UNIVERSITI TEKNOLOGI MARA CAWANGAN

PERAK
KAMPUS TAPAH
Faculty of Applied Sciences
Diploma in Science

CHM 258
FUNDAMENTAL OF ORGANIC
CHEMISTRY
LABORATORY REPORT

PRACTICAL : MELTING POINT DETERMINATION

CLASS : A4AS1203_24

GROUP MEMBERS :
1. MOHAMMAD AMINUDIN BIN MOHD RAZALI (2017287672)
2. MUHAMAD NUR AFIQ BIN SHARI (2017296452)
3. MUHAMMAD HARIZ BIN HAMAZAH (2017679774)

LECTURER : SITI NORHAYATI BINTI MOHAMAD TARMIZI

DATE OF SUBMISSION : 30 OCTOBER 2018

OBJECTIVES
To determine the melting point of recrystallized vanillin and crude vanillin

INTRODUCTION
In previous experiment, the attempted were made to purify a sample of vanillin. Today you
will determine the melting point measurement, the success of the purification. Anytime a
compound is obtained from a natural or synthetic source, its identify must be determined and
or verified. Physical properties also provide a simple method of obtaining a rough indication
of purify. At 5 ℃ differences between an experimental and an expected melting point for
example, indicates that the sample is approximately 95% pure. Each 1%(up to about 10%),
very roughly , depressed the melting point 1 ℃ impurities not only depress melting point but
broaden them. Thus, if compound A is supposed to melt at 65 ℃ but experimentally it is
found that heating causes it to begin softening at 57 ℃ and total liquefy at 65 ℃, we report
that sample has melting range of 57 – 62 ℃ and is considerably impure. The fact that
contamination tend to depress melting points enables one to distinguish between two
compounds with the same melting point.

APPARATUS
1. Capillary tube
2. Pestle and mortar
3. Melting point apparatus

CHEMICALS
1. Crude vanillin
2. Recrystallized vanillin (from Experiment 1)
3. Phenyl carbonate
PROCEDURE
The melting point of sample A,B and C is determined. For the sample C, each compound is
adding approximately equal amounts to mortar grind them together with the pestle before
inserting them into capillary tube.
A : Crude vanillin
B : Recrystallized vanillin from experiment 1
C : 50% recrystallized vanillin mix with 50% phenyl carbonate
1. The capillary tube is filled by pressing the open end onto the powdered sample until
there is a 1 cm length of sample in the tube.
2. Then capillary tube is drop, sealed end down, through a 1 m piece of 6 mm glass
tubing that is being held on a hard surface.
3. The dropping is procedure repeated until the sample is packed in the bottom of the
tube
4. The capillary tube is placed in the sample holder of the melting point apparatus.
5. The ON button is pressed, and the plateau light is observed. When the plateau is on,
the set button is pressed until the heat light is ON
6. The melting point of sample is started to record when the light is ON
7. The sample is observed through magnifying eyepiece part.

RESULT

MELTING POINT (℃)

SAMPLE
START COMPLETE

A 80 ℃ 86 ℃

B 80 ℃ 87 ℃

C 58 ℃ 80 ℃
QUESTION
1. Discuss the importance to identify melting point of recrystallized compound.
 The melting point indicates the level of purity of a sample. It also helps to
identify unknown samples, narrowing the number
of possibilities, because a pure solid melt over a narrow range
of temperatures. The melting point also helps to characterize new compounds.
In this experiment, the identity of an unknown organic compound will be
determined by
comparing its experimental melting point to those of a variety of known
compounds.

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

 When you mix two chemicals you get a melting point depression. Even if say,
one melts at 100C and the other at 120C, the mixture may melt at 85C. It
seems at first to defy logic as you might expect 110C or so. But what is
happening is each is interfering with the crystalline matrix of the other,
causing them to be loose and unstable. This effect makes molecules more
likely to release from the crystal structure, therefore lowering the melting
point of the mixture.

DISCUSSION
In this experiment, the melting point of 3 different types of material were determined. The
three material is crude vanillin, recrystallized vanillin (from experiment 1) and lastly is 50%
recrystallized vanillin mix with 50% phenyl carbonate.

Firstly, in this experiment we need to label the material with A, B and C. A is crude vanillin,
B is recrystallized vanillin while C is 50% recrystallized vanillin mix with 50% phenyl
carbonate. The melting point of these three materials will be measured using melting point
apparatus. After labeled the material using a capillary tube, the next step is to put the
capillary tube inside melting point apparatus. The capillary tube C and B will be tested first
and after one of it has been melting then it need to pull out while inserting the A tube.

After all of that has been melting, the result shown at melting point apparatus need to be
record. The result of this experiment shown which one of the materials has higher melting
point. The starting melting point of material in tube A is 81° and it completed melted at 86°.
Meanwhile, the starting melting point of material in tube B is 80° and it completed melted at
87°. Then, material in tube C start to melt at 58° and its completed melting point is 80°. This
result shown that material A that is crude vanillin has higher melting point compared to the
other two that is recrystallized vanillin and 50% recrystallized vanillin mix with 50% phenyl
carbonate.
CONCLUSION
From this experiment, we can determine the melting point of recrystallized vanillin and crude
vanillin.

REFERENCES
1. https://www.google.com/url?
sa=t&source=web&rct=j&url=http://www.westminster.edu/about/community/sim/doc
uments/sdeterminationofmeltingpoints.pdf&ved=2ahUKEwjCwbPCgaveAhVMpo8K
HeGeBVgQFjADegQIABAB&usg=AOvVaw3V_GhEaoUSUYY6uuFTyCrK
2. https://kirsoplabs.co.uk/lab-aids/impure-solids-melt-lower-temperatures/
3. https://answers.yahoo.com/question/index?qid=20071017083116AAqrhC1