UNIVERSITY OF ENGINEERING AND TECHNOLOGY, LAHORE
DEPARTMENT OF CHEMICAL ENGINEERING
The experiment performed by following group members:
Saad Baig 2022-CH-27
Muhammad Rayan 2022-CH-35
Muhammad Kaif 2022-CH-37
Hafiz Muhammad Dilshad 2022-CH-1
K.M Arslan Khan Khilji 2022-CH-3
Submitted to
Dr. Farhan Javed
ChE-204L Chemical Engineering Thermodynamics-I
Title of experiment:
To study the thermal transitions of the high-density polyethylene
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Table of contents
1. Objective 3
2. Apparatus 3
3. Working principle 3
4. Theory 3
4.1 Differential scanning calorimeter 3
4.2 Glass Transition Temperature 4
4.3 Melting point Temperature 4
4.4 Crystallization Temperature 5
4.5 DSC Curve 5
4.5.1 Peak Temperature 5
4.5.2 Endothermic peak 5
4.5.3 Exothermic peak 6
4.6 Why we use N2 gas? 6
6
5. Procedure
7
6. Observations
8
7. Literature values
8
8. Sources of errors
8
9. Precautions
8
10. Conclusion
9
11. Applications
9
12. References
9
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1. Objective:
To detect the thermal transitions of high-density polyethylene.
To detect the following points:
Melting point
Crystallization point
2. Apparatus:
Differential scanning calorimeter (DSC)
Crimper
Weight balance
Aluminum Pan
High density polyethylene (6.5mg)
Nitrogen gas
Reference Sample
3. Working Principle:
The basic principle of DSC is that when the sample undergoes a phase
transition, more or less heat will need to flow through it then the reference to maintain the both at
same temperatures.
4. Theory:
Thermal transitions refer to change in the physical and chemical properties change with
variations of temperature. These transitions can involve different phases of matters i.e solid, gas
and liquid. Many polymers, metals and compounds exhibit the thermal transitions. Here are some
examples of thermal transitions:
Melting
Freezing
Vaporization
Deposition
Glass Transition
Sublimation
Condensation
4.1 Differential Scanning Calorimeter (DSC):
Differential scanning calorimeter (DSC) is a thermo analysis technique in which
difference in the amount of heat is required to raise the temperature of the sample and the
reference is measured as a function of temperature. Both the sample and reference are
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maintained at nearly the same temperature throughout the experiment. Generally, the
temperature program for a DSC analysis is designed such that the sample holder temperature
increases linearly as a function of time. The reference sample should have a well-defined heat
capacity over the range of temperatures to be scanned. Additionally, the reference sample must
be stable, of high purity, and must not experience much change across the temperature scan.
Typically, reference standards have been metals such as indium, tin, bismuth, and lead, but other
standards such as polyethylene and fatty acids have been proposed to study polymers and organic
compounds, respectively.
Fig 1: DSC Apparatus
The main purpose of DSC experiment is to detect the thermal transitions at following points:
Glass Transition Temperature (Tg)
Melting point Temperature (Tm)
Crystallization Temperature
4.2 Glass Transition Temperature:
The glass transition temperature (Tg) is a critical temperature in the study
of amorphous materials, particularly polymers and glasses. It represents the temperature at which
a material transitions from a hard and brittle state to a rubbery or viscous state. Unlike crystalline
materials that have a distinct melting point, amorphous materials undergo a more gradual
transition from a rigid to a more flexible state as they are heated.
At glass transition temperature, the molecular motion in the substance increases leading to
change in the physical state of the substance. The glass transition temperature is very important
in the polymers process industry, production of the glass and in pharmaceuticals industry.
4.3 Melting point Temperature:
The melting point of the substance is the temperature at which a
substance changes its state from solid to liquid. At melting point, the substance is in equilibrium
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with solid and liquid phase. The melting point is usually dependent upon pressure and the
temperature. Melting point is the crucial factor in the processing of drugs and other industries.
The melting point is also very important in phase transition studies.
4.4 Crystallization Temperature:
Crystallization temperature is a temperature at which a substance
undergoes crystallization. A substance changes its phase from liquid or gas to solid phase as
crystals are formed.
The crystallization temperature is a key parameter in understanding the phase
transitions of materials and is often utilized in various industries for manufacturing and research
purposes.
Fig 2: General PT Thermodynamic diagram
In thermodynamics phase diagram (PT Diagrams), we tell the state of a substance at given
temperature and pressure. We also tell the melting point and the freezing point of the substance.
4.5 DSC Curves:
The graphical representation of the results obtained from the DSC experiment are
called DSC curves. It is a graph between heat flow versus time or temperature versus time. Here
are some terminologies related DSC curve.
4.5.1 Peak Temperature:
The temperature at which a thermal event is intense. This term is usually related
when the substance is fully melted.
4.5.2 Endothermic peak:
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The peak at which substance absorbs heat. These peaks are also called positive
peaks. This peak is usually for the process melting point.
4.5.3 Exothermic peak:
The point at which substance releases heat. These peaks are negative peaks. This
terminology is usually used for the crystallization point.
Fig 3: General DSC curve diagram
4.6 Why we use N2 Gas?
The N2 gas is widely used during DSC experiment. In DSC experiment, an inert has been
built up so that the thermal transition of the given substance is not influenced by the
surroundings. Some substance undergoes oxidation at high temperatures. By purging N 2 gas, it
reduces the amount of oxygen in the chamber which decreases the likelihood of the oxidation.
We use another gas for inert atmosphere but nitrogen gas is easily available and cheaper.
So, it preferred most.
5. Procedure:
Firstly, take an aluminum pan with a lid.
Measure 6.5mg of high-density polyethylene (HDPE) on weight balance.
Place 6.5mg of HDPE in empty aluminum and sealed it by using crimper.
Now switch on the differential scanning calorimeter apparatus.
Open the furnace fitted in DSC apparatus. Place an empty pan in furnace as a reference
and sealed pan.
Give data to the computer about the substance which is under observation such as
substance name, reference compound name etc. Then set the onset and endset
temperature.
Allow the substance to go through the thermal transition.
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After 25-30 minutes, we get a DSC curve of HDPE. A software in the computer
automatically generates a DSC curve.
6. Observations and Calculations:
This is an automatic system which gives the data after the experiment and
give a DSC curve. The two graphs are attached below which are generated by the system:
DSC Thermal Analysis Result
mW
20.00 HDP E 22-Chem.tad DS C
10.00
0.00
-10.00 P eak 0
125.27x
C10
Ons et 119.55 0
x 10
C
E nds et 0
130.14x
C10
Heat -702.53 0
x 10
mJ
-20.00 -108.08 0
x /g
J 10
25.00 50.00 75.00 100.00 125.00 150.00
Temp [C]
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DSC Thermal Analysis Result
Temp
mW C
20.00 HDPE 22-Chem.tad Temp Peak 112.52 0C
x 10 150.00
HDPE 22-Chem.tad DSC
Ons et 114.86 0C
x 10
Ends et 0
104.33x
C10
Heat 0
924.05x
mJ10
10.00 0
142.16x
J /g
10
100.00
0.00
Peak 0
125.27x
C10
-10.00
Ons et 119.59 0C
x 10
Ends et 0
130.28x
C10 50.00
Heat -752.36 0mJ
x 10
-20.00 -115.75 0J
x /g
10
-0.00 8.33 16.67 25.00
Time [min]
Here are the reported data from graphs:
Melting point: 125.27 0C
Heat Flow = ∆HM = 115.75 J/g
Crystallization Temperature: 112.52 0C
Heat Flow = ∆HC = 142.16 J/g
7. Literature Values:
The literature values of High density poly ethylene are given below:
Melting point: 125-132 0C
Crystallization Temperature: 115-122 0C
Latent Heat of Fusion: 188.6 J/g
8. Sources of errors:
Following factors may affect the results of experiment:
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Heat loss to the surroundings due to inadequate insulation or inefficient temperature
control.
Delays in the response time of DSC instrument can lead to inaccuracies, especially when
rapid temperature change occurs.
The choice of sample pan material and geometry can impact the thermal transitions.
Different materials have different heat capacities.
Contamination can also lead to inaccuracies.
Inaccuracies in the calibration of DSC instrument can lead to inaccuracies.
Incorrect sample mass can cause errors in the result.
9. Precautions:
Properly seal sample pans to prevent the exchange of gases to the surroundings.
Avoid using excessive sample quantities, as it may leads to inaccuracy.
Ensure that the reference and sample pans are identical to eliminate discrepancies in heat
flow measurement.
Regularly calibrate the instrument to prevent from errors.
Use a high purity purge gas to minimize interference with sample analysis.
10. Conclusion:
Our results resembled with the literature value. Melting point falls in the
range of the literature value whereas crystallization point slightly deviate from the literature
values. There are many factors that may affect the result. As it is an automated experiment, so
the chances of errors are low. But sample impurities may affect the result. The pan was not
sealed properly may leads to errors.
11. Applications:
DSC is a versatile technique. The applications of the DSC are diverse and covers a
wide range of industrials and scientific fields. Here are some applications of the DSC experiment
are written below:
It is widely used in the determination of melting point and melting enthalpies.
It is used for identification and characterization of phase transitions in materials such as
glass transition etc.
It is used for the detection of impurities in sample.
It plays a crucial role in the study of protein denaturation and thermal transitions in
biomolecules.
It is used for characterization of rubbery and elastic materials.
It is helpful in the analysis of soil components.
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It is used in design and optimization of materials with specific thermal properties.
It plays crucial role in catalysis studies.
It is used for detection of changes in elastomers.
12. References:
1. Young, R. J., & Lovell, P. A. (2007), Introduction to Polymers, Wiley and sons Inc.
2. Bassett, D.C., Daniell, M.F, & Haward, R.N. (2004), Polymer Characterization: Physical
Techniques, ACS Publications
3. David I. Bower (2002), An introduction to polymer physics, Cambridge university press
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