Analysis Through Thermal Energy

King Abdul-Aziz University
Faculty of Science
Department of Chemistry
Analysis Through Thermal Energy

Outline 1
TGA and TMA DSC and DTA

Introduction
Ø Introduction Ø Definition of DTA

Ø Thermal analysis Ø TG curve Ø Description of DTA
Ø Classification of thermal Ø Definition of DSC
techniques Ø Factors affecting TG
Ø Description of DSC
Ø Measuring methods for Ø Applications of TGA Ø Applications of DTA and DSC
thermal analysis of physical Ø Applications of DSC of liquid
Ø TMA curve
properties crystal.
Ø Applications of TMA
2
INTRODUCTION }
3
Thermal analysis
A group of techniques in which a property of the sample is monitored

against time or temperature while the temperature of the sample, in a
specified atmosphere, is programmed.
Fig: Block diagram of Thermal Analysis instrument

4
Classification of thermal techniques
Fig(2):Classification of thermal techniques

5
Measuring methods for thermal analysis of physical properties
Several measuring methods are available. The method used varies according to the physical
properties being analyzed. The most commonly used ones are as follows:
Physical Types of Obtainable Information Measuring Units

Properties Methods
Calorie Transition Temperature, Heat Capacity Transferred, Specific DSC mW(=J/s)

Heat Capacity, Reaction Temperature, Reaction Calorie,
Examination of Thermal History etc.
Temperature Transition Temperature, Reaction Temperature etc DTA μV
Mass Dehydration, Oxidation, Pyrolysis, Evaporation, Sublimation TGA mg

etc.
Dimension Thermal Expansion, Thermal Shrinkage, Glass Transition TMA μm

Temperature, Softening Temperature etc
6
Thermogravimetric Analysis (TGA) }

7
Thermogravimetric Analysis
In this technique the change in sample weight is measured while the sample is heated at a
constant rate (or at constant temperature), under air (oxidative) or nitrogen (inert)
atmosphere.
What are the types of Thermogravimetric Analysis?
The three types of thermographic analysis represent different ways to apply heat to the sample,
as weight change is measured over time.
q Isothermal or static thermogravimetry: Temperature is constant

q Dynamic thermogravimetry: Temperature is changed in a linear manner
q Quasi Static thermogravimetry: A series of increasing temperatures
8
Thermogravimetric curve
The thermogram is plot of change in weight verses temperature or
time.
TG curve has following features

q Horizontal portion AA1 indicates the region
where there is no change in weight.
q ii) The curve A1B1 indicates the weight loss.
q Additional imformation that can be obtained
from a TG curve is that how much weight is lost
by heating a sample at a given temp.
Fig (3): Thermogravimetric curve
9
Thermogravimetric curve
Fig (4):Typical Thermgram for a polymer Fig (5):TG curve for decomposition of hydrated calcium
oxalate and magnesium oxalate
Factors affecting Thermogravimetry 10
Factors affecting
Thermogravimetry
Characteristics of the Instrumental factors

sample
Heating rate Furnace

atmosphere Sample holder
Weight of the Particle size of Heat of reaction
sample the sample
11
Applications of TGA
Generally, the important applications of TGA can be summarized as following:
q Automatic gravimetric analysis

q Thermal stability of materials
q Determination of composition of complex mixtures
q Determination of suitable ignition temperature
q Testing of sample purity
q Evaluation of suitable standard
12
Thermomechanical Analysis (TMA) }

13
Thermomechanical Analysis
q Thermomechanical Analysis (TMA) is the study of the relationships between

the sample’s length (or volume) and its temperature under constant load.
q Measurements can be carried out in the penetration mode, the dilatometry mode,
or the Dynamic Load TMA (DLTMA) mode.
14
Dilatometry
Dilatometry involves the measurement of the expansion or shrinkage of a sample.
Fig (6):TMA measurement of PET in the dilatometry mode

15
Penetration
During the penetration measurements, information related to temperatures are
mainly obtained.
Fig (7): MA of PET measured in the penetration mode

16
Dynamic Load TMA
Dynamic Load TMA (DLTMA) is a highly sensitive technique for determining physical properties.
Contrary to DSC, it involves characterizing the mechanical behavior of samples.
Fig (8): DLTMA measurement of PET from room temperature to 160 °C.
17
Applications of TMA
Generally, the important applications of TMA can be summarized as following:
q Determine coefficient of thermal expansion (CTE ) of material.

q Identify Tg & Tm of material.
q Measure material’s heat deflection temperature (HDT).
q Composite delamination temperature.
18
}
Differential Thermal Analysis (DTA)
19
What is the Differential Thermal Analysis (DTA)?
It is the technique that measures the temperature difference between a sample and a
reference material as a function of temperature as they are heated or cooled or kept at a
constant temperature (isothermal).
Fig(9): Instrument High temperature DTA

20
Description of DTA
q Sample and reference material are simultaneously

heated or cooled at a constant rate.
q Reaction or transition temperatures are then

measured as a function of the temperature
difference between the sample and reference.
q DTA provides vital information of the materials

regarding their endothermic and exothermic
behaviour at high temperatures.
Fig (10):Block diagram of DTA

21
Differential Scanning Caloriemeter (DSC):) }

22
What is the Differential Scanning Caloriemeter (DSC)?
Differential Scanning Caloriemeter (DSC) measures the amount of heat absorbed or released by a
sample as it is heated or cooled or kept at constant temperature (isothermal).
Fig(11): Instrument of DSC

23
Description of DSC
q The sample and reference material are

simultaneously heated or cooled at a constant rate.
q The difference in temperature between them is

proportional to the difference in heat flow between
the two materials.
Fig (12):Block diagram of Heat Flux DSC

24
Applications of DTA and DSC
Generally, the important applications of DTA and DSC as following:
q DTA provides vital information of the materials endothermic and exothermic

behaviour
q DTA are analysing and characterising clay materials, ceramic, ores, etc.
q DSC applied to most of the polymers in the curing process of the thermoset materials.
q DSC is determining the heat of melting and melting point of thermoplastic polymers,
glass transition temperature (Tg.).
25
Applications of DSC of liquid crystals.
It is the well-suited technique in the detection and further studies of liquid crystals materials.
Fig (13) DSC profile of liquid crystal materials at 5 K/min scan rate.
26
References
u INSTRUMENTAL CHEMICAL ANALYSIS, BASIC PRINCIPLES AND

TECHNIQUES.
u https://www.linseis.com/en/products/differential-thermal-analyzer-dta/
u https://www.hitachi-
hightech.com/global/products/science/tech/ana/thermal/descriptions/dta.html
u https://drive.uqu.edu.sa/_/jas/files/7-1/C-
%D8%A8%D8%AD%D8%AB%20%D8%AF_%20%D8%B3%D8%A7%D8%B1%D8
%A9%20%D8%A7%D9%84%D9%87%D9%88%D8%B3%D8%A7%D9%88%D9%8A-
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King Abdul-Aziz University

Analysis Through Thermal Energy

TGA and TMA DSC and DTA

Ø Introduction Ø Definition of DTA

A group of techniques in which a property of the sample is monitored

Fig: Block diagram of Thermal Analysis instrument

Fig(2):Classification of thermal techniques

Physical Types of Obtainable Information Measuring Units

Calorie Transition Temperature, Heat Capacity Transferred, Specific DSC mW(=J/s)

Mass Dehydration, Oxidation, Pyrolysis, Evaporation, Sublimation TGA mg

Dimension Thermal Expansion, Thermal Shrinkage, Glass Transition TMA μm

Thermogravimetric Analysis (TGA) }

q Isothermal or static thermogravimetry: Temperature is constant

TG curve has following features

Characteristics of the Instrumental factors

Heating rate Furnace

Generally, the important applications of TGA can be summarized as following:

q Automatic gravimetric analysis

Thermomechanical Analysis (TMA) }

q Thermomechanical Analysis (TMA) is the study of the relationships between

Fig (6):TMA measurement of PET in the dilatometry mode

Fig (7): MA of PET measured in the penetration mode

Generally, the important applications of TMA can be summarized as following:

q Determine coefficient of thermal expansion (CTE ) of material.

What is the Differential Thermal Analysis (DTA)?

Fig(9): Instrument High temperature DTA

q Sample and reference material are simultaneously

q Reaction or transition temperatures are then

q DTA provides vital information of the materials

Fig (10):Block diagram of DTA

Differential Scanning Caloriemeter (DSC):) }

Fig(11): Instrument of DSC

q The sample and reference material are

q The difference in temperature between them is

Fig (12):Block diagram of Heat Flux DSC

Applications of DTA and DSC

Generally, the important applications of DTA and DSC as following:

q DTA provides vital information of the materials endothermic and exothermic

u INSTRUMENTAL CHEMICAL ANALYSIS, BASIC PRINCIPLES AND

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