in a substance the melting points will be
compromised. The presence of impurities will decrease the melting point of a pure solid.

Vanillin is the primary component of the extract of the vanilla bean. Synthetic vanillin,
instead of natural vanilla extract, is sometimes used as a flavouring agent in foods, beverages,
and pharmaceuticals. It is used by the food industry as well as ethyl vanillin. Artificial vanilla
flavouring is a solution of pure vanillin, usually of synthetic origin.

In this experiment, we managed to obtain the melting point for the crude
vanillin of sample A which is 88℃. However, the melting point for recrystallized
vanillin of sample B from experiment 1 is 85℃ while the melting point for 50%
recrystallized vanillin mix with 50% phenyl carbonate of sample C is 79 ℃. The percentage
recovery for recrystallized vanillin is 90% pure vanillin while the other 10% is its’ loss. This
happened because the sample is impurity as there is some foreign matter present in the
sample. The purity of compound or the pure compound is a homogenous sample
consisting only of molecules having the same structure. So, it could be that the recrystallized
vanillin is impure due to the presence of contaminants like paper fibre from filter paper

While conducting these experiments, some errors occurred like in the first experiment we did
not plaster the Buchner funnel to the Erlenmeyer flask properly. This has caused the loss of
water pressure inside the flask. So, to overcome this problem, we redo the plastering by
plastering it tighter than before. Besides that, in the second experiment we did not stay near
Melting Temperature apparatus when the temperature of recrystallized vanillin exceed to
80℃ thus, we get quite a large range of temperature reading compared to the crude
vanillin temperature range. So, we redo it by using new capillary tube filled with
recrystallized vanillin and stay near the Melting Temperature apparatus until we
managed to get the temperature correctly.
CONCLUSION

In this experiment determination of melting point of vanillin and crude vanillin succeed
with the melting point of recrystallization of vanillin is lower than crude vanillin. it is because
the carbon chain between atoms in pure vanillin is slightly free to react with any substances
rather than crude vanillin which has higher boiling point because crude vanillin has to
undergo the process of initiation to freely react with other substances.

REFERENCES

1. http://murov.info/orglab/8-e3.pdf

2. Gilbert C. J, Martin F. S, Experimental Organic Chemistry A Miniscale

andMicroscale Approach, Third Edition, Thomson, 2002.