Tga Report

Thermalgravimetric Analysis:
Introduction:
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. An Alternate Definition: TGA is a technique in
which, upon heating a material, its weight increases or decreases. A
Simple TGA Concept to remember: TGA measures a sample’s weight
as it is heated or cooled in a furnace.
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.
PerkinElmer offers two types of TGAs, a top-loading TGA 4000™
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. All these quantifiable
applications are usually done upon heating, but there are some
experiments where information may be obtained upon cooling
the TGA 4000 are controlled by PerkinElmer’s proprietary thermal
software, Pyris Software, and have autosampler accessories for
unattended operations.
Thermogravimetric analysis Principle:
TGA gives a quantitative evaluation of any weight changes brought
on by thermally induced transition. The method involves heating a
sample at a controlled rate i.e, for a substance with a known initial
weight, the temperature is raised steadily, and at various time
intervals, the weight changes are recorded as a function of
temperature. The results may be presented in the following two ways:
 as a TG curve (thermogravimetric curve) in which the weight

change is recorded as a function of temperature or time
 as a TG curve derivative (DTG), where the TG curve’s first
derivative is plotted against either temperature or time. The
graph plotted is known as the pyrolysis curve.
Due to the distinct order of physical transitions and chemical
reactions that take place over specified temperature ranges, the TG
curve is unique to a given substance or material. Because of physical
changes and the building and breaking of chemical bonds at high
temperatures, weight changes result. In either inert or reactive
atmospheres, TG typically operates in the 1200oC temperature range.
The molecular structure frequently affects the thermally induced
reaction rates.
Thermogravimetric analysis instrumentation:
The fundamental instrument needed for TG is a precision balance
with a furnace designed to linearly increase temperature over time.
• Recording balance
• Sample holder
• Furnace
• Temperature programmer /controller (thermocouple)
• Recorder
 Recording balance:
A microbalance is used to record a change in mass of sample/

substance. An ideal microbalance must possess following
features:
• It should accurately and reproducibly record the change in mass of
sample in ideal ranges of atmospheric conditions and temperatures.
• It should provide electronic signals to record the change in mass
using a recorder.
• The electronic signals should provide rapid response to change in
mass
• It should be stable at high ranges, mechanically and electrically.
• Its operation should be user friendly
 Sample holder:
• The sample to be studied is placed in sample holder or crucible. It is
attached to the weighing arm of microbalance.
• There are different varieties of crucibles used. Some differ in shape
and size while some differ in materials used.
• They are made up from platinum, aluminium, quartz or alumina and
some other materials like graphite, stainless steel, glass etc
 Furnace:
• The furnace should be designed in such way that it produces a linear
heating range.
• It should have a hot zone which can hold sample and crucible and its
temperature corresponds to the temperature of furnace.
• There are different combinations of microbalance and furnace
available. The furnace heating coil should be wound in such a way
that there is no magnetic interaction between coil and sample or there
can cause apparent mass changes.
 Temperature programmer /controller (thermocouple)
 Temperature measurement is done in no. of ways thermocouple is

the most common technique.
 The position of the temperature measuring device relative to the
sample is very important.
 The major types are:
a) The thermocouple is placed near the sample container

and it has no contact with the sample container. This
isn’t a good arrangement where low pressure are
employed.
b) The sample is kept inside the sample holder but not in
contact with it. This arrangement is better than that of
(a) because is respond to small temperature changes.
c) The thermocouple is placed either in contact with
sample or with the sample container. This is the best
arrangement of sample temperature detection.
 Recorder:
The recording system are mainly of 2 types
1. Time-base potentiometric strip chart recorder.
2. X-Y recorder.
 In some instrument, light beam galvanometer,

photographic paper recorder or one recorder with two or
more pens are also used
 In the X, Y recorder we get curves having plots of
weights directly against temperatures.
 However the percentage mass change against
temperature or time would be more useful.
Working of Thermogravimetric analysis:
In thermogravimetric analysis (TGA), a sample is continually
weighted while heating, as an inert gas atmosphere is passed over it.
Many solids undergo reactions that evolve gaseous by-products. In
TGA, these gaseous by-products are removed and changes in the
remaining mass of the sample are recorded. Three variations are
commonly employed:
 Dynamic TGA - Temperature continues to increase over time as

mass is recorded. This allows simultaneous identification of
how much gas is removed and the temperature at which it
occurs.
 Static TGA - Temperature is held constant as the mass is
measured. This can be used to gain more information on a
decomposition that happens at a certain temperature or to
investigate a material’s ability to withstand a given temperature.
 Quasistatic TGA - Sample is heated in multiple temperature
intervals, and held at those intervals for a time, often until the
mass stabilizes. This is ideal for investigating substances that are
known to decompose in various ways at different temperatures,
and better characterizing the way in which they decompose.
Application of thermogravimetric analysis:

Some of the major applications of TGA are:
 TGA is used for the thermal characterization of polymers.
 Determination of the composition of alloys and mixtures.
 Determining the purity and thermal stability of both primary and
secondary standards.
 It is employed to investigate the moisture content of several
inorganic and organic components, industrial raw materials,
foods, medications, etc.
 Determining the ideal drying temperatures and the
appropriateness of different weighing methods for gravimetric
analysis.
 Used for corrosion studies.
 Also applicable to the study of kinetic of isothermal reactions.
Testing Method:
Heat 50°c to 600°C heating rate 20°c/min (Nitrogen
atmosphere)
Heat 600°C to 800°C heating rate 20°C/min (Oxygen
atmosphere)
Results:
1) HIGHLY VOLATILE CONTENT= 0.212 in %.
HIGHLY VOLATILE CONTENT= 0.023 in mg.
2) POLYMER CONTENT= 72.746 in %.

POLYMER CONTENT= 8.116 in mg.
3) COMBUSTIBLE CONTENT= 25.051 in %.
COMBUSTIBLE CONTENT= 2.795 in mg.
4) ASH CONTENT= 1.991 in %.
ASH CONTENT= 0.222 in mg.

Tga Report

Uploaded by

Copyright:

Available Formats

Tga Report

Uploaded by

Document Information

Original Description:

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Tga Report

Uploaded by

Copyright:

Available Formats

Thermalgravimetric Analysis:

 as a TG curve (thermogravimetric curve) in which the weight

A microbalance is used to record a change in mass of sample/

 Temperature measurement is done in no. of ways thermocouple is

a) The thermocouple is placed near the sample container

 In some instrument, light beam galvanometer,

 Dynamic TGA - Temperature continues to increase over time as

Application of thermogravimetric analysis:

2) POLYMER CONTENT= 72.746 in %.

You might also like