Name: Aqib Ali

Class: 3rd Professional

Roll no: 07
Semester: 2nd semester 2020
Assignment Topic: Instrumentation of TGA
Submitted to: Dr Jawad Ahmed Khan
Name : Dharam Pal (13)
Aqib Ali (07)
Sham Sagar (34)
Class: 3rd Professional Pharmacy
Subject: Analytical Chemistry
Assignment: Thermogravimetric Analysis
Teacher: Dr Jawad Ahmed Khan
 THERMAL ANALYSIS
• Thermal analysis is a branch of materials science & a group of
analysis which study the property of material when the change
with temperature .
• In this technique mass of the substance is measure as the form of
temperature while it a subjected to control temperature.

Types of thermal analysis

 Thermogravimetric Analysis (TGA or TG)
 Differential Scanning Calorimetry (DSC)
 Derivative Thermogravimetry(DTG)
 Differential thermal analysis (DTA)
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 INTRODUCTION (TGA)
 Thermogravimetry(TG) is the branch of thermal analysis which
examines the mass change of a sample as a function of temperature
(in the scanning mode) or as a function of time (in the isothermal
mode).
 Thermogravimetric analysis is a method of thermal analysis in which
changes in physical and chemical properties of materials are
measured as a function of increasing temperature rate or as a
function of time.

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 Types of Thermogravimetry
There are three types of Thermogravimetry :
1. Isothermal /static Thermogravimetry
2. Quasistatic Thermogravimetry
3. Dynamic Thermogravimetry
4.Isothermal /static Thermogravimetry: in this technique the sample
weight is recorded as a function of time at constsnt temperature.
5.Quasistatic Thermogravimetry: in this technique the sample is
heated to constant weight at each of the series of increasing
temperature.
6.Dynamic Thermogravimetry: in this technique a sample is heated in
an environment whose temperature is changing in temperature
manner generally at linear rate .

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Thermo gravimetric analysis(TGA)

Principle:
 In Thermogravimetric analysis, mass of the substance is
measure as the function of temperature while it is subjected to
control temperature program the resulted is TG curve or
Thermogravimetric curve time or temperature is plotted on x-
axis or mass is plotted on y-axis.
 Temperature - 0°c -2000°c
 Change in mass of our analyte is studied because of
different physical or chemical transition.

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 Cont…
 It is used in analysis of volatile products, gaseous
lost during the reaction in Thermoplastics, Thermosets,
products
elastomers, films, fibers, paints etc.
 The change in the weight of the substance is recorded as a
function of temperature or time. The temperature is increased
at a constant rate for a known initial weight of the substance
and the changes in weights are recorded as a function of
temperature at different time interval.

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 Example: TGA Curve for AgNO3

The horizontal portion of the curve

indicates that, there is no change in
weight (AB &CD) and the portion BC
indicates that there is weight change.
The weight of the substance (AgNO3)
remains constant upto a temperature of
473°C indicating that AgNO3 is thermally
stable upto a temperature of 473°C.
At this temperature it starts losing its
The diagram indicates the
weight and this indicates that the TGA curve for AgNO3.
decomposition starts at this temperature.
It decomposes to NO2, O2 and Ag. AgNO3 → Ag + NO2 + O2
 TGA Curve for AgNO3

The loss in weight continues upto 608°C and beyond this

temperature the weight of the sample remains constant,
this is shown by the portion of the curve CD.
The portion between BC, represents the decomposition
of silver nitrate, the decomposition is complete at 608°C
leaving metallic silver as the stable residue
Instrumentation of ThermogravimetricAnalysis
Block diagram of a Thermobalance

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 Instrumentation
Components of instrumentation or Thermobalance
1) Microbalance
2) Recorder balance
3) Sample holder
4) Furnace
5) Furnace Temperature programmer/controller
6) Recorder
7) Data recording unit
8) Heating rate
9) Time measurement
 1.Microbalance
• It is the most important component of thermobalance. It is used
to record a change in mass of sample or substance.
• An ideal microbalance must possess following features:
a) It should provide electronic signals to record the change in mass
b) It should have the capacity of auto weight
c) Modern microbalances have the ability to be not affected by
vibrations

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 2. Recorder balance
Types of recorder balance
1. Deflection balances
2. Null point balances

3. Deflection balances: They are of following types:

a) Beam Type
b) Helical Type
c) Cantilevered Beam
d) Torsion Wire

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(a) Deflection balances Deflection
balances are 4 types :-
• Beam Type
• In these balance,the conversion
of deflected beam take place
into
weight change
• Helical Type
• In these balance, elongation or contraction of spring occurs with
change in weight which is recorded by help of transducer.
• Torsion Wire
• In this the beam is attached to hard torsion wire which act
as
fulcrum
• Cantilevered Beam
• In this balance, one end of beam is fixed and on the other 21
TORSION BALANCE BEAM BALANCE

HELICAL BALANCE
 (b) Null point balances
• It consist of sensor which detects the deviation from
the null point and restores the balance to its null point
by means of restoring force.

3. Sample holder
• The sample to be studied is placed in sample holder or
crucible.
• It is attached to the weighing arm of microbalance.
 4. Furnace
• The furnace should be designed in such a way that it produce a
linear heating rate.
• It should have a hot zone which can hold sample and crucible and
its temperature corresponds to the temperature of furnace.
• The temperature ranges can affect the internal atmosphere of
furnace chamber therefore, it is necessary to choose specific type
of furnace according to the temperature ranges.
• The size of furnace is important .

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 5.Recorder
• The output from the microbalance and furnace are recorded using
either chart recorder.
• The recording systems are mainly of 2 types:-
1. Time- base potentiometric strip chart recorder
2. X-Y recorder
• in the X-Y recorder, weight loss is recorded a the function of
temperature.
• However, the percentage mass change against temperature
or time would be more useful.

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 6.Heating rate
• It is the rate of temperature increases, which is customarily
quated in degrees per minute. The heating or cooling rate is used
to be constant when the temperature/time curve is linear.

7.Time measurement
• It is done by thermocouple. Different materials are used for
measuring different ranges of temperatures i.e. chromal or
alumel thermocouple are used for T=1100°c

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 1.Instrumental factors
• Furnace Heating rate:
The temperature at which the compound (or sample) decompose
depends upon the heating rate is high, the decomposition
temperature is also high. A heating rate of 3.5°c per minute is
usually recommended for reliable and reproducible TGA.

• Furnace atmosphere:
The atmosphere inside the furnace surrounding the sample has a
profound effect on the decomposition temperature of the sample.
A pure nitrogen gas from a cylinder passed through the furnace
which provides an inert atmosphere.

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 Factors affecting the TG curve
The factors which may affect the TG curves are classified into two main
groups-

(1)Instrumental factors
(a) Furnace heating rate
(b) Furnace atmosphere
(c) Sample holder
(2)Sample characteristics includes
(a) Weight of the sample
(b) Sample particle size
(c) Heat of reaction (d)Compctness
of the sample (e)Previous history
of the sample

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 2.Sample characteristics
a)Weight of sample: A small weight of sample is recommended using
a small weight eliminates the existence of temperature gradient
throughout the sample

b)Particle size of sample: The particle size of sample should be small

and uniform. The use of large particle may result in apparent very
rapid weight loss.

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 Applications
1. Physical transition
2. Chemical transition
3. Loss of drying
4. Purity of analyte
5. Stability of analyte
6. Determination of bound and unbound water begins at room
temperature due to dry gas flowing over sample
7. TGA, we can determine the purity and thermal stability of
both primary and secondary standard.
8. corrosion studies
9. Automatic Thermogravimetric analysis
10. Evaluation of suitable standards

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 ADVANTAGES OF TGA
• Any type of solid can be analyzed With minimal sample
preparation (at least 0.1mg) eg : powders, pellets, flakes
• TGA has high accuracy of balance used as well as precise
control of heating/cooling rate and atmospheric condition
• TGA may be convenient and time saving, performance of
technique does suffer due to construction requirements
• Easy sample changing and easy change of sample holder
• Fast heating rate with good resolution can be maintained
• In TGA one can hold the furnace at 1000°C without any balance
drift, which is not balanced in other thermobalance
• Cooling time is very short therefore Thermogram can be
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recorded
•TGA is a rapid process.
 DISADVANTAGES OF TGA

• Solid sample only must be used in quantitative and

qualitative analysis
• Data interpretation is not always straight forward
• Very small Amount of samples are used but non-
homogeneous material cannot be tested
• Sensitive to heating rate and sample masses results in
shift in temperature
• Limited to sample which undergoes weight change. 18

Melting,
crystal phase change etc. Cannot be studied
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