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THARMOGRAVITOMETRIC ANALYSIS
HAFIZ ADNAN HANIF
E11-341
METALLURGY AND
MATERIAL ENGINEERING
1
Introduction
 TGA is a technique which measures the change in
the mass of a sample over a range of
temperatures.
 Principle:
• The basic principle of TGA is that as a sample is
heated, its mass changes. This change can be
used to determine the composition of a material or
its thermal stability, up to 1000oC. Usually, a
sample loses weight as it is heated up due to
decomposition, reduction, or evaporation
What TGA Can Tell You
•Thermal Stability of Materials
•Oxidative Stability of Materials
•Composition of Multi-component Systems
•Estimated Lifetime of a Product
•Decomposition Kinetics of Materials
•The Effect of Reactive or Corrosive Atmospheres
on Materials
•Moisture and Volatiles Content of Materials
Type Of Thermogrvimetry
1. Isothermal / Static Thermogravimetry
2. Quasistatic Thermogravimetry
3. Dynamic Thermogravimetry
1. Isothermal/ Static Thermogravimetry:
In this technique the sample weight is
recorded as a function of time at
constant temperature.
4
2.Qasistatic Thermogravimetry:
In this technique the sample is heated to
constant
weight at each of the series of increasing
temperature.
3. Dynamic Thermogravimetry:
In this technique a sample is heated in
an environment whose temperature is
changing in predetermine manner
generally at linear rate.
5
Thermogravimetric Curve:
 A to B - Thermal
stability of material.
 B to C -Weight loss.
 C – Procedural
decomposition
temperature.
 D- Final temperature
6
A
B
C
D
Factor Affecting TGA Curve:
A. Instrumental factor:-
1. Heating Rate
2. Furnace atmosphere
3. Sample Holder
B. Sample
Characteristic:-
1. Effect of sample
mass
2. Effect of sample
particle size
3. Effect of heat
reaction
4. Compactness of
sample
5. Previous history of
sample
7
Instrumentation
8
Components of
Instrumentation:
A. Recording balance
B. Sample Holder
C. Furnace
D. Furnace temperature
programmer/Controller
E. Recorder
F. Thermobalance
9
A. Balance:-
Recording balance
1. Deflection balance
i. Beam type
ii. Spring/ Helical type
iii. Cantilever type
iv. Torsion type
2. Null balance
10
1. Deflection balance:-
i. Beam type:-
A conversion of
beam deflection
about the fulcrum
into a suitably
identifiably weight
change.
11
ii.Spring/Helical type:-
An elongation or
contraction of
spring with weight
change. This
changes the length
of the spring .
12
iii. Cantilever type:-
 One end of the
beam is fixed &
other end on which
the sample is
placed, is free to
undergo deflection.
13
iv. Torsion type:-
 In this type of
balance the beam
is attach to torsion
wire.
 The wire is fixed at
one or both ends
so that deflection of
beam are
proportional to
weight change.
14
2. Null point balance:-
 In this balance
there should be a
sensor to detect
the deviation of the
balance to detect
the null position .
15
B. Sample Holder:-
Types of sample holder:-
1.Shallow Pans
2.Deep crucibles
3.Loosely covered crucibles
4.Restort cups
16
1.Shallow Pan:
Used for such sample necessary to
eliminate diffusion as a volatile material.
2. Deep Crucible:
Used to study industrial scale calcination
& surface area measurement.
3.Loosely curved crucible:
Used in self generated atom study.
4. Retord cups:
Useful in boiling point study.
17
C.Furnace:-
 Position of furnace with respect to
balance:
18
A B C
The choice of furnace heating element and type of
furnace depend upon the range being studies:-
Temperature Material
 1100˚c
 1100-1500˚c
 1100- 1750 ˚c
 Nichrome
 Platinum /Alloy of
rhodium
 Tungsten
19
D.Temperature
Measurement:-
 The most common method is
thermocouple.
 The temperature 1100,chromel/alumel
thermocouple are made up of alloys of
Pt and rhodium are used.
 Higher temperature tungsten or
rhenium thermocouple are used.
20
E. Recorder:-
Two Types:-
A. Time-base potentiometric strip chart
recorder
B. X-Y recorder
Advantage:-
1. To check the heating rate of the
furnace for linearity.
2. X,Y recorder we get curve having plot
of weight directly against temperature.
21
F. Thermobalance:-
 It records continuously weight change of
the sample as a function of temperature.
 The sensitivity of balance depends on
the size of the sample used.
 The temperature recorded to an
accuracy of better than ±1%
 The weight loss recovered to an
accuracy ±1%
 In market large number of balance are
available.
22
Applications:-
 Purity and thermal stability.
 Solid state reaction.
 Decomposition of organic and inorganic
compound.
 Determining composition of material.
 Corrosion of metals in various
atmosphere.
 Pyrolysis of coal , petroleum and wood.
 Roasting and calcination of minerals.
 Evaluation of gravimetric precipitates.
 Oxidative and Reductive stability.
23
Thermogravimetric analyses and mineralogical study of polymer
modified mortar with silica fume
RESEARCH ARTICLE
Alessandra Etuko Feuzicana de Souza Almeida*; Eduvaldo Paulo Sichieri
RESERCH ARTICLE
TGA curves of pastes with silica fume content of 5% and 10% respectively.
It can be seen that TGA curves for these pastes consist of four zones:
 ~ 25-123.3 °C: dehydration of pore water
 ~ 123.3-420 °C: dehydration of calcium silicate hydrates
 ~ 420-480 °C: dehydroxylation of calcium hydroxide
 ~ 480-730 °C: decarbonation of CaCO3
26

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Thermogravematric analysis

  • 1. THARMOGRAVITOMETRIC ANALYSIS HAFIZ ADNAN HANIF E11-341 METALLURGY AND MATERIAL ENGINEERING 1
  • 2. Introduction  TGA is a technique which measures the change in the mass of a sample over a range of temperatures.  Principle: • The basic principle of TGA is that as a sample is heated, its mass changes. This change can be used to determine the composition of a material or its thermal stability, up to 1000oC. Usually, a sample loses weight as it is heated up due to decomposition, reduction, or evaporation
  • 3. What TGA Can Tell You •Thermal Stability of Materials •Oxidative Stability of Materials •Composition of Multi-component Systems •Estimated Lifetime of a Product •Decomposition Kinetics of Materials •The Effect of Reactive or Corrosive Atmospheres on Materials •Moisture and Volatiles Content of Materials
  • 4. Type Of Thermogrvimetry 1. Isothermal / Static Thermogravimetry 2. Quasistatic Thermogravimetry 3. Dynamic Thermogravimetry 1. Isothermal/ Static Thermogravimetry: In this technique the sample weight is recorded as a function of time at constant temperature. 4
  • 5. 2.Qasistatic Thermogravimetry: In this technique the sample is heated to constant weight at each of the series of increasing temperature. 3. Dynamic Thermogravimetry: In this technique a sample is heated in an environment whose temperature is changing in predetermine manner generally at linear rate. 5
  • 6. Thermogravimetric Curve:  A to B - Thermal stability of material.  B to C -Weight loss.  C – Procedural decomposition temperature.  D- Final temperature 6 A B C D
  • 7. Factor Affecting TGA Curve: A. Instrumental factor:- 1. Heating Rate 2. Furnace atmosphere 3. Sample Holder B. Sample Characteristic:- 1. Effect of sample mass 2. Effect of sample particle size 3. Effect of heat reaction 4. Compactness of sample 5. Previous history of sample 7
  • 9. Components of Instrumentation: A. Recording balance B. Sample Holder C. Furnace D. Furnace temperature programmer/Controller E. Recorder F. Thermobalance 9
  • 10. A. Balance:- Recording balance 1. Deflection balance i. Beam type ii. Spring/ Helical type iii. Cantilever type iv. Torsion type 2. Null balance 10
  • 11. 1. Deflection balance:- i. Beam type:- A conversion of beam deflection about the fulcrum into a suitably identifiably weight change. 11
  • 12. ii.Spring/Helical type:- An elongation or contraction of spring with weight change. This changes the length of the spring . 12
  • 13. iii. Cantilever type:-  One end of the beam is fixed & other end on which the sample is placed, is free to undergo deflection. 13
  • 14. iv. Torsion type:-  In this type of balance the beam is attach to torsion wire.  The wire is fixed at one or both ends so that deflection of beam are proportional to weight change. 14
  • 15. 2. Null point balance:-  In this balance there should be a sensor to detect the deviation of the balance to detect the null position . 15
  • 16. B. Sample Holder:- Types of sample holder:- 1.Shallow Pans 2.Deep crucibles 3.Loosely covered crucibles 4.Restort cups 16
  • 17. 1.Shallow Pan: Used for such sample necessary to eliminate diffusion as a volatile material. 2. Deep Crucible: Used to study industrial scale calcination & surface area measurement. 3.Loosely curved crucible: Used in self generated atom study. 4. Retord cups: Useful in boiling point study. 17
  • 18. C.Furnace:-  Position of furnace with respect to balance: 18 A B C
  • 19. The choice of furnace heating element and type of furnace depend upon the range being studies:- Temperature Material  1100˚c  1100-1500˚c  1100- 1750 ˚c  Nichrome  Platinum /Alloy of rhodium  Tungsten 19
  • 20. D.Temperature Measurement:-  The most common method is thermocouple.  The temperature 1100,chromel/alumel thermocouple are made up of alloys of Pt and rhodium are used.  Higher temperature tungsten or rhenium thermocouple are used. 20
  • 21. E. Recorder:- Two Types:- A. Time-base potentiometric strip chart recorder B. X-Y recorder Advantage:- 1. To check the heating rate of the furnace for linearity. 2. X,Y recorder we get curve having plot of weight directly against temperature. 21
  • 22. F. Thermobalance:-  It records continuously weight change of the sample as a function of temperature.  The sensitivity of balance depends on the size of the sample used.  The temperature recorded to an accuracy of better than ±1%  The weight loss recovered to an accuracy ±1%  In market large number of balance are available. 22
  • 23. Applications:-  Purity and thermal stability.  Solid state reaction.  Decomposition of organic and inorganic compound.  Determining composition of material.  Corrosion of metals in various atmosphere.  Pyrolysis of coal , petroleum and wood.  Roasting and calcination of minerals.  Evaluation of gravimetric precipitates.  Oxidative and Reductive stability. 23
  • 24. Thermogravimetric analyses and mineralogical study of polymer modified mortar with silica fume RESEARCH ARTICLE Alessandra Etuko Feuzicana de Souza Almeida*; Eduvaldo Paulo Sichieri
  • 25. RESERCH ARTICLE TGA curves of pastes with silica fume content of 5% and 10% respectively. It can be seen that TGA curves for these pastes consist of four zones:  ~ 25-123.3 °C: dehydration of pore water  ~ 123.3-420 °C: dehydration of calcium silicate hydrates  ~ 420-480 °C: dehydroxylation of calcium hydroxide  ~ 480-730 °C: decarbonation of CaCO3
  • 26. 26