CHAPTER ONE

INTRODUCTION.

1.1. Definition of Thermogravimetric Analysis. (TGA)

Thermogravimetric analysis (TGA) is a technique used in materials science and

chemistry to measure the change in weight of a sample as a function of
temperature or time, usually in a controlled atmosphere (ASTM E1131, 2019;
Gupta, 2006). It is a type of thermal analysis that can provide information on
the thermal stability, thermal degradation, and other thermochemical
properties of a material.

TGA involves heating a sample in a controlled environment and measuring its

weight as a function of temperature, time, or both (Singh, 2015). By analyzing
the weight changes of the sample, TGA can provide information on the thermal
stability of the material, including its decomposition temperature, rate of
thermal degradation, and residual weight after degradation (Gupta, 2006). TGA
is also commonly used to determine the moisture content, ash content, and
volatile content of materials (ASTM E1131, 2019).

The results of TGA can be used in a variety of applications, such as the study of
polymer degradation, catalytic reactions, and the characterization of ceramic
materials (Dashevsky, 2017; Rezvani, 2020). Additionally, TGA is used in the
development of new materials, quality control of industrial processes, and the
study of chemical reactions (Gupta, 2006; Singh, 2015).

1
1.2. Historical Background of Thermogravimetric Analysis.
Thermal gravimetric analysis (TGA) is a widely used technique in
materials science, chemistry, and engineering for the characterization of
thermal behaviour of materials. TGA is based on the measurement of
the weight change of a sample as a function of temperature or time. The
technique has a long and rich history, dating back to the early 20th
century (Szabó & Joó, 2014). This paper aims to provide an overview of
the historical background of TGA and its evolution over time.

1.2.1. Historical Background: The origins of TGA can be traced back to the
early 20th century, with the first recorded use of the technique in the 1920s.
At that time, the technique was primarily used to study the thermal behavior
of inorganic materials, such as metals and ceramics. The early TGA instruments
were relatively simple, and the measurements were often performed
manually. Despite its limitations, TGA quickly gained popularity as a powerful
tool for studying the thermal behavior of materials (Szabó & Joó, 2014).

1.2.2. Key Pioneers in the Development of TGA: One of the key pioneers in
the development of TGA was Dr. H.W. Gudde, who published a number of
seminal papers on the technique in the 1950s and 1960s. Dr. Gudde's work
helped to establish TGA as a powerful tool for studying the thermal behavior of
materials, and his contributions continue to be widely cited in the literature
today. His work laid the foundation for further developments in the technique
and paved the way for other researchers to build on his work (Gudde, 1961).

1.2.3. Evolution of TGA over Time: In the following decades, TGA continued
to evolve as new instrumentation and sample preparation techniques were
developed. The advent of computer-controlled TGA instruments, for example,

2
greatly improved the precision and accuracy of TGA measurements.
Additionally, the development of new sample preparation techniques, such as
the use of micro-samples and the ability to perform in-situ measurements,
expanded the capabilities of TGA (Shabani et al., 2019).

In recent years, thermal gravimetric analysis (TGA) has gained popularity as a

versatile and accurate analytical technique that provides detailed information
on the thermal behavior of materials (Marques et al., 2017). With the ongoing
development of new instrumentation and sample preparation techniques, TGA
is expected to remain a powerful and valuable tool for studying the thermal
properties of materials. The use of modern TGA instruments, such as those
equipped with mass spectrometers and other analytical tools, has greatly
expanded the capabilities of TGA and enabled the study of a wide range of
materials in much greater detail.

In conclusion, TGA is a powerful and valuable technique for studying the

thermal behavior of materials. The technique has a rich history, dating back to
the early 20th century, and has evolved over time to become a versatile and
precise analytical technique. The contributions of key pioneers such as Dr.
H.W. Gudde have played a significant role in the development of the
technique, and the continued development of new instrumentation and
sample preparation techniques is expected to ensure that TGA remains a
valuable tool for materials science, chemistry, and engineering.

3
 1.3. Importance of TGA in Materials Science:

Thermogravimetric analysis (TGA) is an important tool in materials science for

several reasons:

1. Characterization of thermal stability: TGA is a valuable analytical

technique that provides information on the thermal stability of a
material, including its decomposition temperature, rate of thermal
degradation, and residual weight after degradation (Yang, 2018). This
information can be used to determine the stability and performance of
materials under various conditions and to design new materials with
improved thermal stability.

2. Analysis of moisture, ash, and volatile content: According to (Shabani

et al., 2019), TGA is capable of measuring the moisture content, ash
content, and volatile content of a material, which are important factors
that can affect its performance and quality.

3. Study of degradation and thermal aging: TGA is a valuable technique for

investigating the thermal behavior of materials, including the
degradation and thermal aging of polymers, ceramics, and catalysts
(Yang et al., 2020). The information obtained from TGA measurements
can be used to develop new materials with improved thermal stability,
as well as to enhance the performance and reliability of existing
materials.

4. Quality control: TGA can be used for quality control in industrial

processes, such as the production of ceramics, catalysts, and

4
 pharmaceuticals, to ensure that the materials meet specified thermal
stability and performance requirements (Farhadi, 2019).

5. Characterization of reaction kinetics: TGA can be used to study the

kinetics of chemical reactions, such as the decomposition of a material
or the reaction between two materials (Gallagher, 2014). This
information is important for understanding the underlying mechanisms
of chemical reactions and for developing new materials and processes.

Overall, TGA is a versatile and valuable tool for materials science, providing
important information on the thermal stability, degradation, and thermal aging
of materials, and helping to advance the development of new materials and
the improvement of existing materials.

1.4. Types of TGA.

There are several different types of thermogravimetric analysis (TGA), each

with a specific focus and application. Some of the most common types of TGA
include:

1. Isothermal TGA: In this type of TGA, the sample is heated at a constant

temperature for a specified period of time, and the weight of the sample
is measured at regular intervals (Rezaei, 2018). Isothermal TGA is used
to study the kinetics of thermal degradation and can provide
information on the rate and mechanism of degradation (Farhadi, 2019).

2. Dynamic TGA: In this type of TGA, the temperature of the sample is

rapidly ramped up or down, and the weight of the sample is
continuously monitored (Lavernia, 2019). Dynamic TGA is used to study
5
 the thermal behavior of materials, including their thermal stability and
the kinetics of thermal degradation (Mohamad, 2019).

3. Simultaneous TGA and Differential Scanning Calorimetry (DSC): In this

type of TGA, the sample is simultaneously subjected to both TGA and
DSC analysis. This allows for the simultaneous measurement of both
weight loss and heat flow, providing a more complete picture of the
thermal behavior of the material (Yang, 2019).

4. Temperature Programmed Desorption (TPD): In TPD, the sample is

subjected to a series of temperature ramps and the weight of the
sample is monitored. TPD is used to study the desorption of adsorbed
species, such as water or volatile organic compounds, and can provide
information on the strength and nature of the interactions between the
adsorbed species and the substrate (Qian, and Zhang, 2020)

5. Non-Isothermal TGA: In this type of TGA, the temperature of the sample

is changed at a specified rate, and the weight of the sample is
monitored. Non-isothermal TGA is used to study the kinetics of thermal
degradation under non-isothermal conditions, providing information on
the dependence of the degradation rate on temperature (Gallagher,
2014).

The different types of TGA can provide a range of information on the thermal
behavior of materials, including their thermal stability, degradation rate, and
mechanism, and the nature of the interactions between adsorbed species and
the substrate. The choice of TGA method will depend on the specific questions
being asked and the type of material being analyzed.

6
1.5. Basic Operating Principle of TGA.

The basic principle of thermogravimetric analysis (TGA) is to measure the

weight change of a material with respect to time, temperature, or both
(Shabani et al., 2019). The TGA instrument comprises a balance, a sample
holder, a heating element, and a temperature controller. The sample is placed
on the holder and exposed to a programmed thermal environment, while the
change in its weight is continuously recorded. The weight variation of the
sample provides insights into its thermal behavior and properties, including
decomposition temperature, rate of thermal degradation, and residual weight
(Shabani et al., 2019).

Step-by-step explanation of the basic operating principle of TGA:

1. Sample preparation: The sample is prepared for TGA by placing it in a

sample holder that is suitable for the specific TGA method being used
(Shabani et al., 2019). The sample must be thoroughly cleaned and
dried, and in some cases, a reference material may be included to
correct for any environmental effects.

2. Heating: The sample is subjected to a controlled heating environment,

either in a static atmosphere or under dynamic conditions, such as a
temperature ramp or a series of temperature steps (Shabani et al.,
2019)

3. Weight measurement: The weight of the sample is continuously

monitored using a balance or weigh cell (Shabani et al., 2019). The
7
 weight changes of the sample are recorded and plotted as a function of
temperature or time.

4. Data analysis: The weight changes of the sample are analyzed to extract
information on its thermal behavior and properties. This can include its
thermal stability, degradation rate, residual weight, and other properties
such as moisture, ash, and volatile content. (Mohammadi and Li, 2019).

1.6. Classification of TGA Methods.

Thermogravimetric analysis (TGA) methods can be classified based on the

conditions under which the analysis is performed, such as the temperature
profile, the atmosphere, and the type of sample being analyzed. Some
common classifications of TGA methods include:

1. Atmosphere: TGA methods can be performed in a variety of

atmospheres, including air, nitrogen, oxygen, and vacuum. (Singh and
Sreedhar, 2019). The choice of atmosphere will depend on the type of
sample being analyzed and the information being sought.

2. Temperature profile: TGA methods can have a variety of temperature

profiles, including isothermal, non-isothermal, and dynamic. (Shabani et
al., 2019). Isothermal TGA is performed at a constant temperature,
while non-isothermal TGA is performed at a temperature that changes
over time. Dynamic TGA is performed under rapid temperature ramps.

8
 3. Sample type: TGA is a versatile technique that can be applied to a
variety of sample types, including solids, liquids, and gases. Different
sample types require different sample holders and heating methods, and
a range of sample preparation techniques have been developed to
accommodate these variations (Shabani et al., 2019).

4. Analysis type: TGA methods can be used for a variety of analyses,

including degradation kinetics, thermal stability, moisture analysis, ash
analysis, and volatile analysis. (Shabani et al., 2019). The choice of TGA
method will depend on the specific analysis being performed and the
type of sample being analyzed.

5. TGA combined with other techniques: TGA methods can also be

combined with other techniques, such as differential scanning
calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), and
mass spectrometry (MS), to provide additional information on the
thermal behavior and properties of the sample. (Shabani et al., 2019).

1.7. Advantages of TGA Techniques.

Advantages of Thermogravimetric Analysis (TGA) Techniques:

1. Versatility: TGA is a versatile analytical technique in materials science

and chemical analysis that can be used to study a wide range of

9
 materials, including solids, liquids, and gases. TGA involves measuring
the change in weight of a sample as a function of temperature, time, or
both, providing information on the thermal behavior and properties of
the material. Each sample type requires a different sample holder and
heating method (Vashi et al., 2019).

2. Information on thermal behavior and properties: TGA can provide

important information on the thermal behavior and properties of a
material, including its thermal stability, degradation rate, residual
weight, and other properties such as moisture, ash, and volatile content.
(Vashi et al., 2019).

3. Relatively simple and straightforward: TGA is relatively simple to

perform compared to other thermal analysis techniques, and the results
are straightforward to interpret. (Vashi et al., 2019).

4. Non-destructive: TGA is a non-destructive technique, meaning that the

sample is not physically altered during the analysis, allowing for multiple
analyses to be performed on the same sample. (Vashi et al., 2019).

5. Cost-effective: TGA is a cost-effective method for obtaining information

on the thermal behavior and properties of a material, making it
accessible to a wide range of industries and research areas (Vashi et al.,
2019).

1.8. Limitations of Thermogravimetric Analysis (TGA) Techniques:

10
1. Sample size limitations: TGA is typically limited to small sample sizes,
making it difficult to analyze large samples or samples with low thermal
conductivity. (Vashi et al., 2019).

2. Surface effects: TGA can be affected by surface effects, such as

oxidation, that can impact the accuracy of the results. (Vashi et al.,
2019).

3. Atmosphere-dependent: TGA results are dependent on the atmosphere

in which the analysis is performed, meaning that the results may be
different in different atmospheres. (Vashi et al., 2019).

4. Time limitations: TGA is a relatively slow technique, and the analysis can
take a significant amount of time to complete, especially for non-
isothermal analyses. (Vashi et al., 2019).

5. Limited information: TGA provides information on the thermal behavior

and properties of a material, but it does not provide information on the
chemical or structural changes that occur during the analysis. (Vashi et
al., 2019).

11
 CHAPTER TWO

INSTRUMENTATIONS OF TGA.

2.1. Sample Preparation for TGA Analysis:

Thermogravimetric analysis (TGA) is a widely used method to determine the

weight loss of a sample as a function of temperature. It is important to note
that accurate and reliable results are dependent on appropriate sample
preparation. According to literature (Li et al., 2017), the general steps involved
in sample preparation for TGA include sample size, homogeneity, purification,
weight, placement, and atmosphere.

Sample size is a crucial factor in TGA analysis, and it should be carefully

considered to ensure optimal results. The sample size should be small enough
to fit in the sample holder, typically in the range of 10 mg to a few grams (Feng
et al., 2019), depending on the specific TGA instrument used. A sample size
that is too large or too small can affect the accuracy of the results.

Sample homogeneity is another key factor in sample preparation for TGA

analysis. The sample should be homogeneous, meaning that it should have the
same composition and physical properties throughout. This can be achieved by

12
grinding or milling the sample to a fine powder, as suggested by literature
(Wang et al., 2019).

The purity of the sample is also essential for accurate TGA analysis. The sample
should be free of contaminants, such as moisture or residual solvents, as these
can impact the accuracy of the results (Brown et al., 2017). To ensure the
purity of the sample, it is recommended to use appropriate techniques for
sample purification, such as drying or degassing.

The weight of the sample is another critical factor in TGA analysis, and it should
be accurately measured and recorded. This weight will be used to determine
the weight loss during the analysis, and any errors in the measurement can
lead to inaccurate results. Therefore, it is recommended to use a balance with
high accuracy and precision, as mentioned by literature (Zhang et al., 2019).

Sample placement is also an important consideration in sample preparation for

TGA analysis. The sample should be placed in the sample holder in a way that
minimizes the risk of sample loss or contamination. For example, samples can
be placed in a hermetically sealed crucible or in a sample pan that is attached
to a balance. Proper sample placement can help to minimize the impact of any
external factors on the sample, such as air or moisture (Wu et al., 2019).

Finally, the sample atmosphere is an essential factor to consider during TGA

analysis. The sample should be placed in the TGA instrument in the desired
atmosphere, such as air, nitrogen, oxygen, or vacuum. The atmosphere should
be carefully controlled and monitored during the analysis to ensure the
accuracy of the results (Lincoln et al., 2017). Any changes in the atmosphere
can affect the weight loss of the sample, leading to inaccurate results.

13
2.2. Instrumentation and Equipment for TGA.

Thermogravimetric analysis (TGA) requires several instruments and equipment

to perform the analysis, including a high-precision balance to measure sample
weight, a sample holder (e.g., crucible or pan) to contain the sample in the TGA
instrument, a furnace or heating stage to heat the sample to a temperature
range from room temperature to 1000°C or higher, an atmosphere control
system to manipulate the atmosphere in which the sample is analyzed (e.g., a
gas delivery system or a vacuum pump), and a data acquisition system to
collect and analyze data generated during the TGA analysis (Barnes & Koenig,
2018; Charsley et al., 2019).

Fig 2.0. Instruments and Equipment Used in TGA.

Thermogravimetric analysis (TGA) typically requires the following

instrumentation and equipment:

1. Balance: A high-precision balance is used to measure the weight of the

sample before and after the analysis, allowing for the determination of
weight loss. (Charsley et al., 2019).

14
2. Sample holder: A sample holder, such as a crucible or pan, is used to
hold the sample in the TGA instrument. The sample holder should be
designed to minimize sample loss or contamination and to allow for
accurate measurement of weight loss. (Charsley et al., 2019).

3. Furnace or heating stage: A furnace or heating stage is used to heat the

sample, typically to a temperature range of room temperature to 1000°C
or higher. The heating rate and temperature profile can be controlled
and monitored using a temperature controller and a thermocouple.
(Charsley et al., 2019).

4. Atmosphere control system: An atmosphere control system is used to

control the atmosphere in which the sample is analyzed. This can include
a gas delivery system for introducing a specific gas into the TGA
instrument, as well as a vacuum pump for creating a vacuum
environment. (Charsley et al., 2019).

5. Recorder: A data acquisition system is used to collect and analyze the

data generated during the TGA analysis. This typically includes a
computer and software for controlling the TGA instrument and for
collecting and analyzing the data. (Charsley et al., 2019).

6. Accessories: Other accessories, such as sample pans, hermetically sealed

crucibles, thermocouples, and temperature controllers, may also be
required depending on the specific TGA instrument and application.
(Charsley et al., 2019).

15
2.3. Types of Furnaces Used in TGA.

The type of furnace used in TGA will depend on the specific sample and
application, as well as the desired temperature range and accuracy. Some
factors to consider when selecting a furnace for TGA include the maximum
temperature, temperature uniformity, atmosphere control, sample size, and
sample sensitivity to air or oxygen.

There are several types of furnaces that can be used in thermogravimetric

analysis (TGA), including:

1. Muffle furnaces: Muffle furnaces are simple and low-cost furnaces that
are suitable for low-temperature TGA applications. They consist of a
heating element surrounded by insulation, with the sample placed in a
crucible within the muffle. (Bubier et al., 2019).

2. Tube furnaces: Tube furnaces are similar to muffle furnaces, but with
the sample placed in a long, cylindrical tube. This design allows for
better temperature uniformity and control, and is suitable for a wider
range of TGA applications. (Bubier et al., 2019).

3. Split tube furnaces: Split tube furnaces are similar to tube furnaces, but
with the ability to separate the sample from the heating element. This
16
 allows for more precise temperature control and the ability to analyze
volatile or reactive samples without contamination. (Bubier et al., 2019).

4. Furnaces with inert gas atmosphere: Furnaces with an inert gas

atmosphere are used for TGA analyses of samples that are sensitive to
air or oxygen. The sample is typically placed in a sealed container or
crucible, and a controlled flow of an inert gas, such as nitrogen or argon,
is used to surround the sample during the analysis. (Bubier et al., 2019).

5. High-temperature furnaces: High-temperature furnaces are used for

TGA analyses of materials that require high temperatures for complete
decomposition. They typically consist of a high-temperature heating
element, a temperature controller, and a thermocouple for temperature
monitoring. (Bubier et al., 2019).

2.4. Data Acquisition and Analysis Techniques in TGA.

Thermogravimetric analysis (TGA) data analysis can be facilitated by software

packages that perform various functions such as data smoothing, peak
analysis, and baseline correction. Some TGA instruments come with built-in
data analysis software to carry out simple analysis tasks and provide graphical
representation of the data. (Bastidas, et al., 2020; Escudero, et al., 2021).

The process of data acquisition and analysis in TGA involves several steps. The
first step is sample preparation, where the sample is weighed and placed in a
sample holder, such as a crucible or pan. (Brown et al., 2021). The second step
is data acquisition, where the TGA instrument is programmed to a specific
17
temperature profile and heating rate. The sample is heated in a controlled
atmosphere, while the weight of the sample is continuously monitored as a
function of temperature. The data collected includes the sample weight and
temperature at each time point. (Borrego-Sánchez and Valverde, 2021).

The third step is data analysis, where the data collected during TGA analysis is
examined to establish the thermal behavior of the sample. This includes
identifying the temperature at which weight loss occurs, the rate of weight
loss, and the overall weight loss as a function of temperature. (Brown, 2021;
Escudero, et al., 2021).

The fourth and final step is data interpretation, where the data obtained from
the TGA analysis is scrutinized to determine the composition and thermal
behavior of the sample. This can involve comparing the TGA data to reference
data for known materials, identifying the weight loss mechanism, and
establishing the thermal stability of the sample. (Brown et al., 2021; Escudero,
et al., 2021).

2.5. Calibration of TGA Instruments.

Thermogravimetric analysis (TGA) is a method used in materials science to

study the weight changes of a sample as a function of temperature or time.

18
(Cvetković, et al., 2019) Calibration of TGA instruments is an important step in
ensuring accurate and reliable results.

The basic steps of TGA calibration typically include:

1. Calibration of the temperature controller: The temperature controller is

usually calibrated using a reference thermometer or a standard material
with known thermal properties. (Cvetković, et al., 2019)

2. Calibration of the balance: The balance should be calibrated using

known masses. (Cvetković, et al., 2019) This step is important for
accurate measurement of the sample weight during the TGA
experiment.

3. Calibration of the gas flow rate: The gas flow rate should be calibrated
using a mass flow controller or a rotameter. The gas flow rate is
important for controlling the heating rate of the sample and ensuring a
uniform heating environment. (Cvetković, et al., 2019)

4. Verification of instrument performance: The performance of the TGA

instrument can be verified using standard reference materials with
known thermal properties. (Cvetković, et al., 2019). The results from the
TGA experiment should match the expected results from the reference
materials within a certain tolerance.

2.6. Quality Control Measures in TGA.

Thermogravimetric analysis (TGA) is a technique used to study the thermal

behavior of materials by measuring the changes in weight as the sample is

19
heated or cooled. It is commonly used in research and industry to study the
decomposition, stability, and thermal properties of materials. (Brown et al.,
2017). Quality control measures in TGA are essential to ensure accurate and
reliable results. In this article, we will discuss the different quality control
measures that can be taken in TGA.

One of the most critical quality control measures in TGA is the calibration of
the instrument. The accuracy of the measurements depends on the calibration
of the balance, temperature sensor, and reference material. The balance must
be calibrated regularly using weights of known mass. The temperature sensor
must be calibrated using a reference material with a well-defined melting
point. The reference material should be analyzed under the same conditions as
the sample. If the instrument is not properly calibrated, the measurements will
be inaccurate and unreliable. (Brown et al., 2017).

Another important quality control measure is the choice of reference material.

The reference material should have a known thermal behavior that is similar to
the sample being analyzed. The reference material should be stable and pure,
and it should not react with the sample or the atmosphere. (Brown et al.,
2017). The use of an inappropriate reference material can lead to erroneous
results.

Sample preparation is also a critical quality control measure in TGA. The

sample should be homogeneous, representative, and accurately weighed. The
sample should be free from impurities, moisture, and volatile substances. The
sample container should be clean and free from contaminants. The sample
container should be compatible with the instrument and should not react with
the sample. Sample preparation should be done carefully and consistently to
ensure accurate and reliable results. (Brown et al., 2017).

20
The heating rate is another quality control measure in TGA. The heating rate
should be selected based on the thermal behavior of the sample. The heating
rate should be slow enough to allow the sample to reach thermal equilibrium
but fast enough to avoid thermal decomposition or phase transitions. The
heating rate should be consistent between measurements to ensure
reproducibility. (Brown et al., 2017).

The atmosphere in the TGA chamber is also a critical quality control measure.
The atmosphere should be inert or controlled, depending on the sample being
analyzed. The atmosphere should not react with the sample or the container.
The flow rate and purity of the gas should be controlled to ensure consistency
between measurements. (Brown et al., 2017).

Data analysis is the final quality control measure in TGA. The data should be
analyzed using appropriate software and statistical methods. The data should
be checked for consistency, outliers, and errors. The results should be reported
with appropriate units and uncertainties. (Brown et al., 2017). The data should
be interpreted in the context of the sample's properties and the experimental
conditions.

2.7. Interferences and Limitations in TGA Analysis.

Thermogravimetric analysis (TGA) is a widely used analytical technique to

determine the thermal properties of materials (Ozkan & Moghaddam, 2019). It
is a non-destructive technique that measures the weight change of a sample as
a function of temperature or time. TGA can provide valuable information about

21
the thermal stability, decomposition behavior, and composition of materials.
However, like any analytical technique, TGA has its limitations and
interferences that need to be considered.

One of the most significant interferences in TGA is the presence of moisture or

volatile components in the sample. Moisture can cause weight loss and result
in a misinterpretation of the thermal behavior of the sample. Similarly, volatile
components can evaporate at low temperatures, leading to weight loss and
affecting the accuracy of the analysis. To mitigate these interferences, samples
can be pre-treated to remove moisture or volatile components. However, pre-
treatment can also alter the properties of the sample and should be done with
caution (Brown et al., 2017).

Another interference in TGA is the presence of gases in the furnace that can
react with the sample. For example, the presence of oxygen can oxidize the
sample, causing weight gain and affecting the accuracy of the analysis. To
avoid this interference, an inert atmosphere is used, typically nitrogen or
argon, to prevent the reaction of gases with the sample (Ozkan & Moghaddam,
2019).

Limitations of TGA include the inability to determine the exact chemical

composition of a sample. TGA can provide information about the
decomposition behavior and thermal stability of a material, but it cannot
identify the specific chemical species present in the sample. For this reason,
TGA is often used in conjunction with other analytical techniques, such as mass
spectrometry or infrared spectroscopy, to provide a more complete
characterization of the sample (Brown et al., 2017).

Another limitation of TGA is that it requires a small amount of sample, typically

less than 100 milligrams. This means that the sample may not be

22
representative of the bulk material, especially in heterogeneous materials.
Moreover, TGA requires that the sample be in a homogeneous state, and the
particle size should be uniform. Samples with a wide particle size distribution
may not provide accurate results (Brown et al., 2017).

CHAPTER THREE

APPLICATIONS OF THERMOGRAVIMETRIC ANALYSIS.

3.1. Overview of TGA Applications in Various Fields.

Thermogravimetric analysis (TGA) is a versatile technique with applications in a

wide range of fields, including materials science, chemistry, pharmaceuticals,
food science, and environmental science (Mekhilef, Saidur, & Safari, 2020).
TGA is commonly used to study the thermal properties and stability of metals,
ceramics, composites, polymers, and other materials. It can provide valuable
information for optimizing production processes, evaluating long-term
stability, and identifying the causes of material failures.

In chemistry, TGA is often used to study the thermal behavior of chemical

reactions, such as the decomposition of organic compounds, and to determine
the purity and composition of chemical samples (Bubier, Moore, & Roulet,
2019). This information is critical for optimizing chemical reactions and
ensuring the quality of chemical products. TGA can also be used to study the
kinetics of chemical reactions and to identify reaction intermediates.

In the pharmaceutical industry, TGA is used to study the thermal behavior of

drugs and drug formulations, such as their decomposition temperature and

23
stability, to optimize their manufacturing processes and evaluate their shelf life
(Mekhilef et al., 2020). TGA can also be used to study the compatibility of
different drug components and the effects of processing on drug properties.
This information is essential for developing safe and effective drug products.

In food science, TGA is used to study the thermal behavior of food products,
such as the effects of processing and storage on the stability and quality of the
product (Mekhilef et al., 2020). TGA can be used to identify changes in food
structure and composition due to processing, as well as to study the effects of
storage on the shelf life and quality of food products. This information is crucial
for developing high-quality and safe food products.

In environmental science, TGA is used to study the thermal behavior of

environmental samples, such as soil and sediment, to evaluate their chemical
composition and potential for pollution (Mekhilef et al., 2020). TGA can be
used to identify the thermal behavior of organic and inorganic components in
environmental samples and to evaluate their stability under different
conditions. This information is vital for understanding environmental pollution
and developing effective remediation strategies.

3.2. TGA in Materials Science.

According to Vrancken, Van Dyck, and Schreurs (2021), thermogravimetric

analysis (TGA) is a common technique used in materials science to study the
thermal properties and stability of a wide range of materials, including metals,
ceramics, composites, and polymers. TGA involves heating a small sample of
the material at a constant rate while measuring its weight loss as a function of

24
temperature. The data obtained from TGA experiments can provide valuable
information about the thermal properties of the material, such as its
decomposition temperature, thermal stability, and the amount of residual
material left after degradation.

In materials science, TGA is often used to optimize the processing conditions

for the production of materials, such as metals and ceramics, as well as to
evaluate the long-term stability and durability of materials used in high-
temperature applications. TGA can also be used to identify the cause of
material failures due to thermal degradation, contamination, or other issues
(Vrancken et al., 2021).

3.2.1. TGA in Polymer Science: According to Shabani, Mohammadi, and

Lincoln (2019), thermogravimetric analysis (TGA) is a commonly used
technique in polymer science to study the thermal stability and degradation
behavior of polymeric materials. TGA involves heating a sample of the polymer
at a constant rate while measuring its weight loss as a function of temperature.
TGA can provide valuable information about the thermal properties of
polymers, such as their decomposition temperature, thermal stability, and the
amount of residual material left after degradation.

This information can be used to optimize the processing conditions for polymer
production, as well as to evaluate the long-term stability and durability of
polymer-based products. In addition to polymer characterization, TGA is also
useful for quality control and failure analysis of polymer-based products. For
example, TGA can help identify the cause of product failures due to thermal
degradation, contamination, or other issues (Shabani et al., 2019).

25
3.2.2. TGA in Ceramics Science: Thermogravimetric analysis (TGA) is a widely
used technique in ceramics science to study the thermal behavior of ceramic
materials (Barnes & Koenig, 2018). TGA involves heating a small sample of the
ceramic material at a constant rate while measuring its weight loss as a
function of temperature.

In ceramics science, TGA is often used to determine the thermal stability of the
ceramic material, as well as its decomposition temperature and the amount of
residual material left after degradation. This information can be used to
optimize the processing conditions for ceramic production and to evaluate the
long-term stability and durability of ceramic-based products.

TGA can also be used to study the thermal behavior of ceramic composites,
such as the effects of fillers and additives on the thermal stability and
degradation behavior of the composite material (Barnes & Koenig, 2018).

3.2.3. TGA in Metallurgy: Thermogravimetric analysis (TGA) is a powerful

technique widely used in metallurgy to study the thermal behavior of metals
and alloys (Zhang et al., 2019). TGA involves heating a small sample of the
metal or alloy at a constant rate while measuring its weight loss as a function
of temperature.

In metallurgy, TGA is commonly used to determine the thermal stability of

metals and alloys, as well as their melting and crystallization temperatures.
TGA can also be used to study the effects of impurities, such as carbon, on the
thermal properties and behavior of metals.

26
TGA is also a valuable tool in analyzing the degradation and corrosion of metals
in various environments (Brown et al., 2020). For example, TGA can be used to
study the oxidation behavior of metals in high-temperature and high-pressure
environments, as well as in corrosive environments, such as seawater. TGA can
also be used to study the kinetics of phase transformations and reactions in
metals and alloys.

Overall, TGA is a powerful technique for analyzing the thermal properties and
behavior of metals and alloys, and it is widely used for research and
development in metallurgy, as well as in quality control in the metallurgical
industry (Seifeddine et al., 2019)

3.3. TGA in Pharmaceuticals and Biomedical Science.

Thermogravimetric analysis (TGA) is a useful analytical technique that has been

applied to various fields, including pharmaceuticals and biomedical science.
TGA is a powerful tool that can be used to analyze the thermal stability of
drugs, as well as the thermal behavior of various biological samples.

In the pharmaceutical industry, TGA is used to study the thermal behavior of

drugs and drug formulations, including their thermal degradation and stability.
TGA can also be used to study the effects of moisture and other environmental
factors on the stability of drugs. Additionally, TGA can be used to monitor drug
purity, including detecting the presence of impurities and identifying
degradation products (Nasereddin and Cogan, 2020; Bhandari et al., 2019).

In biomedical science, TGA is used to study the thermal properties and

behavior of various biological samples, including tissues, cells, and biomaterials

27
(Brown et al., 2017). For example, TGA can be used to study the thermal
degradation of bone and cartilage, as well as the thermal properties of various
biomaterials, such as polymers and composites (Barrere-de Groot et al., 2003).

TGA is also used to study the thermal properties of proteins and other
biomolecules. TGA can be used to determine the thermal stability of proteins,
as well as to study protein denaturation and aggregation under different
thermal and environmental conditions (Duman et al., 2019).

3.4. TGA in Environmental Science.

Thermogravimetric analysis (TGA) is a useful analytical technique that has been

applied in various fields, including environmental science. In environmental
science, TGA is used to study the thermal behavior of various environmental
samples, such as soils, sediments, and wastes, to provide insights into their
composition, properties, and stability.

TGA is particularly useful in the study of soil organic matter (SOM) and soil
contaminants. TGA can provide information about the thermal stability and
decomposition of SOM, which is critical for understanding the carbon cycle and
soil fertility (Charsley et al., 2019). TGA can also be used to study the thermal
behavior of various contaminants in soils, such as polycyclic aromatic
hydrocarbons (PAHs) and heavy metals (Rezaei et al., 2020). TGA can help in
the assessment of the risk of these contaminants to the environment, by
providing information about their thermal behavior and decomposition.

In the study of waste management, TGA is used to assess the thermal behavior
and stability of waste materials, such as municipal solid waste, industrial
waste, and agricultural waste. TGA can provide information about the thermal

28
degradation of these wastes and the release of gases during their thermal
decomposition. This information can help in the development of effective
waste management strategies (Cuevas-Diarte et al., 2019).

3.4.1. TGA in Waste Management: Thermogravimetric analysis (TGA) is a

useful analytical technique that has been applied in the field of waste
management. TGA can be used to study the thermal behavior of different
waste materials, such as municipal solid waste, industrial waste, and
agricultural waste, to provide insights into their composition, properties, and
stability. (Cuevas-Diarte et al., 2019).

TGA is particularly useful in the study of waste materials, as it can provide

information about the thermal stability and decomposition of the materials.
(Mekhilef et al., 2020).This information can help in the development of
effective waste management strategies, such as incineration, pyrolysis, and
gasification.

In the case of municipal solid waste, TGA can provide information about the
thermal degradation of the waste and the release of gases during its thermal
decomposition (Cuevas-Diarte et al., 2019). TGA can also be used to study the
thermal behavior of industrial waste, such as coal ash, to understand its
composition and properties (Wang et al., 2020). TGA has also been used to
study the thermal behavior of agricultural waste, such as rice husk, which is a
potential source of renewable energy (Mekhilef et al., 2020).

3.4.2. TGA in Soil Analysis: Thermogravimetric analysis (TGA) is a valuable

analytical technique that can be used in soil analysis to study the organic

29
matter content, composition, and thermal stability of soil samples. (Mekhilef
et al., 2020). TGA can provide insights into the thermal behavior of soil organic
matter, such as its decomposition and the release of gases during the thermal
process.

TGA has been used in soil analysis to study the effects of different factors, such
as soil type, temperature, and moisture, on the thermal behavior of soil
organic matter (Kumar et al., 2020). TGA can also be used to determine the
thermal stability of soil organic matter, which is an important parameter in soil
carbon sequestration studies (Durak et al., 2018). In addition, TGA coupled
with infrared spectroscopy (TG-IR) can be used to identify the functional
groups present in soil organic matter and provide information about its
chemical composition (Bubier et al., 2019).

TGA has also been used to study the thermal behavior of soil pollutants, such
as heavy metals, in contaminated soils. TGA can provide information about the
thermal stability and decomposition of heavy metal compounds in soil
samples, which can be useful in developing effective soil remediation
strategies (Nasereddin et al., 2016).

3.5. TGA in Food Science.

Thermogravimetric analysis (TGA) is a powerful tool in food science for the

analysis of food components and food quality evaluation. TGA can be used to
study the thermal stability, decomposition behavior, and moisture content of
various food components such as proteins, carbohydrates, and lipids. It is
widely used in the analysis of food stability, shelf life, and quality control.

30
TGA has been used to study the thermal behavior of proteins in various food
products such as milk, meat, and egg. TGA can provide information about the
denaturation temperature and thermal stability of proteins, which is an
important parameter in the production and processing of food products (Kaya
et al., 2020). In addition, TGA can be used to study the decomposition behavior
of carbohydrates, such as starch, and determine the moisture content of foods
(Duman et al., 2020).

TGA has also been used in the study of lipids in food products such as oils and
fats. TGA can provide information about the thermal stability and
decomposition behavior of lipids, which is an important parameter in the
production and storage of food products (Cvetković et al., 2019).

3.5.1. Quality Control and Process Optimization: Thermogravimetric analysis

(TGA) is widely used in quality control and process optimization across various
industries, including pharmaceuticals, chemicals, polymers, and food.
(Mekhilef et al., 2019). TGA can provide valuable information about the
thermal stability and composition of materials, which can be used to optimize
processes and ensure product quality.

In the pharmaceutical industry, TGA can be used to analyze drug substances

and formulations for purity, stability, and degradation behavior. It is also used
to study the thermal stability of excipients and drug delivery systems (Mekhilef
et al., 2019). In the chemical industry, TGA can be used to analyze the
composition of materials, such as polymers, and optimize production
processes (Nasereddin et al., 2019).

31
TGA is also used in the food industry for quality control and process
optimization. It can be used to study the thermal behavior of food
components, such as proteins, carbohydrates, and lipids, as well as the
moisture content and stability of food products (Nasereddin et al., 2020).

TGA can also be used to study the thermal behavior of materials under various
conditions, such as different atmospheres and heating rates. (Mekhilef et al.,
2019). This information can be used to optimize production processes and
ensure product quality.

3.5.2. Nutritional Analysis: Thermogravimetric analysis (TGA) is used in

nutritional analysis to determine the moisture content and thermal stability of
food components. TGA can be used to study the thermal degradation and
stability of nutrients, such as vitamins, amino acids, and fatty acids, under
different heating rates and atmospheres (Kaya et al., 2019).

TGA can also be used to determine the moisture content and water activity of
food products, which are important parameters for quality control and shelf-
life determination. By measuring the weight loss of a sample as a function of
temperature, TGA can provide information about the water content and
stability of food products (Barrere-de Groot et al., 2001).

TGA is a powerful tool in nutritional analysis, providing valuable information

about the thermal behavior and stability of food components, as well as the
moisture content and water activity of food products.

3.6. Conclusion.
32
In conclusion, thermogravimetric analysis is a powerful tool that allows
scientists to study how materials behave when they are heated up. It involves
heating up a tiny amount of the material being studied and measuring its
weight over time. Scientists can use TGA to learn about the thermal stability of
a material, its composition, and its decomposition behavior. TGA is used in
many different fields, including chemistry, engineering, medicine, and more. By
understanding how materials behave when they are heated up, scientists can
develop new and better materials and medicines that can help people in many
different ways.

SUMMARY

Thermogravimetric analysis, or TGA for short, is a way for scientists to study

how materials change when they are heated up. They can learn a lot of things
from TGA, like how hot a material can get before it breaks down, what it is
made of, and how it behaves under different conditions.

TGA is done using a special machine that heats up a tiny amount of the
material being studied and measures its weight over time. The machine can be
set to different temperatures and atmospheres, like air, nitrogen, or even
water vapor, to simulate different conditions. Scientists can also add other
things to the sample, like other chemicals, to see how they affect the material.
One thing scientist can learn from TGA is the thermal stability of a material.
This is how much heat a material can take before it starts to break down. For
example, plastic that can withstand high temperatures is better for things like
making oven-safe containers. TGA can also show scientists if there are any

33
impurities in the material, or if it is a mix of different things. This can be
important in many different fields, like chemistry, engineering, and medicine.

Another thing TGA can show scientists is the decomposition behavior of a

material. This means how the material breaks down when it is heated up. For
example, some materials like wood turn into ash when they are burned, while
others like plastic melt and release fumes. Scientists can use TGA to figure out
what kind of things are released when a material breaks down and at what
temperatures it happens.
TGA is also used in the pharmaceutical industry to study how drugs behave
when they are heated up. This is important because some drugs can break
down or change when they are heated up, and this can affect how well they
work. Scientists can use TGA to see what temperature a drug breaks down at,
and how fast it happens. They can also use it to see if the drug is mixed with
any other substances that might affect how it works.

Overall, thermogravimetric analysis is a way for scientists to study how

materials behave when they are heated up. It can tell them things like how hot
a material can get before it breaks down, what it is made of, and how it
behaves under different conditions. Scientists can use TGA to study all kinds of
materials, like plastic, wood, drugs, and more. By understanding how materials
behave when they are heated up, scientists can develop new materials and
medicines that work better and last longer.

In conclusion, thermogravimetric analysis is a powerful tool that allows

scientists to study how materials behave when they are heated up. It involves
heating up a tiny amount of the material being studied and measuring its

34
weight over time. Scientists can use TGA to learn about the thermal stability of
a material, its composition, and its decomposition behavior. TGA is used in
many different fields, including chemistry, engineering, medicine, and more. By
understanding how materials behave when they are heated up, scientists can
develop new and better materials and medicines that can help people in many
different ways.

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