Thermal Absorptiometry

(Thermal Analysis)

Prepared by:
Bade, Michaela Lei A.
 What is Thermal Absorptiometry

• It 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
 Types of Thermal Analysis

• TGA (Thermo gravimetric analysis)

• DTA(Differential Thermal Analysis)
• DSC (Differential Scanning Calorimetry)
 What is Thermogravimetric
Analysis
• Thermogravimetric analysis or thermal gravimetric analysis (TGA) is
a method of thermal analysis in which the mass of a sample is measured
over time as the temperature changes.
• This measurement provides information about physical phenomena, such
as phase transitions, absorption, adsorption and desorption; as well as
chemical phenomena including chemisorptions, thermal decomposition,
and solid-gas reactions (e.g., oxidation or reduction).
There are three types of thermogravimetry:
• Isothermal or static thermogravimetry: In this technique, the
sample weight is recorded as a function of time at a constant
temperature.
• Quasistatic thermogravimetry: In this technique, the sample
temperature is raised in sequential steps separated by isothermal
intervals, during which the sample mass reaches stability before
the start of the next temperature ramp.
• Dynamic thermogravimetry: In this technique, the sample is
heated in an environment whose temperature is changed in a
linear manner.
 Differential thermal analysis (DTA)
• is
a thermoanalytic technique that is similar to
differential scanning calorimetry. In DTA, the material under study and an
inert reference are made to undergo identical thermal cycles, (i.e., same
cooling or heating programme) while recording any temperature difference
between sample and reference.
• This differential temperature is then plotted against time, or against
temperature (DTA curve, or thermogram). Changes in the sample, either
exothermic or endothermic, can be detected relative to the inert reference.
Thus, a DTA curve provides data on the transformations that have
occurred, such as glass transitions, crystallization, melting and
sublimation. T
 Application
• A DTA curve can be used only as a finger print for
identification purposes but usually the applications of this
method are the determination of phase diagrams, heat change
measurements and decomposition in various atmospheres.
• DTA is widely used in the pharmaceutical[3] and food
industries.
• DTA may be used in cement chemistry,mineralogical
research and in environmental studies.
 Differential scanning calorimetry (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. Both the sample and reference are maintained
at nearly the same temperature throughout the experiment.
There are two main types of DSC:

Heat-flux DSC which measures the difference in heat flux

between the sample and a reference (which gives it the
alternative name Multi-Cell DSC) and Power differential
DSC which measures the difference
in power supplied to the sample and a reference.[
 Heat-flux DSC
• With Heat-flux DSC, the changes in heat flow are calculated by integrating
the ΔTref- curve. For this kind of experiment, a sample and a reference
crucible are placed on a sample holder with integrated temperature sensors
for temperature measurement of the crucibles.
• This arrangement is located in a temperature-controlled oven. Contrary to
this classic design, the distinctive attribute of heat-flux DSC is the vertical
configuration of planar temperature sensors surrounding a planar heater.
This arrangement allows a very compact, lightweight and low heat
capacitance structure with the full functionality of a DSC oven.
 Power differential DSC

• For this kind of setup, also known as Power compensating DSC, the
sample and reference crucible are placed in thermally insulated furnaces
and not next to each other in the same furnace like in Heat-flux-DSC
experiments.

• Then the temperature of both chambers is controlled so that the same

temperature is always present on both sides. The electrical power that is
required to obtain and maintain this state is then recorded rather than the
temperature difference between the two crucibles.
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