BAHIR DAR UNIVERSITY

ETHIOPIAN INSTITUTE OF TEXTILE AND FASHION TECHNOLOGY

TEXTILE MANUFACTURING
POST GRADUATE PROGRAM
SEMINAR ON THERMOGRAVIMETRIC ANALYSIS (TGA)

ANDEBET KASSAW
FIRST YEAR MSC.

BAHIR DAR, ETHIOPIA

ASSOC. PROFESSOR ADANE H.
MARCH 13 , 2022
 Contents

Introduction

Theoretical background

Instrumentation and Principles

Data interpretation and analysis

TGA characterization of some fibers

Limitation

Summary

Reference

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 Introduction

Thermal analysis

 The physical and chemical properties of a materials are determined as a

function of temperature and /or time, while sample is subjected to a
controlled temperature.

 Differential Thermal Analysis (DTA)- temperature

 Differential scanning calorimetry (DSC)- Energy
 Dynamic mechanical analysis (DMA) - deformation
 Thermogravimetric Analysis (TGA) -mass
 Thermomechanical analysis (TMA) - dimensions
 Thermo-optical analysis (TOA) -optical properties

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 Thermogravimetric Analysis (TGA)

 TGA is a thermo-analytical technique that measures the weight changes of a

sample at a given time and temperature.
 To determine the thermal and/or oxidative stabilities of materials as well as
their compositional properties.
 It analyze materials that exhibit either mass loss or gain.
 The study of polymeric materials, including thermoplastics, thermosets,fibers.
 To provide information to select materials for certain end-use applications,
predict product performance and improve product quality.

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 Application of TGA

 Compositional analysis of fibre blends

 Thermal stabilities
 Oxidative stabilities
 Decomposition kinetics
 Effects of reactive atmospheres on textile materials
 Filler content of materials
 Moisture and volatiles content

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 Theoretical background

 Thermal analysis was first introduced by Le Chatelier in 1887.

 The earliest TGA experiments were performed by heating the samples to a specific
temperature and then removing the sample at specific time intervals for weighing.
 In 1912, Urbain and Boulanger built device that comprised a conventional balance
adapted for null point electromagnetic compensation.
 The measurement of mass change using temperature thermogravimetry (TG) was
discovered by Honda, a physicist from Japan in 1915.
 In modern TGA, it determines the quantity and the frequency of the weight variation of
the samples against temperature and time in a controlled atmosphere.

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 Sample preparation

 The sample weight affects the accuracy of weight loss measurement.

 Maximizing the surface area of the sample in a TGA pan improves resolution
and reproducibility of weight loss by the temperature.
 Typically 10-20mg of sample is preferred in most application.
 Whereas, if the sample has volatiles 50-100mg of sample is considered
adequate.
 Ensure good sample contact between the sample and heat flux sensor.

Experimental condition
 Atmosphere : in air or inert gas (He,Ar, N2)
 Heating/cooling rate : 10-20 oc /min Mostly for textile materials
 Temperatures : 0 oc - 1000 oc

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 Instrumentation and Operating Principles

Null-point balance system

 Components to provide the flexibility for the accurate analytical data
 Balance
 Furnace
 Recorder

 Temperature programmer
 It can be isothermal (T (t) is constant) or non-isothermal (heating rate is constant)
 The heating rate(𝛽) can be expressed as 𝛽 = dT/dt

Principles
 The sample is heated in a given environment at controlled rate.
 The change in the weight of the substance is recorded as a function of temperature or time.
 The temperature is increased at a constant rate for a known initial weight of the substance and the
changes in weight are recorded as a function of temperature at different time interval.
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 Data interpretation and analysis

 The high volatility weight loss is due to the loss of plasticizers from the polymer.
 The low volatility weight loss is due to degradation of the residual polymer.
 Weight loss due to combustion of compounds such as residual carbon from
polymer breakdown or burn off of carbon black filler.
 The residue value is the remaining ash due to inorganic filler materials that were
present in the material. 

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Typical TGA curves

1.No change/decomposition
2.desorption/drying (rapid initial mass loss)
3.single stage decomposition
4.multi-stage decomposition with relatively
stable intermediate
5. multi-stage decomposition with no stable
intermediates
6.atmospheric reaction(gain in mass)
7. Product decomposes at higher temperature.

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 Factors affecting the shape of the TG curves

 Furnaces Atmosphere – different furnaces atmosphere will give different TG curves.

 Heating rate – sample heated at faster rate decompose at higher T o
 Weight of the sample – a smaller weight gives better results.
 Particle size of the sample – small particle size of sample decompose at lower T o
 Source of the sample - two different sample sources have different decomposition T o
 Compactness of the sample – a compressed sample decompose at higher T o

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 TGA characterization of some fibers

1. Cotton fiber with a micronaire of 4.8, a strength of 28.5cN/tex, and MR of 0.9 in N 2 gas.

4.2% 65.8% 26.1%

Thermal decomposition between 37 and 150 0C for region I,225 and 425 0C for region
II,425 and 600 0C for region III.
At a temperature below 200 0C due primarily to the loss of adsorbed water.
At a temperature above 200 0C due to thermal decomposition and depolymerization.
Between 250 and 290 0C primary volatile decomposition releases CO2, CO, and H2O.
 2.Poly(ethylene terephthalate)(PET) fibers in nitrogen and air atmospheres

Under inert gas only mass loss (above 80 %) due to thermal dissociation of the fibers. The
highest rate of mass loss at 458.8 0C.
Under atmosphere of air additional more than 15 % mass loss due to ignition and
combustion of the sample.The highest rate of combustion is obtained at 545.5 0C.
 3.TGA curves of nylon 6,6 fiber under a nitrogen purge gas

The nylon 6,6 fibre under goes thermal degradation beginning at 482 ˚C and
final degradation temperature
. 530 ˚C with a total mass loss of 99.0%. There is
a small amount of inert residue remaining (0.15%).

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 Limitation of TGA

 The chemical and physical changes which are not accompanied by mass change are not
indicated.
 TGA curves are not ‘fingerprint’ curves – different parameters will yield different results.
 Secondary means of material identification –if the material is unknown ,it may be
necessary to run other tests such as DSC,FTIR prior to TGA testing.
 Overlap separation of multiple parts with similar decomposition temperature ranges are
difficult.

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 Summary

 TGA is a reliable technique that can be used to study the thermal stability and
decomposition of textile materials.
 It determines the rate of change in weight of the material, whereas the material is
being heated or cooled at a controlled temperature.
 It is applicable to different industrial sectors to characterize materials.
 TGA is commonly employed in research and testing to determine characteristics of
materials such as textile polymers and fibers.

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 Reference

1. https://resources.perkinelmer.com/corporate/cmsresources/images/44-132088app_cha
racterizationofpolymersusingtga.pdf
2. https://www.researchgate.net/publication/328959555_Thermogravimetric_Analysis_o
f_Polymers
3. Abidi, N., Hequet, E., & Ethridge, D. (2007). Thermogravimetric analysis of cotton
fibers: relationships with maturity and fineness. Journal of applied polymer
science, 103(6), 3476-3482.
4. Matthias Wagner,Thermal Analysis in Practice,Hanser,2018,Pages 162-186,ISBN
9781569906439
5. https://www.sciencedirect.com/topics/materials-science/thermal-analysis
6. https://www.lpdlabservices.co.uk/analytical_techniques/chemical_analysis/tga_interp
ret.php
7. http://instrument-specialists.com/thermal-analysis-applications/
8. https://www.sctce.ac.in/faculty/facultylogin/Admin/Attachments/Upload/1559024845
_1559024845.pdf
9. https://www.ri.se/en/what-we-do/services/thermogravimetric-analysis-tga
10. Gawłowski, A., Fabia, J., Graczyk, T., Ślusarczyk, C., Janicki, J., & Sarna, E. (2016).
Study of PET fibres modified with phosphorus–silicon retardants. Journal of Thermal
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Analysis and Calorimetry, 125(3), 1327-1334.
 THANK YOU
FOR YOUR
ATTENTION!!

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