Thermal Analysis

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 Thermal analysis

• Thermal analysis is a branch of materials

science where the properties of materials are
studied as they change with temperature.

• Several methods are commonly used – these

are distinguished from one another by the
property which is measured.

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 Thermal analysis
• Dielectric thermal analysis (DEA): dielectric permittivity and loss factor
• Differential thermal analysis (DTA): temperature difference
• Differential scanning calorimetry (DSC): heat difference
• Dilatometry (DIL): volume
• Dynamic mechanical analysis (DMA): mechanical stiffness and damping
• Evolved gas analysis (EGA): gaseous decomposition products
• Laser flash analysis (LFA): thermal diffusivity and thermal conductivity
• Thermogravimetric analysis (TGA): mass
• Thermomechanical analysis (TMA): dimension
• Thermo-optical analysis (TOA): optical properties

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Common Thermal Analysis Methods and the Properties Measured

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 Introduction
• Thermal analysis is defined as “series of techniques for
measuring the temperature dependency of a physical
property of a certain substance while varying the
temperature of the substance according to a specific
program.”

• The substance referred to here includes reaction

products.

• Physical properties include mass, temperature,

enthalpy, dimension, dynamic characteristics, and
others, and depending on the physical properties to be
measured, the techniques of thermal analysis.
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 Introduction
• Conventionally thermal analysis has been mainly
employed in measurements for research and
development, but in recent times it is used in many
practical applications, as the testing standards on the
basis of thermal analysis have been established, for
example, in quality control in the production field,
process control, and material acceptance inspection.

• It is also applied in wide fields, including polymer,

glass, ceramics, metal, explosives, semiconductors,
medicines, and foods.

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 OBJECTIVES
• The main objective to introduce thermal
analysis and its applications at an entry level
in the pharmaceutical industry.
• In the process, instruments were successfully
calibrated using pharmaceuticals.
• Studying the behavior of pharmaceuticals by
different thermal analysis instruments, under
different conditions and then compare the
results was another objective.

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Basic Principles of Thermal Analysis

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Thermal Analysis Techniques

IUPAC: International Union of Pure and Applied Chemistry

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 Thermal Analysis
• Differential Scanning • Thermal Gravimetric
Calorimetry (DSC) Analysis (TGA)
– Measure heat absorbed or – Measure change in
liberated during heating or weight during heating or
cooling cooling
• Differential Thermal • Thermomechanical
Analysis (DTA) Analysis (TMA)
• They are use for thermal – Measure change in
investigation where dimensions during
thermal change can be heating or cooling
observed and
characterised 10
DIFFERENTIAL SCANNING CALORIMETRY
(DSC)

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 Differencial Scanning Calorimetry
(DSC)
• Characterization of
pharmaceutical compounds and analysis of
complex modern formulations, together with
an increasing need for data to support
regulatory submissions, means that the
pharmaceutical industry now depends on the
range of thermal analysis techniques.

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 Definitions
• A calorimeter measures the heat into or out of a
sample.
• A differential calorimeter measures the heat of a
sample relative to a reference.
• A differential scanning calorimeter does all of the
above and heats the sample with a linear
temperature
ramp.
• Endothermic heat flows into the sample.
• Exothermic heat flows out of the sample.

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 Differential Scanning Calorimetry (DSC)

Temperature

 DSC measures differences in the amount of heat required to increase

the temperature of a sample and a reference as a function of
temperature
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 Circuitry of a DSC

Two separat heating circuits:

• The average-heating controller
(The temperatures of the sample (Ts) and reference (Tr) are measured and
averaged and the heat output is automatically adjusted to increase the
average temperature of the sample and reference in a linear rate)
•
Differential-heating circuit
(Monitor the difference in Ts and Tr, and automatically adjust the power to
either the reference or sample chambers to keep the temperatures equal)

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Sample containers and sampling

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Differential Scanning Calorimeter

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Conventional DSC
Sample Empty

Metal Metal Metal Metal

1 2 1 2
Sample Reference
Temperature Temperature

Temperature
Difference
= Heat
Flow

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 Variants of
• Heat flux DSC
– 1955 Boersma
– 1 large (30 – 100 g) furnace
• Power compensated
– Separate small (1 g) microheaters for sample and
reference
• Hyper DSC
– Very fast scan rates 500°C/min
– Mimic processing conditions
• StepScan DSC
– Short dynamic and isothermal scan steps
– Separate reversible and irreversible effects
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Variants of
DSC

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Differential Scanning Calorimetry
(DSC)

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 DSC Technique
• Principle Heat Flux
• Power Compensation
• Sample Preparation
• -Sample Shape
-Sample pans
-Sample Weight
Experimental Conditions
• -Start Temperature
-End Temperature
-Reference Pan
-Heating Rate
-Effects of heating rate
Purge Gas
• DSC Calibration
•

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 DSC- Principle
DSC is a thermo-analytical technique in which the
difference in the amount of heat required to increase
the temperature of a sample and reference is measured
as a function of temperature.

The differences in heat flow occur with the occurrence of

two major events:
1)The heat capacity of the sample which increases
with temperature (baseline)
2)Transitions that occur in the sample
(events superimposed on the heat capacity baseline)
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 DSC- Principle
• Heat Flow Rate is expressed in a variety of units
which can also be normalized for the weight of
sample used

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Principle Of DSC

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Typical DSC Curve

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 DSC Thermogram

Oxidation
Crystallisation Cross-
Linking
(Cure)

Glass
Transition

Melting

Temperature
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Transitions in a DSC Curve

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 DSC – Applications
• Glass Transition Temperature (Tg)
• Glass Transition Size (ΔCp)
• Crystallization temperature (Tc)
• Crystallinity (based on J/g and adjusted to %)
• Polymorphic Transitions.
THANK YOU

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