Scribd
Upload
5 views16 pages

unit III TGA

Unit III covers various spectrometric and thermogravimetric methods, including thermal analysis techniques such as TGA, DTA, and DSC, along with chromatographic methods like gas chromatography and HPLC. It discusses the applications of spectrophotometry, including infrared, UV, visible spectrophotometry, NMR, and Raman spectroscopy. The document emphasizes the importance of thermal analysis in determining thermal stability, decomposition temperatures, and other material properties.

Uploaded by

sukrit syal
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
5 views16 pages

unit III TGA

Unit III covers various spectrometric and thermogravimetric methods, including thermal analysis techniques such as TGA, DTA, and DSC, along with chromatographic methods like gas chromatography and HPLC. It discusses the applications of spectrophotometry, including infrared, UV, visible spectrophotometry, NMR, and Raman spectroscopy. The document emphasizes the importance of thermal analysis in determining thermal stability, decomposition temperatures, and other material properties.

Uploaded by

sukrit syal
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 16

Unit III: Spectrometric & Thermo-

gravimetric Methods
 Thermal Method of Analysis: Elementary discussions
of TGA, DTA & DSC.
 Chromatographic Methods of Separation, Gas
Chromatography, HPLC & Potentiometric methods
 Spectrophotometer : Infrared, Ultra-Violet and
Visible spectrophotometer, NMR and Raman
Spectroscopy and their application

Dr. Manjari Sharma 1


Thermal Method of Analysis
TGA: Thermo Gravimetric Analysis
DTA: Differential Thermal analysis
DSC: Differential Scanning Calorimetry

Dr. Manjari Sharma 2


Thermal analysis
Provides information about the Thermal Stability of
Compounds /Compositions.
Thermal analysis can be done using
1) Differential Scanning Calorimetry (DSC),
2) Thermal Gravimetric Analysis (TGA),
3)Thermal Method of Analysis (DTA)
3) Dynamic Mechanical Analysis (DMA) &
4) Thermo Mechanical Analysis (TMA).

Dr. Manjari Sharma 3


Thermal analysis
Following parameters can be studied by Thermal
analysis:
 Melting Point using DSC
 Glass transition temperature using DSC, DMA &
TMA.
 Degree of Cure using DSC.
 Decomposition temperature using DSC & TGA.
 Component quantification using TGA
 Percentage Crystallization using DSC
 Co-efficient of thermal expansion using DSC.

Dr. Manjari Sharma 4


TGA: Thermo -Gravimetric
Analysis
Thermo-gravimetric 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.
 Upon heating a material, its weight increases or
decreases
 measures a sample’s weight as it is heated or
cooled in a furnace

Dr. Manjari Sharma 5


Analysis by TGA

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.

Dr. Manjari Sharma 6


TGA Model
Perkin Elmer Thermal Analyzer

Dr. Manjari Sharma 7


Analyser
Analyzer for TGA is often referred to as a
thermo balance.
There are two essential components
i) Furnace system
ii) Balance system.
It informs about the
Thermal degradation,
Kinetics of materials and
Service lifetime prediction
along with the thermal breakdown as a
function of time in an instrument called
thermo-balance.
Dr. Manjari Sharma 8
TGA Procedure
 Thermal degradation of samples is analysed in the
dynamic mode and weight loss of samples is subject to
controlled temperature program.
 The samples are taken in a crucible situated in the electric
furnace and heated from room temperature 40-500°C.
 The approximate 6-10 mg of each sample is used for
analysis. Each sample is subjected to heating rate of
10°C/min under nitrogen atmosphere.
 Prior to conduct the experiment approximately 10
milligram samples are dried in vacuum oven at 60 C for 2
hours. The onset of degradation temperature is recorded
for each sample.

Dr. Manjari Sharma 9


How is a TGA Thermal Curve displayed?

The abscissa (X-axis) can be displayed as time or


temperature and the ordinate (Y-axis) can be displayed as
weight (mg) or weight percent (%).

Dr. Manjari Sharma 10


Classification of TGA Curves

Dr. Manjari Sharma 11


What does a TGA Thermal Curve look like?

 A TGA thermal curve is


displayed from left to
right.
 The descending TGA
thermal curve indicates
a weight loss occurred.

Dr. Manjari Sharma 12


ANALYSIS OF CALCIUM OXALATE
DECOMPOSITION.
A 15.013 mg sample of
calcium carbonate was
analyzed By TGA.
Temperature Program =
Heat Cycle : from 100 °C
to 900 °C @ 10 °C/minute
in Nitrogen atmosphere
with a purge rate of 20
mL/minute.

Dr. Manjari Sharma 13


ANALYSIS OF TGA OF CALCIUM
OXALATE DECOMPOSITION.

Dr. Manjari Sharma 14


Dr. Manjari Sharma 15
Application of TGA
 Determination of mass loss in composites/blends
 Thermal stability assessment
 Percentage weight loss of components
 Percentage of moisture and volatiles
 Percentage of fillers and additives
 Degradation temperature and decomposition kinetics
study

Dr. Manjari Sharma 16

You might also like