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Experiment No. 4 TGA Analysis

1. The document describes the procedure for conducting a thermal gravimetric analysis (TGA) experiment to determine the thermal stability of a sample. 2. Key steps include switching on the TGA module and nitrogen gas, loading a sample into a crucible, running the analysis software to heat the sample and measure weight changes at various temperatures, and analyzing the resulting data. 3. As an example, a TGA analysis of the metal organic framework Mil-53 found it was stable up to 460-500°C, with weight changes in that range attributed to removal of unreacted reagents and complete degradation occurring above 500°C.

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SIDDHARTH BHASNEY
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32 views2 pages

Experiment No. 4 TGA Analysis

1. The document describes the procedure for conducting a thermal gravimetric analysis (TGA) experiment to determine the thermal stability of a sample. 2. Key steps include switching on the TGA module and nitrogen gas, loading a sample into a crucible, running the analysis software to heat the sample and measure weight changes at various temperatures, and analyzing the resulting data. 3. As an example, a TGA analysis of the metal organic framework Mil-53 found it was stable up to 460-500°C, with weight changes in that range attributed to removal of unreacted reagents and complete degradation occurring above 500°C.

Uploaded by

SIDDHARTH BHASNEY
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Experiment No: 4

Experiment Name : Thermal Gravimetric Analysis of (sample name).

I. Aim: To determine the thermal stability of (Sample Name) using TGA.


II. Procedure :
Steps for doing analysis :
1. Switch on cpu, monitor, water bath (22 0C set temperature (ST)), TGA module.
2. Log on into cpu and open the back side switch of module.
3. Start N2 generator and set the flow 40 cc/min.
4. After reaching “ ideal furnace off temperature” in module, follow software steps (from 1 to 5)
5. In module click furnace Keep appropriate crucible again click furnace click into tare and
wait up to ST in module screen Take out crucible by clicking furnace and keep the sample
click furnace again to insert the crucible and wait for ST again
6. Click into OK in monitor screen, the green portion will turn into red color.
7. Once analysis is done this red will change to green and prompt to press OK.
8. Press OK tab of module and take out the crucible. After that go to main window (small) of software and
go to exit option. Entire software will be closed.
9. Wait until temperature is decreased to 25 oC. Now switch off TGA, cpu, N2 generator, monitor and
water bath.

Steps for using software (if any):


1. Click on software minimize DSC window Go to TGA window edit
remove previous file.
2. Go to routine editor Select either “open” or “new” option
3. If new, New Add dyn enter appropriate data for temperature range and heating rate
Click into Pan and select the correct one (Either of 70 or 900 µl alumina) save as
4. Give the name as Min temperature- Max temperature@heating rate_Pan name.
5. Give sample name Send experiment (green color will appear).
6. Data will be stored automatically and to extract the data – Main window evaluation graph
import/export open correct file (you have to see file name) save as text file.

III. Result and Analysis

1. Instrument name(make and model):


2. Sample name :
3. Sample amount:

Table 1: Observed data

Weight degradation step Attributed to

Calculation for derivative plot:


Data will be obtained in form of text file, so we have to extract the data in excel. Here weights (w) of sample
will be obtained at different temperatures depending upon the input conditions for temperature range and step
size.
Zero value of dm/dT signifies stability of the sample for that temp regime.

( w1 − w2 )
(dm / dT )1 =
(T2 − T1 )
Where
(dm/dT)1 is value of derivative at point 1
w1, w2 are weight of sample at point 1 and point 2 respectively
T1, T2 are the absolute temp at point 1 and point 2 respectively.

Discussion:

IV. Precautions to be taken :


1. Care is required when handle with the crucible.
2. Never switch off the module if software is running.

V. Example analysis
Aim : determination of thermal stability of Mil-53 using TGA
Result :
1. Sample name : Mil-53 ( metal organic framework)
2. Sample amount: 20 mg
Plot:

Table 1: Observed data (Mil-53)

Weight degradation step Attributed to


Upto 100 oC Removal of water
460 oC – 500 oC Removal of unreacted Benzene dicarboxylic acid
500 oC - onwards Complete degradation

Discussion: TGA analysis shows the thermal stability of Mil-53 up to (673 K). DTH plot shows the
stability of sample from 100 to 400 oC.

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