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Thermal Analysis Method

Thermal analysis method

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692 views28 pages

Thermal Analysis Method

Thermal analysis method

Uploaded by

hanumanpujari.77
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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THERMAL ANALYSIS OF

COMPOUNDS
Master of science in chemistry

Submitted by:
Himanshu Shekhar Das
Roll no:- 21CHE20
Semester:- 3rd
GUIDED By:
Malaya
naik
CONTENTS
(1) introdution of thermal analysis of compounds
(2) types or techniques for thermal analysis
(3) introdution of Thermogravimetry analysis(TGA)
(4)mechanism for weight change in TGA
(5) principles for TGA
(6) what TGA inform you
(7) instruments for TGA
(8) analysis of TGA data
(9) classification of TGA curve
(10) Factors affecting the TGA curve
(12) Examples
(13) limitation
THERMAL ANALYSIS
OF COMPOUNDS
Thermal analysis includes those techniques in
which some physical parameter of the system
is determined and recorded as a function of
temperature (ΔT)
- the estimations or calculations are based on
dynamic relationship between temperature
and mass, Volume, heat of reaction
- temperature is primary in thermal analysis.
TYPES OR
TECHNIQUES
TGA:- THERMOGRAVIMETRY
ANALYSIS
Defination:-
Thermogravimetry is a technique
measuring the variation in mass of a
sample when it undergoes temperature
scanning in a controlled atmosphere this
variation in mass can be either a loss of
mass (vapour emission) or a gain of
mass( gas fixation)
MECHANISM OF WEIGHT
CHANGE IN TGA
WEIGHT LOSE:
(1) Decomposition: the breaking apart of chemical bond
(2)Evaporation: the loss of volatiles with elevated
temperature
(3) Reduction: interaction of sample to a reducing
atmosphere ( hydrogen, ammonia ,etc..)
• WEIGHT GAIN:
• (1) Oxidation:- interaction of the sample with
an oxidizing atmosphere
• (2) absorption or adsorption
PRINCIPLES
FOR TGA:
(1) The substance
understudy is either
heated or cooled at a
controlled rate the
weight of the substance
is recorded as a function
of time and temperature
(2) if the temperature
varies during the study
then the weight is
plotted as a function of
temperature
(3) if the
temperature kept
constant the
weight is plotted
as a function of
time
(4) the change in
weight is used for
quantitative
analysis and the
change in
temperature at
which the change
WHAT TGA
INFORM YOU ?
(1)thermal stability of materials:
explains
A. decomposition mechanism
B. fingerprint materials for
identification
(2) oxidative stability of
materials. indicate the
A. oxidation of metals in air
B. oxidative decomposition of
organic substances in air
C. thermal decomposition in
inert atmosphere
(3) composition of multi - component
system:- different behaviours of the
sample on the temperature scale can be
identified and it helps to formulated with
reaction mechanisms.
4) estimated lifetime of a product:-
5) kinetic decomposition of materials
6) the effect of reactive or corrosive
atmosphere on mater :--corrosive studies
of materials
7) The amount of moisture and volatile
content in materials.
loss of moisture , drying , desorption.
INSTRUMENTS: -IT HELPS TO RECORD THE
CHANGE OF MASS
:- IT CONSIST OF FOLLOWING MAIN PARTS
TGA 5500 MACHINE
(1) Sample Holder :- it should be made by high
thermal conducting material like( quartz,
glass,alumina, pt, graphite etc..) because these
materials are not affected by high temperature
Geometry:- geometry should be flat surface because
the evolution of gas is taking place very easily
(2)Temperature sensor:-
(a) Temperature measurement of the sample is done
with the help of temperature sensor
(b) it should have high thermal conductivity
(C) it placed closed with the sample
(3) Furnace:-
(a) The design of furnance should be in such a way
that it produces a linear heating rate
(4) Temperature programmer:- it control the
temperature of furnace
(5) Atmosphere controller:-
(a) To stop the reaction of gases present in the
furnace with the sample atmosphreric controller
is required
(b) inert gases will be circulated through that
atmosphere to stop the reactions
(6)Balance:-
It measure the loss of mass or gain of mass
Of the sample
(7) Recorder :-
it connected with both the temperature
sensor and Balance which recorded the loss of
mass or gain of mass with temperature and
plotted the graph
FACTORS AFFECTING
THE TGA CURVE
-any experimental parameter that can effect the
reaction rate will change the shape of the curve
These things include
(1) Geometry of the sample holder
(2) Heating rate :-
High heating rate create thermal lag which affect
the curve
(3) Reactive Gases are influnced the TGA curve
(4) Sample masses :- high mases sample gives
thermal gradiant which affect the curve
Effect of sample weight on TGA Curve
TGA OF COPPER SULPHATE
PENTAHYDRATE
LIMITATIONS
only solid substance can be
• (1)
studied in TGA
• (2) exact temperature can not be
detrmined of the sample

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