APPLICATIONS OF THERMO

GRAVIMETRIC ANALYSIS (TGA)

 APPLICATIONS OF TGA
Thermal stability:
TGA can be used to evaluate the thermal stability of a
material in a desired temperature range. TGA also gives
the upper use temperature of a material. Beyond this
temperature the material will begin to degrade. We can
determine the purity and thermal stability of both primary
and secondary standard.
Prediction of stability:
Predictions of lifetime (stability) at desirable time &
temperature conditions in desirable environment
 APPLICATIONS OF TGA
Kinetics of reaction rate:
• TGA is used to study the kinetics of the reaction rate constant.
• Thermo gravimetric kinetics may be explored for insight into
the reaction mechanisms of thermal (catalytic or non-catalytic)
decomposition involved in the pyrolysis and combustion
processes of different materials. Activation energies of the
decomposition process can be calculated using Kissinger
method.
• Though a constant heating rate is more common, a constant
mass loss rate can illuminate specific reaction kinetics. For
example, the kinetic parameters of the carbonization of
polyvinyl butyral were found using a constant mass loss rate of
0.2 wt. %/min.
 APPLICATIONS OF TGA
Used in the study of catalyst:
• The change in the chemical states of the catalyst may be
studied by TGA techniques. (Zn-ZnCrO4) Zinc-Zinc chromate is
used as the catalyst in the synthesis of methanol.
Extend lifetime of DSC cell:
• In an overview of thermal analysis testing it is always preferable
to do a TGA experiment on unknown samples before doing a
DSC experiment (especially for pharmaceuticals) because
Decomposition of pharmaceuticals renders products which are
insoluble and generally sticky on the inside of a DSC cell.
• These products will lower the life use of a DSC cell. Therefore,
knowing of the decomposition temperatures of all drugs, heat in
a DSC evaluation should maintain 50°C below to those
decomposition temperatures.
 APPLICATIONS OF TGA
Measure evaporation rates:
• Can be used to measure evaporation rates, such as to
measure the volatile emissions of liquid mixtures
• Evaporation of free (unbound) water begins at room
temperature due to dry gas flowing over the sample.
• Dehydration/Desolvation of bound water always begins at
temperatures above room temperature and typically at 125°C.
• E.g. Determination of the bound and unbound water in the
suspension of Milk of Magnesia (MoM), used as a laxative.
• Decomposition can have multiple stages (weight losses) but
the presence of multiple weight loss steps can also indicate
the presence of multiple components in the sample.
 APPLICATIONS OF TGA
Lifetime of product:
• Estimate lifetime of a product
Measure residual solvent:
• TGA is often used to measure residual solvents and moisture, but can
also be used to determine solubility of pharmaceutical materials in
solvents.
Reactive and corrosive material:
• The effect of reactive or corrosive atmosphere on materials
Characterization of material:
• TGA is used as a technique to characterize materials used in various
environmental, food, pharmaceutical, and petrochemical applications.
• Determination of the composition of complex mixture and
decomposition of complexes can also be done.
• Use for studying the sublimation behavior of various substances.
 APPLICATIONS OF TGA
Determination of purity:
• Can determine the purity of a mineral, inorganic compound, or
organic material
Temperature and weight change:
• Determine temperature and weight change of decomposition
reactions, which often allows quantitative composition analysis.
Also used to determine water content in sample
Analysis of reaction:
• Allows analysis of reactions with air, oxygen, or other reactive
gases
Determination of Curie temperature:
• Allows determination of Curie temperatures of magnetic transitions
by measuring the temperature at which the force exerted by a
nearby magnet disappears on heating or reappears on cooling.
 APPLICATIONS OF TGA
Inorganic Filling materials:
• Used to measure the weight of fiber glass and inorganic fill
materials in plastics, laminates, paints, primers, and composite
materials by burning off the polymer resin. The fill material can
then be identified by XPS and/or microscopy. The fill material may
be carbon black, TiO2, CaCO3, MgCO3, Al2O3, Al (OH)3,
Mg(OH)2, talc, Kaolin clay, or silica, for instance. It can measure
the fill materials added to some foods, such as silica gels and
titanium dioxide.
Distinguish mineral’s composition:
• Distinguishes different mineral compositions from broad mineral
types, such as borax, boric acid, and silica gels
Analysis of Impurities:
• Impurities analysis in materials.
 APPLICATIONS OF TGA
Analysis of polymeric formulation:
• Used in compositional analysis of polymeric formulation.
• TGA is used in the analysis of polymers. Polymers usually
melt before they decompose, thus TGA is mainly used to
investigate the thermal stability of polymers. Most
polymers melt or degrade before 200 °C. However, there
is a class of thermally stable polymers that are able to
withstand temperatures of at least 300 °C in air and 500
°C in inert gases without structural changes or strength
loss, which can be analyzed by TGA.
 APPLICATIONS OF TGA
Oxidation and combustion:
• The simplest materials characterization is the residue
remaining after a reaction.
• For example, a combustion reaction could be tested by
loading a sample into a thermogravimetric analyzer at
normal conditions. The thermogravimetric analyzer would
cause ion combustion in the sample by heating it beyond
its ignition temperature. The resultant TGA curve plotted
with the y axis as percentage of initial mass would show
the residue at the final point of the curve. Oxidative mass
losses are the most common observable losses in TGA.
 APPLICATIONS OF TGA
Contid…
• Studying the resistance to oxidation in copper alloys is
very important. For example, NASA (National Aeronautics
and Space Administration) is conducting research on
advanced copper alloys for their possible use in
combustion engines. However, oxidative degradation can
occur in these alloys as copper oxides form in
atmospheres that are rich in oxygen. Resistance to
oxidation is very important because NASA wants to be
able to reuse shuttle materials. TGA can be used to study
the static oxidation of materials such as these for practical
use.
 APPLICATIONS OF TGA
Contid…
• Combustion during TG analysis is identifiable by distinct traces
made in the TGA thermograms produced. One interesting
example occurs with samples of as-produced unpurified carbon
nanotubes that have a large amount of metal catalyst present.
Due to combustion, a TGA trace can deviate from the normal
form of a well-behaved function. This phenomenon arises from a
rapid temperature change. When the weight and temperature are
plotted versus time, a dramatic slope change in the first derivative
plot is concurrent with the mass loss of the sample and the
sudden increase in temperature seen by the thermocouple. The
mass loss could be the result of particles of smoke released from
burning caused by inconsistencies in the material itself, beyond
the oxidation of carbon due to poorly controlled weight loss.