thermal analysis

Views:
 
Category: Education
     
 

Presentation Description

DSC,TG

Comments

By: mahendranip (36 month(s) ago)

plz allow me for down load this i need it ......... thanks and regards

By: ammufornani (41 month(s) ago)

please allow me to download

By: babuagoodboy (42 month(s) ago)

i want this ppt can u plzz send this ppt to my mail

By: lordes (43 month(s) ago)

ok

By: iam4u15 (45 month(s) ago)

Hi Sir, I am very much impress with your slides,So can you share with me thes slides. Best regards, Ravi

Presentation Transcript

Thermal Analysis : 

Thermal Analysis Terry A. Ring Chemical Engineering University of Utah

Different Techniques : 

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 : 

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 : 

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

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 : 

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 : 

DTA + DTG

TMA : 

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 : 

TMA Polymer with glass transition

DMA : 

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 : 

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 : 

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 : 

TGA – Ca(C204)*xH2O

Different Heating Rates : 

Different Heating Rates

Heating Rate : 

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 : 

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 : 

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)