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Name .

Anas Yaqoob
Regis.No. 2017-pe-31

(Thermo-Gravimetric Analysis):
The experiment by which mass of given material is estimated over some
known time frame by thermal analysis is called as thermo gravimetric analysis.

Figure.1:lab scale TGA


What is the purpose of TGA?
The purpose behind thermo gravimetric analysis is to give us
information about physical process like desorption, Absorption, phase
transition as well as Chemical process like thermal degradation and chemical
absorption.

Example:
If we want calculation about thermal stability of material then it is done
by TGA. it depends upon mass of material if mass of material does not change
with respect to given temperature range provided than we can say that this
material is thermally stable. But if mass loses with change in temperature it is
thermally unstable and material may also start degradation with increasing
temperature.
Apparatus for TGA:
Thermo-gravimetric analyzer: this is the apparatus from this thermal
gravimetric analysis is perform. With the help of this apparatus mass material
can be measured that is placed into it with respect to change in temperature
range over time.

Base calculations:
There are three base calculations in thermo gravimetric analyzer.

1. Mass

2. time

3. Temperature

others measures can be done by above notice estimation.

Apparatus description:
A standard thermo gravimetric analyzer is comprised of an accurate
balance having test container situated inside the heater tube.

The temperature program is automatically attached to PC to investigate the


temperature control. With the help of this we can do our analysis for various
temperature readings at single point. For the most part the temperature is
expanded continually to watch thermal response and discover mass loses. Yet,
for certain analyses we have to know the approximated mass loss of material
that is the reason we utilize the temperature controller.

Different atmospheric conditions for Thermal reaction:


By Different atmospheric conditions thermal reaction can do are
(vacuum , Ambient air ,inert gas, various pressure ,liquid vapors)

Graph for different polymers:


Data collected from thermal reaction is drawn in the form of graph.

X-axis lable as (temperature).

Y-axis lable as (mass).


Figure 2: TGA curves for various polymers
(PVC, PMMA, LDPE, PTFE, PI)
From different curves as shown above it is clear that as temperature
increases quantity of mass decreases i.e mass loss of polymers
increases.
It is also stated that if maximum moisture content is present in the
material than degradation of material will accur at high temperature
and deviation of TGA graph can be seen from its original position.

Designing of TGA:
Heating tube is guided with nitrogen (N2) gas to offer the tube with
an idle situation. The purity of the torpid gas ought to be amazingly over the
top. It isn't basic that the gasoline equipped is idle we in like manner can finish
assessments in closeness of responsive gas nearby Oxygen to discover warm
adequacy in a particular circumstance.

The needle valve makes a positive head (stress) to hold the favored
stream rate of nitrogen fuel to be cultivated. To get a most satisfying float
charge of latent gasoline of various qualities are tested. Extremely little mass
(ideally 1-10mg) of material under perception is embedded into the heating
tube. The mass of the example should be saved as little as suitable relying on
the heating rate, affectability of the parity and the homogeneity of the
example. Vacuum pump at the last a piece of the schematic chart is utilized to
pump out any undesirable gas in the heating tube.

Figure.3 schematic of Thermo Gravimetric Analyser


Description:
The PC program stores everything about data motioned to it by the
thermo gravimetric analyzer for time, temperature and change in mass. At the
end the PC program (recording device) have ability to show required TGA .The
graphs weight balance gauges slight of progress in mass of the material under
discernment. The adjustment should have breaking point of least 10 mg and
affectability of +-10 μg.

A temperature sensor is in like manner joined to the machine which has


accuracy of +-0.1oC to observe the temperature of the heating tube. The pot
used in this assessment should in like manner be inert to material under
observation.

Methodology:
 Take weighted amount in standard form and then it is placed in sample
crucible.
 At room temperature and pressure we have to put sample crucible in
TGA.
 By temperature controller Constant heat rate should be set.
 % loss mass is noted of provided material with respect to time and
temperature.
 When significant mass loss of material will accur experiment will be
ended.
 Then container is exited.
 Then TGA should cool by cooling fan button at temperature controller
for next performance.
 5-10 mg of material is required for doing experiment and temperature
range should be in range between (25-600)oC.

Reference :
 Manual of TGA by victory firms and ISPS.
 Book: Fundamental of Polymeric material by Christopher
S.Brazel.
 https://www.ebatco.com/laboratory-
services/chemical/thermogravimetric-analysis-tga/
 https://www.researchgate.net/figure/Schematic-diagram-of-
TGA_fig1_7042754

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