Vous êtes sur la page 1sur 3

Differential Thermal Analyzers

Thermal Analysis Techniques


Thermal analysis comprises a group of techniques in which a physical property of a
substance is measured as a function of temperature, while the substance is subjected to a
controlled temperature programme. 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.

Types of Thermal Analysis


1. Thermogravimetric (TG) analysis – Mass
2. Differential Thermal Analysis (DTA) – Temperature difference
3. Differential Scanning Calorimetry (DSC) – Heat difference

Differential Thermal Analyzer


A differential thermal analyzer, also commonly referred to as a DTA analyzer, is used in
analytical chemistry to identify and quantitatively analyze the chemical compositions of a sample
by heating the sample and recording the behavior of the sample, which includes the temperature
and heat flow between phase transition (i.e. melting point, crystallization, etc.). As a sample will
undergo reactions and phase changes as it is heated. This results in the absorption or emission of
heat. These exothermic or endothermic changes in the sample can be detected relative to a
reference. Differential thermal analyzers are widely used for metallurgy, semiconductors,
pharmaceuticals, food testing, cement chemistry, and environmental research.

Principle
Differential thermal analysis (DTA) involves the technique of recording the difference in
temperature between a substance and a reference material against either time or temperature.
Thus, a differential thermogram consists of a record of the differences in sample and reference
temperature (differential temperature, ΔT) plotted as a function of time t, sample temperature
(Ts), reference temperature (Tr) or furnace temperature (Tf). Substance and reference material
are subjected to controlled temperature.
a. Emissions of heat (exothermic).
b. Absorptions of heat (endothermic)
Sharp endothermic peaks give ideas of changes in crystallinity or fusion processes whereas broad
endosperms signify dehydration reactions. Physical changes give rise to endothermic curves
whereas chemical reactions (particularly those of an oxidative nature) give rise to exothermic
peaks. DTA allows the detection of every physical or chemical change whether or not it is
accompanied by a change in weight.

Factors affecting the DTA curve


a. Environmental factors.
b. Instrumental factors.
c. Sample factors.

Phenomena causing changes in heat / temperature


*Physical - Adsorption (exothermic), Desorption (endothermic), A change in crystal structure
(endo/exothermic), Crystallization (exothermic), Melting (endothermic), Vaporization
(endothermic) Sublimation (endothermic)
*Chemical - Oxidation (exothermic) ,Reduction (endothermic), Break down reactions (endo/
exothermic), Chemisorption (exothermic), Solid state reactions (endo/ exothermic)

Advantages:
1. Instruments can be used at very high temperatures.
2. Instruments are highly sensitive.
3. Characteristic transitions or reaction temperatures can be accurately determined.

Disadvantages:
1. Uncertainty of heats of fusion, transition or reaction estimations is 20-50%

Application
The DTA allows the detection of any change of temperatures of a sample due to the chemical
modifications of various categories of materials under controlled atmospheres for various
applications:
1. Characterisation of polymers (determination of their decomposition temperature);
2. Determination of the chemical change of inorganic materials (silicates, ferrites, oxides,
ceramics, catalysts, glasses, etc)
3. Construction of phase diagram

References:
1. Encyclopaedia Britannica
https://www.britannica.com/science/differential-thermal-analysis
2. Differential Thermal Analysis
Mr. Shaise Jacob
Department of Pharmaceutical Analysis
Nirmala College of Pharmacy
Muvattupuzha, Kerala, India
3. http://www.groupes.polymtl.ca/lanomat/modules/facilities/index.php?content_id=15

Vous aimerez peut-être aussi