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Thermogravimetric Analysis

Introduction to Thermogravimetry

In this technique (TG or TGA), changes in


the mass of a sample are studied while
the sample is subjected to a controlled
temperature
programme.
The
temperature programme is most often a
linear increase in temperature, but
isothermal studies can also be carried
out, when the changes in sample mass
with time are followed.

The main processes amenable to study are listed below


Process
Ad- or
absorption

Weight gain

Weight loss

Desorption

Dehydration/d
esolvation

Sublimation

Vaporization

Decomposition

Solid-solid
reactions

Solid-gas
reactions

TG is inherently quantitative, and therefore an


extremely powerful thermal technique, but gives
no direct chemical information. The ability to
analyse the volatile products during a weight
loss is of great value.
Instrumentation

The essential components of the equipment


used, called a thermobalance, are a
recording balance, furnace, temperature
programmer, sample holder, an enclosure for
establishing the required atmosphere, and a
means of recording and displaying the data.

Applications
Thermal Stability: related materials can be compared
at elevated temperatures under the required
atmosphere. The TG curve can help to elucidate
decomposition mechanisms.
Kinetic Studies: a variety of methods exist for
analysing the kinetic features of all types of weight loss
or gain, either with a view to predictive studies, or to
understanding the controlling chemistry.
Material characterisation: TG and DTG curves can be
used to "fingerprint" materials for identification or quality
control.

Simulation of industrial processes: the


thermobalance furnace may be thought of as a minireactor, with the ability to mimic the conditions in
some types of industrial reactor.
Compositional analysis: by careful choice of
temperature programming and gaseous environment,
many complex materials or mixtures may be analysed
by selectively decomposing or removing their
components. This approach is regularly used to
analyse e.g. filler content in polymers; carbon black in
oils; ash and carbon in coals, and the moisture
content of many substances.
Corrosion studies: TG provides an excellent means
of studying oxidation, or reaction with other reactive
gases or vapours

PRECAUTION: NEVER OPEN THE FURNACE


WHEN THE TEMPERATURE IS ABOVE 100 C
Procedure:
To Do A Correction Run
Click on the measurement Icon and wait for the signals on,
mg, temp
Place empty crucible in the sensor Select FILE, NEW
Select Correction mode.
Enter necessary details and click continue
Select Tcalzero and click open
Press Dynamic ,Enter the End temperature and heating rate
and then click add
Press Final and click add, and then press continue
Save the file
Click start

To Do a Sample + Correction measurement:


Select FILE , OPEN
Select the suitable correction file
Choose Sample + Correction Mode
Enter necessary Details and click continue
Select Tcal Zero
Here we have only option to change the end
temperature.
Heating
rate
and
initial
temperature has to be same.
Click continue
Save file
Click start

To Do the analysis.
Click on Proteus analysis Icon
Click File and open the data you want to analyse
If the measurement just got over. In the
measurement window press tools Run analysis
program
Click on the curve Change time to temperature
Click on AXIS,CURVE,GRID and remove flow
meter readings
Click on Mass change and find the Loss
percentage
Click on Residual mass and find the Remaining
mass

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