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Thermal Analysis: Terry A. Ring Chemical Engineering University of Utah

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Ahmed Halawa

The document discusses various thermal analysis techniques including thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), thermal mechanical analysis (TMA), dynamic mechanical analysis (DMA), and differential thermal analysis (DTA). It provides details on the basic principles, experimental setup, data obtained, and applications of each technique. TGA is used to measure weight loss of a sample during heating, DSC measures heat flow, TMA measures dimensional changes, DMA measures viscoelastic properties, and DTA measures temperature differences between a sample and reference.

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Thermal Analysis: Terry A. Ring Chemical Engineering University of Utah

Uploaded by

Ahmed Halawa
168 views18 pages
The document discusses various thermal analysis techniques including thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), thermal mechanical analysis (TMA), dynamic mechanical analysis (DMA), and differential thermal analysis (DTA). It provides details on the basic principles, experimental setup, data obtained, and applications of each technique. TGA is used to measure weight loss of a sample during heating, DSC measures heat flow, TMA measures dimensional changes, DMA measures viscoelastic properties, and DTA measures temperature differences between a sample and reference.

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Thermal Analysis

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Thermal Analysis

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The document discusses various thermal analysis techniques including thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), thermal mechanical analysis (TMA), dynamic mechanical analysis (DMA), and differential thermal analysis (DTA). It provides details on the basic principles, experimental setup, data obtained, and applications of each technique. TGA is used to measure weight loss of a sample during heating, DSC measures heat flow, TMA measures dimensional changes, DMA measures viscoelastic properties, and DTA measures temperature differences between a sample and reference.

Copyright:

© All Rights Reserved
Download as PPT, PDF, TXT or read online from Scribd
Download as ppt, pdf, or txt
168 views18 pages

Thermal Analysis: Terry A. Ring Chemical Engineering University of Utah

Uploaded by

Ahmed Halawa
The document discusses various thermal analysis techniques including thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), thermal mechanical analysis (TMA), dynamic mechanical analysis (DMA), and differential thermal analysis (DTA). It provides details on the basic principles, experimental setup, data obtained, and applications of each technique. TGA is used to measure weight loss of a sample during heating, DSC measures heat flow, TMA measures dimensional changes, DMA measures viscoelastic properties, and DTA measures temperature differences between a sample and reference.

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© All Rights Reserved
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Thermal Analysis

Terry A. Ring
Chemical Engineering
University of Utah
Different Techniques
Thermometric Titration (TT)
Heat of mixing
Thermal Mechanical Analysis (TMA)
Thermal Expansion Coefficient
Dynamic Mechanical Analysis (DMA)
Viscoelastic Properties
Differential Scanning Calorimetric (DSC)
Heat flow during Transitions
Thermal Gravimetric Analysis (TGA)
Weight Loss due to decomposition
Derivative Thermogravimetric Analysis (DTG)
Differential Thermal Analysis (DTA)
Heat of Transitions
Temperature Programmed Desorption (TPD)
Temperature at which gas is desorbed from (catalyst) surface
Emission gas Thermoanalysis (EGT)
Basic Principle
Sample is heated at a constant heating
rate
Samples Property Measured
Wt TGA
Size TMA
Heat Flow DSC
Temp DTA
Gas evolved TPD
TGA
Constant Heating
Rate
Initial Temp
Final Temp
Heating Rate (C/min)
Data
Weight vs Time
Weight vs Temp.
Differential This Data
(DTG)
DSC
DSC
Constant Heating Rate
Initial Temp
Final Temp
Heating Rate (C/min)
Data
Heat flow to sample minus
Heat flow to reference vs
Time (Temp.)
Measures heat of
crystallization

Polymer without weight change in this temperature range


DTA
Sample and Reference Placed in Heater
Constant Heating Rate
Initial Temp
Final Temp
Heating Rate (C/min)
Data
Temp of Sample vs Time (or Temp)
Temp of Reference vs Time (or Temp)
Reference should be inert, e.g. nothing but latent heat
Measures
Heat of crystallization
Glass Transition Temperature
DTA + DTG
TMA
Constant Heating Rate
Initial Temp
Final Temp
Heating Rate (C/min)
Data
Size of Sample vs Time (or Temp.)
Measures
Thermal Expansion Coefficient
Volume change on crystalization or crystal
transformations
Sintering
Glass Transitions in Polymers
TMA

Polymer with glass transition


DMA
Constant Heating Rate
Initial Temp
Final Temp
Heating Rate (C/min)
Data
Force vs Time (or Temp.)
Force delay vs Time (or
Temp.)
Viscoelastic Properties
Storage and Loss Modulus
Measures
Glass Transition
Viscoelastic Properties Polymer with Glass Transition
We have TGA - only
Heating a sample of Calcium oxalate

Ca(C204)*xH2O Ca(C204) *H2O + x-1 H2O


Ca(C204)*H2O Ca(C204) + H2O
Ca(C204) CaCO3 + CO
CaCO3 CaO + CO2
TGA
Constant Heating
Rate
Initial Temp
Final Temp
Heating Rate (C/min)
Data
Weight vs Time
Weight vs Temp.
Differential This Data
(DTG)
TGA Ca(C204)*xH2O
Different Heating Rates
Heating Rate
Heating Too Fast
Overlaps Transitions
Interpretation Problems
Kinetics of Decomposition
Sample Size
Mass Transfer
Convective Mass Transfer
Pore Diffusion
Heat Transfer
Convective Heat Transfer
Thermal Conductivity
Porous solid
Precipitated Zr5O8(SO4)2*15 H2O

This sample was dried fro 48 hrs at 110C before TGA analysis.
What is going on?
Analysis of Filtrate from
Precipitation
Precipitation
5ZrOCl2 + 2H2SO4 + xH2O
Zr5O8(SO4)2*15 H2O (s) + 10 HCl

Decomposition
Zr5O8(SO4)2*15 H2O (s)
Zr5O8(SO4)2*14 H2O (s) + H2O (v)

Zr5O8(SO4)2 5
ZrO2 (s) +2 SO2 (v)

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