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POST GRADUATE PROGRAM
Fiber Chemistry and Physics
Seminar on:- Thermo Gravimetric analysis (TGA)
Worku Tegegene
First Year MSc. in Textile Chemistry
Submitted to: Assoc. Professor. Adane H.
January,2021
.
Outlines
Introduction
Theoretical background
Working Principles
Data Interpretation and Analysis
TGA Characterization
summery
References
Introduction
Physical changes :- melting, vaporization,
Heat
Change in property
Chemical changes :- oxidation, decomposition …
Applied thermal
analysis techniques
Thermal Analysis
Thermo Gravimetric
Analysis
Mass
Evolved Gas
Analysis
Gas
decompose
Dilatometry volume
Differential Thermal
Analysis
ΔT ΔH
Differential Scanning
Analysis.
Dynamic
Mechanical
Analysis
Physical Properties
Deformation
Laser Flash
Analysis
Thermal
diffusivity
TGA
Mass of material as a
functions of temperature.
Reactant(s)  Product(s) + Gas
Gas + Reactant(s)  Product(s)
(a mass loss)
(a mass gain)
Processes occurring without
change in mass cannot be
studied by TG.
Dynamic TGA Static TGA Quasi static TGA
Theoretical background
Thermal analysis was first introduced by Le
Chatelier in 1887
The measurement of mass change using
temperature thermogravimetry (TG) was
discovered by Honda, a physicist from Japan.
Instrumentation
Restoring Force
Null Detector
weight change
Operating Principles
Changes in the mass of a
sample are studied while the
sample is subjected to a
program
Changes in temperature affect the
sample:- desorption, absorption,
sublimation, vaporization, oxidation
It is used in analysis of volatile prod
gaseous products lost,
desorption, absorption,
sublimation, vaporization,
oxidation, reduction and
decomposition ….change
melting, crystallization …no change
Data Interpretation and Analysis
Plateau: Thermal stability (AB)
Weight/Mass Loss (BC)
Procedural Decomposition
Temperature (B)
Composition
A: No mass change over entire
range of temperature.
B: Desorption/Drying. Mass loss
is
large followed by mass plateau.
C: Single Stage Decomposition
D: Multistage Decomposition
E: Similar to D but either due to
faster heating rates or due to no
intermediaries
F: Atmospheric Reaction, Increase
in mass, reactions like surface
oxidation
G: Similar to Curve F, but product
decomposes at higher
temperatures.
no change in weight (AB &CD)
portion BC :- weight change
The weight remains constant
up to a temperature of
473°C, thermally stable
decomposition starts @473°C
The loss in weight continues up to
608°C & ends up @ 608°C
portion CD:-sample remains
constant
Factors affecting the TG curve Instrumental factors :-Furnace heating rate &
Furnace atmosphere
Sample characteristics:- Weight of the sample &Sample particle size
Plateau:AB no change in mass
Procedural Decomposition
Temperature:Ti&Tf
Composition:amount/percentage/weig
ht of a compound
TGA Characterization for selected polymers
1. nylon 6,6
.
thermal degradation
wight loss for nylon 6,6
under
a
nitrogen
purge
. TGA degradation for
two different HDPE
bottles
Weight loss
2. high density polyethylene (HDPE)
3, SAN and butadiene components
compositional analysis of polymeric
blends
significant weight loss
overlapping decomposition
butadiene :-rubbery component
Applications of TGA
Thermal Stability:- decomposition mechanism
Material characterization:-
Compositional analysis:- temperature programm
Simulation of industrial processes:-
industrial reactors
Kinetic Studies:- controlling chemistry
Corrosion studies:- studying oxidation
summery
TGA analysis is widely used to characterize
and verify materials.
TGA is applicable to most industries.
Environmental, food science, pharmaceutical,
and petrochemical
applications are the mainstay of Thermo
gravimetric Analysis and Evolved Gas Analysis
References
Gurdeep R. Chatwal, Sham K. Anand, Himalaya Publishing House, 2002.
Instrumental Methods Of Chemical Analysis: Thermal Methods, pg. 2.701, 5th
Ed.
T. Hatakeyama and F.X. Quinn, Jhon Wiley and Sons Publications, 1999.
Thermal Analysis Fundamentals and Applications to Polymer Science:
Thermogravimetry, pg. 45-71, 2nd Ed.
Coats, A. W.; Redfern, J. P., 1963. "Thermogravimetric Analysis: A Review",
pg. 88: 906–924.
Fleming Polymer Testing And Consultancy, http://www.flemingptc.co.uk/our-
services/dsc-tga/
Sharma B.K. Goel Publishing House “Instrumental Methods of Analysis” pg.
234-237.
Thermal Analysis Dr. S. Anandhan, Asst. Professor, Dept. of Met. And Mat.
Engg., NITK
D. A. Skoog et al., Principles of instrumental analysis, fifth edition, Harcourt
Publishers, 2001.
Analytical Compendium, Chapter 5, Section 2,
http://old.iupac.org/publications/analytical_compendium/Cha05sec2.pdf
TGA-SEM Analysis of Fiber Chemistry

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TGA-SEM Analysis of Fiber Chemistry

  • 1. POST GRADUATE PROGRAM Fiber Chemistry and Physics Seminar on:- Thermo Gravimetric analysis (TGA) Worku Tegegene First Year MSc. in Textile Chemistry Submitted to: Assoc. Professor. Adane H. January,2021 .
  • 2. Outlines Introduction Theoretical background Working Principles Data Interpretation and Analysis TGA Characterization summery References
  • 3. Introduction Physical changes :- melting, vaporization, Heat Change in property Chemical changes :- oxidation, decomposition … Applied thermal analysis techniques Thermal Analysis
  • 4. Thermo Gravimetric Analysis Mass Evolved Gas Analysis Gas decompose Dilatometry volume Differential Thermal Analysis ΔT ΔH Differential Scanning Analysis. Dynamic Mechanical Analysis Physical Properties Deformation Laser Flash Analysis Thermal diffusivity
  • 5. TGA Mass of material as a functions of temperature. Reactant(s)  Product(s) + Gas Gas + Reactant(s)  Product(s) (a mass loss) (a mass gain) Processes occurring without change in mass cannot be studied by TG. Dynamic TGA Static TGA Quasi static TGA
  • 6. Theoretical background Thermal analysis was first introduced by Le Chatelier in 1887 The measurement of mass change using temperature thermogravimetry (TG) was discovered by Honda, a physicist from Japan.
  • 8. Operating Principles Changes in the mass of a sample are studied while the sample is subjected to a program Changes in temperature affect the sample:- desorption, absorption, sublimation, vaporization, oxidation It is used in analysis of volatile prod gaseous products lost, desorption, absorption, sublimation, vaporization, oxidation, reduction and decomposition ….change melting, crystallization …no change
  • 9. Data Interpretation and Analysis Plateau: Thermal stability (AB) Weight/Mass Loss (BC) Procedural Decomposition Temperature (B) Composition
  • 10. A: No mass change over entire range of temperature. B: Desorption/Drying. Mass loss is large followed by mass plateau. C: Single Stage Decomposition D: Multistage Decomposition E: Similar to D but either due to faster heating rates or due to no intermediaries F: Atmospheric Reaction, Increase in mass, reactions like surface oxidation G: Similar to Curve F, but product decomposes at higher temperatures.
  • 11. no change in weight (AB &CD) portion BC :- weight change The weight remains constant up to a temperature of 473°C, thermally stable decomposition starts @473°C The loss in weight continues up to 608°C & ends up @ 608°C portion CD:-sample remains constant Factors affecting the TG curve Instrumental factors :-Furnace heating rate & Furnace atmosphere Sample characteristics:- Weight of the sample &Sample particle size
  • 12. Plateau:AB no change in mass Procedural Decomposition Temperature:Ti&Tf Composition:amount/percentage/weig ht of a compound
  • 13. TGA Characterization for selected polymers 1. nylon 6,6 . thermal degradation wight loss for nylon 6,6 under a nitrogen purge
  • 14. . TGA degradation for two different HDPE bottles Weight loss 2. high density polyethylene (HDPE)
  • 15. 3, SAN and butadiene components compositional analysis of polymeric blends significant weight loss overlapping decomposition butadiene :-rubbery component
  • 16. Applications of TGA Thermal Stability:- decomposition mechanism Material characterization:- Compositional analysis:- temperature programm Simulation of industrial processes:- industrial reactors Kinetic Studies:- controlling chemistry Corrosion studies:- studying oxidation
  • 17. summery TGA analysis is widely used to characterize and verify materials. TGA is applicable to most industries. Environmental, food science, pharmaceutical, and petrochemical applications are the mainstay of Thermo gravimetric Analysis and Evolved Gas Analysis
  • 18. References Gurdeep R. Chatwal, Sham K. Anand, Himalaya Publishing House, 2002. Instrumental Methods Of Chemical Analysis: Thermal Methods, pg. 2.701, 5th Ed. T. Hatakeyama and F.X. Quinn, Jhon Wiley and Sons Publications, 1999. Thermal Analysis Fundamentals and Applications to Polymer Science: Thermogravimetry, pg. 45-71, 2nd Ed. Coats, A. W.; Redfern, J. P., 1963. "Thermogravimetric Analysis: A Review", pg. 88: 906–924. Fleming Polymer Testing And Consultancy, http://www.flemingptc.co.uk/our- services/dsc-tga/ Sharma B.K. Goel Publishing House “Instrumental Methods of Analysis” pg. 234-237. Thermal Analysis Dr. S. Anandhan, Asst. Professor, Dept. of Met. And Mat. Engg., NITK D. A. Skoog et al., Principles of instrumental analysis, fifth edition, Harcourt Publishers, 2001. Analytical Compendium, Chapter 5, Section 2, http://old.iupac.org/publications/analytical_compendium/Cha05sec2.pdf