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SSK 4242
INTRODUCTION
Lecture 5 4-Nov-04 1
Thermal Analysis
SSK 4242
Exercise:
• Give examples of reactions/processes for each of the physical
and chemical changes above.
• Write down the chemical equation for the examples given
Lecture 5 4-Nov-04 2
Thermal Analysis
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APPLICATION OF TGA
Lecture 5 4-Nov-04 3
Thermal Analysis
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Application of TGA in Catalysis
TGA can be used to optimise catalytic processes. The
effects of parameters (e.g. the catalyst composition,
temperature, gas flow) on the catalyst can be quickly
studied for its effectiveness before a large scale
production of the catalyst is carried out.
Example: The support
material is soaked in the NiNO3
solution. After dehydration
and decomposition of the
metal salt in the air, the
The effect of heating rate, gas atmosphere is changed to
flow, and the temperature for hydrogen to produce a metal
each step can be varied and their powder that is impregnated on
effects on the development of the surface of the support.
catalyst can easily be studied.
Figure 4.1 TGA application for optimisation of the method for the production of a catalyst.
Lecture 5 4-Nov-04 4
Thermal Analysis
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the conditions of the surface area of the support materials that is coated with
the catalyst at the temperature when a mono-layer is formed;
Example: TGA and DTA have been used for the preparation studies of the
following:
- for the oxidation of catalyst La1-xMxMnO3 where M is Pb, Ca, Sr or Ba
- for the thermal decomposition and catalytic studies of BaxLn1-xCoO3 where
Ln is La, Nd, Sm and Dy.
Lecture 5 4-Nov-04 5
Thermal Analysis
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Application of TGA in Clay and Mineral Industries
Evaluation by characterisation of the raw material deposits,
Classification and analysis,
Investigation on the raw materials that have underwent various industrial
processes,
Technique for solving various problems arising from the changes of the
raw materials, new technologies, and new specifications.
Example:
mass loss due to dehydroxylation of the clay may be used for the
determination clay content of a mixture.
If the curve shows overlapping mass losses of two processes, separation
of the two processes may be carried out by an isothermal heating, such as
in the determination of alunite and kaolinite in the alunitic clay and the
determination of MgCO3 and CaCO3 in dolomite.
See next page … Lecture 5 4-Nov-04 6
Thermal Analysis
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TGA And DTG Curves of Kaolinite Standard.
• Kaolinite is an important clay which is used as filler or mixture in the paper,
ceramics, and rubber industries.
• Available naturally in most countries, clay represents a secondary mineral that is
formed out of the weathering and hydrothermal processes on aluminum silicate,
particularly the feldspar.
• Adsorbed water is
liberated within the
temperature range up to
200 oC with a quantity
0.2 % of the kaolinite
sample mass.
• The hydroxylation
process takes place
within the temperature
range of 400 – 700 oC
causing mass loss of
13.8 %.
• The DTG curve has a
peak shape (similar to a
Figure 4.2
DTA curve) and the
position of the peak may
alter with the change in
the heating rate, sample
particle size, etc.
Lecture 5 4-Nov-04 7
Thermal Analysis
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Application of TGA in Coal Industries
Figure 4.3
From one sample (10 – 30 mg) several parameters such as the moisture content,
volatile materials, carbon, and the ash residue were determined simultaneously.
Lecture 5 4-Nov-04 8
Thermal Analysis
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Application of TGA in Petroleum Industry
Figure 4.4: TGA of three petroleum products: the crude oil, light oil and
asphalt
The sample was placed in a sample holder with a pin-holed cover.
The light oil (low molecular mass) distilled out at the temperature range of
100 – 330 oC, crude oil 300 – 600 oC, and the asphalt 250 – 650 oC.
Lecture 5 4-Nov-04 9
Thermal Analysis
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Application of TGA to Inorganic Analysis
TGA may be used for the determination of The figure shows that the
calcium, strontium and barium as a mixture decomposition process of the
of their salts. oxalates are independent to each
other. The water of hydration is
The ions (Ca2+, Sr2+, and Ba2+) are removed at 100 – 250 oC.
precipitated as their oxalates and then
decomposed under N2 atmosphere in a TGA Based on the individual curve of
system. The Ca, Sr and Ba contents are the respective compounds, the
derived directly from the TGA thermogram water content removal from the
(Figure 4.5). oxalates takes place according to
See Figure 4.5 the order of barium, strontium and
calcium. However, in the mixture,
decomposition of the oxalates of
The quantities of calcium, C, strontium, S, and
strontium and calcium take place
barium, B, can be calculated from the data
simultaneously.
extracted from the voltammogram as follows:
The determination error using this
• The amount of Calcium, C = 0.91068 . G technique is about 1 %.
• The amount of Strontium, S = 1.9911 . L
• The amount of Barium, B = 0.58603 . D - 1.9456 . G - 2.5788 . L
Lecture 5 4-Nov-04 10
Thermal Analysis
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Figure 4.6 shows the TGA and DTA curves for the decomposition of
Cu2(C2H3O2)4 . 2H2O.
The TGA curve shows that two main thermal processes
have taken place, but the DTA curve indicates that the
thermal process is much more complex.
See Figure 4.7 for the TGA and DTA of the decomposition of Cuprum
Trichloroacetate 4-dihydrate.
Lecture 5 4-Nov-04 11
Thermal Analysis
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Figure 4.9 shows the TGA and DTA curves for the
thermal decomposition and transformation of
rhenium metal oxide: RhOOH (orthorombic) and
RhO2 (tetragonal)
Lecture 5 4-Nov-04 12
Thermal Analysis
Application of TGA in Pharmaceutical SSK 4242
• Medication materials normally contain analgesic agents (reduce pain due to organic and/or
psychological confusion).
• Among those analgesics that have been in use are (I) acetylsalicylic acid (aspirin), (II)
salicylamide, (III) phenasetin, and (IV) N-Acetil-p-aminophenol (acetaminophen)
Figure 4.11(a) dan (b) show the TGA curves of 12 analgesic agents
found in the market
(a) (b)
Lecture 5 4-Nov-04 14
Thermal Analysis
Figure 4.12 a and 12b show the TGA curves for antacids (medication for SSK 4242
the treatment of gastric or internal digestion system). Each preparation has
different capacities to neutral acid in the internal digestion system.
The active components of antacids are calcium carbonate, sodium hydrogen carbonate, aluminum hydroxide,
magnesium trisilicate, dihidroxy aluminum aminoacetate, etc.
(a) (b)
Lecture 5 4-Nov-04 15
Thermal Analysis
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Determination of Pharmaceutical Material Composition
The thermal processes that are useful for the determination of pharmaceutical
material composition are:
Lecture 5 4-Nov-04 17