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THERMOGRAVIMETRIC
ANALYSIS
Anita Kumbhakar
18901919005
Advanced Instrumentation Techniques
PT 810C
4TH Year B. Pharm
01
04
02
05
Table of contents
Introduction Factors affecting
TG Curve
Principle Advatages
03
06
Types Applications
Instrumentation
07
08
What we get
from TGA
 Thermogravimetric Analysis is a technique in which
the mass of a substance is monitored as a function
of temperature or time as the sample specimen is
subjected to a controlled temperature program in a
controlled atmosphere.
 TGA is a technique in which, upon heating a
material, its weight increases or decreases.
 TGA measures a sample’s weight as it is heated or
cooled in a furnace.
Introduction
• A TGA consists of a sample pan that is supported by a
precision balance. That pan resides in a furnace and is
heated or cooled during the experiment. The mass of the
sample is monitored during the experiment. A sample purge
gas controls the sample environment. This gas may be inert
or a reactive gas that flows over the sample and exits
through an exhaust.
• These instruments can quantify loss of water, loss of solvent,
loss of plasticizer, decarboxylation, pyrolysis, oxidation,
decomposition, weight % filler, amount of metallic catalytic
residue remaining on carbon nanotubes, and weight % ash.
Contd.
PRINCIPLE
• A TGA analysis is performed by gradually raising the temperature of
a sample in a furnace as its weight is measured on an analytical
balance that remains outside of the furnace.
• In TGA, mass loss is observed if a thermal event involves loss of a
volatile component.
• Chemical reactions, such as combustion, involve mass losses,
whereas physical changes, such as melting, do not.
• The weight of the sample is plotted against temperature or time to
illustrate thermal transitions in the material – such as loss of solvent
and plasticizers in polymers, water of hydration in inorganic
materials, and, finally, decomposition of the material.
TYPES
The three types of thermographic analysis represent different ways to
apply heat to the sample, as weight change is measured over time.
• Isothermal or static thermogravimetry: Temperature is
constant
• Dynamic thermogravimetry: Temperature is changed in a linear
manner
• Quasi Static thermogravimetry: A series of increasing
temperatures
INSTRUMENTATION
The major components of the thermogravimetric
analyzer (thermobalance) are:
• Balance
• Furnace assembly
• Sample container, temperature sensor, furnace liner,
thermocouple, etc.
• Recorder and display
• A purge gas system for providing an inert
atmosphere.
The balance and the furnace assembly are the two key
components of thermobalance. A shallow platinum
crucible (also known as a sample container) is used to
hold the samples and is connected to an automatic
recording microbalance. In thermogravimetry, null point
balances are the most often used form of the balance
system. The null point approach causes the balance
beam to move away from its normal position whenever
there is a change in weight.
FACTORS AFFECTING TG CURVE
INSTRUMENTAL FACTORS
SAMPLE CHARACTERISTICS
FURNACE HEATING RATE:
The temperature at which the
compound decompose depends
upon the heating rate. When the
heating rate is high, the
decomposition temperature is
also high
FURNACE ATMOSPHERE:
The atmosphere inside the
furnace surrounding the sample
has a profound effect on the
decomposition temperature of
the sample
WEIGHT OF SAMPLE:
A small weight of the sample
is recommended using a small
weight eliminates the existence
of temperature gradient
throughout the sample.
SAMPLE PARTICLE SIZE:
The particle size of the sample
should be small & uniform. The use
of large particle or crystal may
result in apparent very rapid weight
loss during heating.
ADVANTAGES OF TGA
A relatively small set of data is to be treated
Continuous recording of weight loss as a function
of temperature ensures equal weightage to
examination over the whole range of study
As a single is analyzed over the whole range of
temperature, the variation in the value of the kinetic
parameters, if any, will be indicated
1
2
3
APPLICATIONS
Filler content of polymer resins
Residual solvent content
Carbon black content
Decomposition temperature
Moisture content of organic and inorganic materials
Plasticizer content of polymers
Oxidative stability
Performance of stabilizers
Low molecular weight monomers in polymers
It is beneficial in routine
analysis of content
determination to get
accurate understanding of
sample composition.
It helps in understanding
the reactivity corrosivity of
sample materials when
exposed to specific
environments.
TGA analyzes the changes
in size, shape and overall
mass when exposed to
varying temperatures.
It gives accurate details of
the mass change of the
materials under test.
It provides necessary data
for a wide range of
materials characterization
objectives.
Determines the stability of
pharmaceutical drugs.
What do we get from TGA?
Thanks!

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THERMOGRAVIMETRIC ANALYSIS

  • 2. 01 04 02 05 Table of contents Introduction Factors affecting TG Curve Principle Advatages 03 06 Types Applications Instrumentation 07 08 What we get from TGA
  • 3.  Thermogravimetric Analysis is a technique in which the mass of a substance is monitored as a function of temperature or time as the sample specimen is subjected to a controlled temperature program in a controlled atmosphere.  TGA is a technique in which, upon heating a material, its weight increases or decreases.  TGA measures a sample’s weight as it is heated or cooled in a furnace. Introduction
  • 4. • A TGA consists of a sample pan that is supported by a precision balance. That pan resides in a furnace and is heated or cooled during the experiment. The mass of the sample is monitored during the experiment. A sample purge gas controls the sample environment. This gas may be inert or a reactive gas that flows over the sample and exits through an exhaust. • These instruments can quantify loss of water, loss of solvent, loss of plasticizer, decarboxylation, pyrolysis, oxidation, decomposition, weight % filler, amount of metallic catalytic residue remaining on carbon nanotubes, and weight % ash. Contd.
  • 5. PRINCIPLE • A TGA analysis is performed by gradually raising the temperature of a sample in a furnace as its weight is measured on an analytical balance that remains outside of the furnace. • In TGA, mass loss is observed if a thermal event involves loss of a volatile component. • Chemical reactions, such as combustion, involve mass losses, whereas physical changes, such as melting, do not. • The weight of the sample is plotted against temperature or time to illustrate thermal transitions in the material – such as loss of solvent and plasticizers in polymers, water of hydration in inorganic materials, and, finally, decomposition of the material.
  • 6. TYPES The three types of thermographic analysis represent different ways to apply heat to the sample, as weight change is measured over time. • Isothermal or static thermogravimetry: Temperature is constant • Dynamic thermogravimetry: Temperature is changed in a linear manner • Quasi Static thermogravimetry: A series of increasing temperatures
  • 7. INSTRUMENTATION The major components of the thermogravimetric analyzer (thermobalance) are: • Balance • Furnace assembly • Sample container, temperature sensor, furnace liner, thermocouple, etc. • Recorder and display • A purge gas system for providing an inert atmosphere. The balance and the furnace assembly are the two key components of thermobalance. A shallow platinum crucible (also known as a sample container) is used to hold the samples and is connected to an automatic recording microbalance. In thermogravimetry, null point balances are the most often used form of the balance system. The null point approach causes the balance beam to move away from its normal position whenever there is a change in weight.
  • 8. FACTORS AFFECTING TG CURVE INSTRUMENTAL FACTORS SAMPLE CHARACTERISTICS FURNACE HEATING RATE: The temperature at which the compound decompose depends upon the heating rate. When the heating rate is high, the decomposition temperature is also high FURNACE ATMOSPHERE: The atmosphere inside the furnace surrounding the sample has a profound effect on the decomposition temperature of the sample WEIGHT OF SAMPLE: A small weight of the sample is recommended using a small weight eliminates the existence of temperature gradient throughout the sample. SAMPLE PARTICLE SIZE: The particle size of the sample should be small & uniform. The use of large particle or crystal may result in apparent very rapid weight loss during heating.
  • 9. ADVANTAGES OF TGA A relatively small set of data is to be treated Continuous recording of weight loss as a function of temperature ensures equal weightage to examination over the whole range of study As a single is analyzed over the whole range of temperature, the variation in the value of the kinetic parameters, if any, will be indicated 1 2 3
  • 10. APPLICATIONS Filler content of polymer resins Residual solvent content Carbon black content Decomposition temperature Moisture content of organic and inorganic materials Plasticizer content of polymers Oxidative stability Performance of stabilizers Low molecular weight monomers in polymers
  • 11. It is beneficial in routine analysis of content determination to get accurate understanding of sample composition. It helps in understanding the reactivity corrosivity of sample materials when exposed to specific environments. TGA analyzes the changes in size, shape and overall mass when exposed to varying temperatures. It gives accurate details of the mass change of the materials under test. It provides necessary data for a wide range of materials characterization objectives. Determines the stability of pharmaceutical drugs. What do we get from TGA?