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Thermal Analysis

Dr. Saima Shabbir, MS&E


Basic Principle
Sample is heated at a constant heating rate
Samples Property Measured
Weight TGA (Thermalgravimetric Analysis)
Size TMA (Thermal Mechanical Analysis)
Heat Flow DSC (Differential Scanning Calorimetric)
Temperature DTA (Differential Thermal Analysis)
Gas evolved TPD (Temperature Programmed Desorption)

Dr. Saima Shabbir, MS&E


Thermogravimetric Analysis

TGA

Dr. Saima Shabbir, MS&E


Introduction
TGA is the most widely used thermal method.
It is based on the measurement of mass loss
of material as a function of temperature
A plot of mass change versus temperature (T)
is referred to as the thermogravimetric curve
(TG curve).

Dr. Saima Shabbir, MS&E


Introduction
A technique in which the mass of a
substance is measured as a function of
temperature, while the substance is
subjected to a controlled temperature
programme.
Controlled temperature programme can
mean:
Heating and/or cooling at a linear rate
Dr. Saima Shabbir, MS&E
TGA Output
The measurements are used primarily to
determine:
The thermal stabilities
The oxidative stabilities
The extent of purity
The compositional properties.

Dr. Saima Shabbir, MS&E


TGA Applications
The technique can analyze materials that
exhibit either mass loss or gain due to
decomposition, oxidation or loss of volatiles
(such as moisture).
It is especially useful for the study of
polymeric materials, including thermoplastics,
thermosets, elastomers, composites, films,
fibers, coatings and paints.

Dr. Saima Shabbir, MS&E


TGA Applications
TGA measurements provide valuable
information that can be used:
To select materials for certain end-use
applications,
To predict product performance
To improve product quality.

Dr. Saima Shabbir, MS&E


TGA Applications
The technique is particularly useful for the following
types of measurements:
Compositional analysis of multi-component materials
or blends
Thermal stabilities
Oxidative stabilities
Estimation of product lifetimes
Decomposition kinetics
Effects of reactive atmospheres on materials
Filler content of materials
Moisture and volatiles content

Dr. Saima Shabbir, MS&E


Thermogravimetric Analyzer

Dr. Saima Shabbir, MS&E


Instrumentation
The instrument used in thermogravimetry
(TG) is called a thermobalance.

Dr. Saima Shabbir, MS&E


TG Curve Interpretation
In thermogravimetry, the term
decomposition temperature is a
complete misnomer.
In a TG curve of a single stage
decomposition, there are two
characteristic temperatures;
The initial Ti and the final temperature
Tf.
Ti is defined as the lowest temperature
at which the onset of a mass change
can be detected and Tf as the final
temperature at which the particular
decomposition appear to be complete.

Dr. Saima Shabbir, MS&E


TG Curve

The 1st derivative peak temperature indicates the point of


greatest rate of change on the weight loss curve. This is also
known as the inflection point.
Dr. Saima Shabbir, MS&E
Different Heating Rates

10 mg samples of PTFE, heated at 2.5, 5, 10


and 20 C/min in nitrogen
Dr. Saima Shabbir, MS&E
Different Heating Rates
When the heating rate is low enough, equilibrium
could be readily obtained at any point of
increasing temperature
Whereas with increasing heating rate, the heating
rate is too fast for the equilibrium to reach
because of heat diffusion, making Td, increase
steadily.
As a result, higher decomposition temperatures
would be observed if faster heating rates were
applied.
Dr. Saima Shabbir, MS&E
Characterization of Polymers
Using TGA

Dr. Saima Shabbir, MS&E


TGA results
obtained for Nylon
6,6 bristles
showing thermal
degradation
under a nitrogen
purge.
Approximately 10
mg of sample was
heated at a rate of The TGA results show that the nylon-6,6
20 oC/min. polymer undergoes thermal degradation
o
beginning at 482 C and with a total mass
loss of 99.0%. There is a small amount of
inert residue remaining (0.15%).
Dr. Saima Shabbir, MS&E
Moisture Content in Polymers
Nylon polymers absorb a small amount of ambient moisture
and TGA can be used to determine this level of water.
At about 56 oC, the nylon polymer starts to evolve the small
amount of moisture, which is found to be 0.86% by TGA.
A high performance TGA instrument is required to detect this
small level of moisture content.
Knowing this moisture content
is important as it has a major
bearing on the end use
properties and processing
performance of nylon.
Dr. Saima Shabbir, MS&E