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Thermal Analysis: Terry A. Ring Chemical Engineering University of Utah
Thermal Analysis: Terry A. Ring Chemical Engineering University of Utah
Thermal Analysis: Terry A. Ring Chemical Engineering University of Utah
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
• Sample’s 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
This sample was dried fro 48 hrs at 110C before TGA analysis.
What is going on?
Analysis of Filtrate from
Precipitation
• Precipitation 15 H2O Water Loss Wt. Loss % loss
1 18.0152 1.721573
• 5ZrOCl2 + 2H2SO4 + xH2O 2 36.0304 3.443146
Zr5O8(SO4)2*15 H2O (s) + 10 HCl 3 54.0456 5.164719
4 72.0608 6.886292
5 90.076 8.607865
• Decomposition 6 108.0912 10.32944
7 126.1064 12.05101
• Zr5O8(SO4)2*15 H2O (s) 8 144.1216 13.77258
Zr5O8(SO4)2*14 H2O (s) + H2O (v) 9 162.1368 15.49416
10 180.152 17.21573
11 198.1672 18.9373
• Zr5O8(SO4)2 5 12 216.1824 20.65887
ZrO2 (s) +2 SO2 (v) 13 234.1976 22.38045
14 252.2128 24.10202
15 270.228 25.82359
SO2 1 64.0588 31.9452
2 128.1176 38.0668