Differential Thermal

Analysis
Khawar yaqoob
M13-330
 Thermal analysis
 When a material is heated its structural and chemical composition
can undergo changes such as fusion, melting, crystallization,
oxidation, decomposition, transition, expansion and sintering.

 Using Thermal Analysis such changes can be monitored in every

atmosphere of interest. The obtained information is very useful in
both quality control and problem solving.
 Techniques for thermal analysis

 Thermogravimetric Analysis (TGA)

 Differential Thermal Analysis (DTA)

 Differential Scanning Calorimetry (DSC)

 Differential Thermal Analysis (DTA)
 In Differential Thermal Analysis, the temperature difference that
develops between a sample and an inert reference material is
measured, when both are subjected to identical heat – treatments
 This is a comparison method
 Analytical method for recording the difference in temperature
(∆T) b/w a substance and an inert reference material as a function
of temperature or time
 Any transformation – change in specific heat or an enthaply of
transition can be detected by DTA
 In DTA both test sample & an inert reference material (alumina) –
controlled heating or cooling programming
 Differential Thermal Analysis (DTA)
DTA is used by analysts for analyzing certain properties
like:
• Glass transition temperature
• Chemical reactions
• Crystalline phase changes
• Decomposition of glass batch materials
∆T VS Temp.
Sharp Endothermic – changes
in crystallanity or fusion
Broad endotherms -
dehydration reaction
Physical changes usually
result in endothermic curves
Chemical reactions are
exothermic
Phenomena causing changes in
temperature
 Apparatus

 Differential thermal analysis mainly consist of

1. Sample holder comprising thermocouples, sample containers

and a ceramic or metallic block.
2. Furnace.
3. Temperature programmer.
4. Recording system.
DTA apparatus
Diagram
 Procedure
 Heart of the analysis – heating block
 Identical pair of cavities for the sample, ref. material
 Whole unit is set in an oven- control pressure
 Thermocouple is place directly in contact with the sample and
another in contact with the reference
 Temperature of the block is raised, the temperature of the sample
& reference follow
 Zero temp. difference – no physical or chemical change
 If any reaction – difference in ∆T
Graphical Representation
Factors affect results in DTA
Factors that influence DTA curve
DTA

Advantages:
• Instruments can be used at very high temperatures
• Instruments are highly sensitive
• Characteristic transition or reaction temperatures can be
accurately determined
• Accurate Low detection limit (up to 10-7 g) Reliable data Easy to use Rather
cheap Minimal sample preparation

Disadvantages:

• Uncertainty of heats of fusion,

• Transition or reaction estimations is 20-50%
• Destructive Limited range of samples Time consuming Usually not qualitative
Applications

 Quantitative identification and

purity assessment
of materials are accomplished by comparing the
DTA curve of sample to that of a reference curve
 Impurities may be detected by depression of the
M.P
 Pharm industry Food industry Cosmetic industry

Applications

Polymer industry Research and Development Ceramic industry

 Limitations

 ΔT determined not so accurate (2,3 0C)

 Very small value of ΔT cannot be determined and
quantified
 Due to heat variation between sample and reference
makes it less sensitive