Thermo Analysis Techniques

1.What is Thermogravimetric Analysis?

Also known as “thermal gravimetric analysis” or “TGA,” thermogravimetric analysis is a method of
thermal testing wherein the tested substance is subjected to constant changes in temperature over
time. This test is administered in order to induce a thermal reaction, so that resulting changes in
the mass or weight of the tested substance as a result of the reaction may be observed and
analyzed.

By measuring and monitoring mass, temperature, and time as base measurements during testing,
thermogravimetric analysis can also use this information to derive a wide variety of additional
measurements, such as the loss of water, solvent, or plasticizer in the material, the amount of filler
in the material, and the material’s rate of oxidation and/or decarboxylation.

How Does Thermogravimetric Analysis Work?

TGA is conducted using an instrument called a thermogravimetric analyzer, which is a furnace
containing a sample pan supported by a precision balance. This precision balance is connected to a
highly sensitive scale outside of the furnace that can record minute changes in mass of the
substance placed on the sample pan as it is heated.

During testing, a gas capillary inside the furnace continuously introduces a gas that purges the
volume of the furnace, ensuring a consistent and controlled environment for testing. Reactive
gases, gaseous and combustion products produced by the sample during heatingare all expelled
from a gas outlet located at the back of the furnace.

TGA typically occurs in stages. At each stage, the internal temperature of the furnace is increased
in a linear fashion or held at a constant temperature to produce a thermal reaction from the tested
substance. The effect of each stage is charted by comparing weight on the Y Axis to time or
temperature on the X Axis. This type of chart is known as a “TGA Thermal Curve.”
What Are the Applications of TGA?

TGA is primarily used to characterize materials by measuring their change in mass as a function of
temperature. Through this process and the measurements that can be very accurately derived
from it, TGA can be used to determine a substance’s:

• Changes in mass due to decomposition, oxidation, evaporation, or combustion

• Absorbed moisture content

• Volatilization rate of materials

• Thermal cracking point of base fluids or formulations contained within the substance

TGA is especially useful for studying polymer-based products that need to react to (or withstand)
high heat or rapid temperature changes in specific ways.

The most common application of TGA in business and industry is to test the thermal resistance of
products for quality assurance and safety purposes.

Oxidation reactions are highly observable and measurable in TGA, and so TGA is frequently used to
study them, especially in products such as copper alloys, which require high resistance to
oxidation.

When a sample is heated using TGA, it frequently loses mass. By analyzing the TGA thermal curve,
TGA can show researchers exactly what is being lost during combustion, which can provide
valuable information about both the composition of the material and how the material will react
to temperature fluctuations.

Both oxidation and combustion research is important for determining how products should be
stored, distributed, produced, and applied in practice. TGA is frequently used to test
Pharmacologic products before they are approved for distribution and patient use.

2.Differential Thermal Analysis

A technique in which the difference in temperature between the sample and a reference material
is monitored against time or temperature while the temperature of the sample, in a specified
atmosphere, is programmed.
The sample and the reference are placed symmetrically in the furnace. The furnace is controlled
under a temperature program and the temperature of the sample and the reference are changed.
During this process, a differential thermocouple is set up to detect the temperature difference
between the sample and the reference.
Also, the sample temperature is detected from the thermocouple on the sample side.

Graph (a) shows the temperature change of the furnace, the reference and the sample against
time.
Graph (b) shows the change in temperature difference (ΔT) against time detected with the
differential thermocouple.
ΔT signal is referred to as the DTA signal.

Matters that do not change in the measurement temperature range (usually α-alumina) are used
as reference.

When the furnace heating begins, the reference and the sample begin heating with a slight delay
depending on their respective heat capacity, and eventually heat up in according to the furnace
temperature.
ΔT changes until a static state is reached after the heating begins, and after achieving stability,
reaches a set amount compliant with the difference in heat capacity between the sample and the
reference. The signal at the static state is known as the baseline.

When the temperature rises and melting occurs in the sample, for example, the temperature rise
stops as shown in graph (a) and the ΔT increases. When the melting ends, the temperature curve
rapidly reverts to the baseline.
At this point, the ΔT signal reaches the peak, as shown in graph (b).
From this, we can detect the samples transition temperature and the reaction temperature from
the ΔT signal (DTA signal).

Applications of DTA
1. DTA curves for two substances are not identical. Hence they serve as finger prints for
various substances. 2. Used to study the characteristic of polymeric material. 3. This
technique is used for testing the purity of the drug sample and also to test the quality
control of number of substances like cement, soil, glass,etc. 4. Used for the determination
of heat of reaction, specific heat and energy change occurring during melting etc. 5. Trend
in ligand stability (thermal stability of the ligands) gives the information about the ligands
in the coordination sphere.
3. Differential Scanning Calorimetry (DSC)
It is a powerful and most employed thermal analysis technique. It is widely used in
materials science, chemistry, pharmaceuticals, and various other scientific and industrial
fields.

Principles of Differential Scanning Calorimetry

Differential Scanning Calorimetry measures the heat flow into or out of a sample as a
function of temperature or time. The basic setup consists of a sample cell and a reference
cell, both housed in a temperature-controlled environment.
As the temperature is varied, the heat absorbed or released by the sample is compared to
that of the reference. This allows for the detection of phase transitions, chemical reactions,
and other thermal events.

Applications of Differential Scanning Calorimetry

DSC finds numerous applications in various scientific and industrial fields. In materials
science, it is widely used to study phase transitions, such as melting, crystallisation, glass
transitions, and polymorphic transformations.
DSC can provide valuable information about the thermal stability, purity, and composition
of materials.
Differential Scanning Calorimetry is also a valuable tool in pharmaceutical research and
development. It helps characterise drug formulations, analyse drug-polymer interactions,
and determine the stability of pharmaceutical products.

In the field of polymers and plastics, DSC allows for the investigation of thermal properties,
including glass transition temperature, curing kinetics, and thermal stability.
This information aids in the development of new materials, optimization of processing
conditions, and assessment of product performance.
DSC can be applied to analyse food products as well. It can determine parameters like the
enthalpy of freezing or crystallisation, as well as detect adulteration or changes in food
composition due to storage conditions or processing methods.
Differential Scanning Calorimetry is a versatile and powerful technique used for thermal
analysis in a wide range of fields. Its ability to measure heat flow and detect thermal
events makes it invaluable for understanding material behaviour, identifying phase
transitions, and assessing thermal stability.

By harnessing the power of DSC, we gain deeper insights into the thermal behaviour of
materials, leading to advancements in industries worldwide.