Submitted By: Muhammad Abubakar Qamar

Roll no: 17-MME-S2-328

Group: 5
Submitted To: Mr. Muhammad Ishtiaq
Subject: Ceramics & Glasses

Department of Metallurgy & Materials Engineering

College of Engineering & Emerging Technologies

University of the Punjab, Lahore

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 Lab Report # 02

Experiment # 02:
To perform thermogravimetric analysis of china clay, bentonite clay, fire clay, soda feldspar or
potash, feldspar and silica.
Objective:
To perform thermogravimetric analysis of china clay, bentonite clay, fire clay, soda feldspar or
potash, feldspar and silica.
Principle:
The principle of thermogravimetric analysis is that with the change in temperature of given
sample of clay, the weight of clay also changes. The graph plot of weight against change in
temperature is called thermogravimetric curve or thermogram, this is basic principle of TGA.
Background:
Thermogravimetric analysis is a branch of thermal analysis that deals with the mass change of a
sample as a function of temperature. Also thermogravimetric analysis is in which physical and
chemical properties of material or sample are measured as a function of increase in its
temperature [1]. This process is used to study materials that change their properties when
subjected to thermal events such as oxidation, decomposition, reduction etc.
There are 3 types of TGA
1. Dynamic TGA: In this type, sample is subjected to condition of continuous increase in
its temperature usually linear with time.
2. Isothermal or Static TGA: In this type sample is maintained at a constant temperature
for a period of time during which change in weight is recorded.
3. Quasi-static TGA: In this technique the sample is heated to a constant weight at each of
a series of increasing temperature [2].

Ceramic raw materials loss their weight after heating or when subjected to thermal events
because these contain some types of water trapped in these substance. For instance they contain
the water or moisture content in following different forms;
 Combined water
 Absorbed water

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  Adsorbed water
 Free water
Each of these contents remove at different temperatures that is why we get weight difference at
different temperatures. The applications of this process is to know the composition of a
substance at different temperatures and to know the thermal stability of substances.
Apparatus:
Crucible, oven, vacuum desiccator, muffle furnace, tongs, gloves, digital weighing balance,
stopwatch.
Material required:
China clay, fire clay, bentonite clay, silica sand, river sand.
Procedure:
 Crucible was washed, dried and weighed on a weighing balance. Its reading was noted as
W1
 Then the given sample of clay or a sand was weighed as W 2 and total weight of crucible
and sand was determined by adding W1 and W2.
 The crucible with sand was then placed in an oven at a temperature of 200°C for about 10
minutes to remove moisture or other contents in it.
 After 10 minutes, the crucible was removed from oven and placed in desiccator for
cooling for about 5-10 minutes. Then it was weighed again and difference of weights
before and after 10 min heating was noted.
 Crucible was then placed in muffle furnace for next 10 minutes at a temperature of about
400°C. After 10 minutes, then it was removed from furnace and cooled down in vacuum
desiccator and then weight difference was calculated between 10-20 minutes of heating.
 The same procedure as mentioned above was repeated for crucible at temperature of
600°C and 800°C and then their weight difference was also calculated separately and in
same way as prior.
 Then overall weight change was observed and weight against temperature graph was
plotted with temperature on x-axis and weight on y-axis as shown in figure 2.1.
Observations and calculations:
Weight of crucible = w1 = 22.07 gm (River sand)
Weight of crucible + sand = w2 = 32.17 gm
Weight of sand = w3 = 10.1 gm

Table 1 Representing residual weight percent in give samples

Sample Weight Weight of sample after Residual Percentage of

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 before heating at temperature weight residual weight
heating (°C)
W1
(gm) W2 W3 W4 W5 W6= (W6/W1)*
200 400 600 800 (W1-W5) 100
°C °C °C °C -W1 (%)
(gm)
China 28.45 28.33 28.24 28.24 28.10 28.01 98.45
clay
Fire clay 28.17 28.00 27.93 27.92 27.81 27.81 98.72

Bentonite 28.97 28.86 28.76 28.76 28.76 28.76 99.27

clay
Silica 32.57 32.56 32.54 32.51 32.51 32.51 99.81
sand
River 32.17 32.16 32.11 32.11 32.09 32.09 99.75
sand

Results:
China clay:

Fire clay:

4
Silica sand:

Bentonite Clay:

5
River sand:

The maximum weight change in the given samples was observed in china clay sample i.e.
1.55%. The second observed in weight change was fire clay. After heating at 800°C its weight
was dropped 1.28%. Bentonite clay was observed as third in weight drop that was 0.73% of total
weight. The fourth one observed was river sand that was 0.25% of its initial weight. The least
weight loss was observed in case of silica sand that was 0.19% of its total weight as represented
in table 1.
Discussion:
The whole thermogravimetric process deals with the concept that the weight of sample is lost
when it is heated to a high temperature, this is done to find the thermal stability and to find the

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composition of sample at different temperatures. The fact that the weight is lost is due to, when
sample is heated firstly more volatile components or impurities or moisture entrapped in the
sample gets vaporized, and with the increase in temperature, the impurities that require more
energy to get free or vaporize gets free. As less impurities are trapped in with strong forces so
with increase in temperature weight loss becomes usually less. The point of inflection is a point
on derivative curve from where weight change or weight loss starts and onset degradation point
is a point at which change in weight becomes constant.
In case of china clay, as represented in table (1) and displayed in Fig (1) i.e. showing graph
plotted of residual weight of sample on y-axis and its derivative on alternate Y-axis against
temperature on X-axis, when it was heated to a temperature of 200°C for 15 minutes and was
cooled down in vacuum desiccator 0.4% of its weight was lost and after 400°C, the weight loss
observed was about 0.72% of its total initial weight. After heating it at 600°C, the change in
weight was not observed and after heating at 800°C again weight change was observed and that
was 1.24% of total weight and residual weight that was left behind was 98.77%.and at a
temperature of about 325°C a point is represented in figure 1 presenting onset degradation point.
Also there is the highest point represented on derivative curve is point of inflection as shown in
fig 1.
Figure 2 is representing the graph of fire clay which shows the normal curve and derivative curve
of fire clay to show the change in weight with respect to temperature. The point at a temperature
of about 300°C to 400°C shown by a small square in fig 2 shows the degradation point of the
curve and the highest point on the derivative curve is representing point of inflection. And the
last point of LHS curve shows us that the residual weight of fire clay that was left behind was
98.72% as represented in table 1. The most of weight of sample was lost, when it was heated
from 200°C to 400°C.
Figure 3 shows a graph plotted for the sample of silica sand and this graph represents a normal
curve that has a onset of degradation point on it at coordinates, where value of residual weight is
99.5 at 200°C, a tangent is drawn which cuts another tangent that touches curve where value of
residual weight is 99.90 at 400°C. Where these tangents cut each other a normal is drawn down
from this point and touches x-axis and that point shows onset of degradation as shown in
fig.2.The much of weight loss was observed when the sample was heated from 400°C to 600°C
that was 0.19% of its total weight. The point on the derivative curve that is at the highest value
shows the point of inflection.
Figure 4 shows a graph plotted for given sample of bentonite clay. In case of bentonite clay the
most of weight was lost in heating between room temperature and 400°C as shown in figure 4 by
a steep curve and the onset degradation point was found by tangent method as presented in figure
4. The highest and the lowest point of derivative curve represents the point of inflection.
Figure 5 shows the graph plotted for given sample of river sand. The much of weight loss was
observed in between 200°C and 400°C and the point of onset degradation is represented by a
small box as shown in figure 5. The point of inflection is shown by the highest point on the
derivative curve.

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Conclusion:
As represented in table 1 and figure 1, 2, 3, 4 & 5, it is concluded that in the given samples of
various sands and clays the percentage of weight loss was as follows;
China clay > Fire clay > Bentonite clay > River sand > Silica sand
References:
[1] Gurdeep R. Chatwal, Sham K. Anand, Himalya Publishing house, 2002, Instrumental
method of Chemical Analysis: Thermal methods, pg. 2701, 5th Edition.
[2] Sharma B.K. Goel publishing house, “Instrumental method of analysis”, pg. 234-237
[3]Ch#01 Material Science and Engineering by William D. Callister, Jr.,
David G. Retiwisch.