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Simultaneous Differential Scanning Calorimetry & Thermogravimetric Analysis

A simultaneous DSC-TGA device that can be used to characterize any material exhibiting a weight change or  a phase change between ambient and 1500 oC.(i.e.); the mass of a substance and the difference in energy inputs into a substance   and a reference material are both measured simultaneously as a function of temperature while the substance and reference material are subjected to a controlled temperature program.

DSC-TGA

DSC Measurements

1. We will use TA instruments model SDT 2960 Simultaneous DSC-TGA
2. For instrument controller, data collection, and analysis, the software named Thermal Advantage is employed. The user interface and functional panes are shown as below.

DSC Measurement

3.This measurement will perform differential scanning calorimetry (DSC).
4. Before your experiment, consult your advisor.
5. Select the desired instrument for your experiment (Here the computer controller is running both DSC 2010 and SDT 2960 system), using the Window menu fount on the Controller menu or the click on the desired button on the instrument task bar.
6. Selecting the desired mode of operation as DSC-TGA. You can use the Experimental/Mode menu or click the MODE button on the tool bar to find Mode Parameters Window and select the instrument mode. The modes supported by the instrument are listed in the Mode Selection field.
7. DSC Heat Flow Calibration is available only for DSC-TGA mode and the DSC Heat Flow Calibration is required when running in the DSC-TGA mode. To use menu item to perform a DSC heat flow calibration, the DSC Heat Flow window is displayed after you select this mode option. Heat flow calibration is based on analyzing the heat capacity curve for sapphire over the range 200 to 1500°C.
8. Selecting and preparing a sample. This involves preparing a sample of the appropriate size, selecting the sample cup, and placing the sample in the cup. For DSC-TGA experiments, the ceramic (aluminum) 90µL cups must be used.
9. Loading and taring the sample cup (and a reference cup) on the balance. Taring the cups ensures that the weights measured by the balance reflect the weight of the sample only. This should be done before each experiment with the furnace closed. When you tare a cup and than the SDT read the weight of the empty cup and store the weight as an offset, which is subtracted from subsequent weight measurements.
10. Entering experimental information through the TA controller. Select the desired technique to set up your experiment by accessing the Experimental View or starting the Wizard functions. You also can use procedure file (.prc), which contains parameters and information including the method name and segments that are more familiar to our experienced customers.
11. Creating and selecting the thermal method on the controller, and schedule the run. If you have method files from experiments that were done before the Advantage software became available, you can still use these files. Otherwise, You can set up your own experimental parameters by clicking the Editor button on the Procedure Page to display the Method Editor window.
12. Setting up any external accessories, such like Air Cool Option, a Purge Gas, and Gas Switching Accessory.
13. Starting the experiment with Control/Start or click the Start button on the tool bar.
14. As results from the measurements, you can monitor the real-time signals, plot, and method progress as the example in Figure: the DSC-TGA plot of AgGaTe2 showing the melting peak and the weight loss occurring at the elevated temperatures.

DSC Measurement 2

TGA Measurements

1. Here we will use TA instruments model SDT 2960 Simultaneous DSC-TGA.
2. For instrument controller, data collection, and analysis, the software named Thermal Advantage is employed. The user interface and functional panes are shown the same as DSC measurements.
3. This measurement will perform thermogravimetric analysis (TGA).
4. Before your experiment, your advisor need be consulted.
5. Select the desired instrument for your experiment (Here the computer controller is running both DSC 2010 and SDT 2960 system), using the Window menu fount on the Controller menu or the click on the desired button on the instrument task bar.
6. Selecting the desired mode of operation as TGA-DTA. Here you can use the Experimental/Mode menu or click the MODE button on the tool bar to find Mode Parameters Window and select the instrument mode. The modes supported by the instrument are listed in the Mode Selection field.
7. TGA Weight Calibration should be performed on the SDT at least once a month. It is based on two runs conducted in the TGA-DTA calibration mode -- one using calibration weights and one using no weights (empty beams). The data from both runs is analyzed and beam and weight corrections factors are calibrated. This calibration is applied when using either the DSC-TGA or TGA-DTA mode. But the calibration data must be obtained with the instrument in TGA-DTA Calibration mode
8. Selecting the desired mode of operation as DSC-TGA or TGA-DTA. Here is the same as above mode selecting method.
9. Selecting and preparing a sample involve preparing a sample of the appropriate size, selecting the sample cup, and placing the sample in the cup. For DSC-TGA experiments, the ceramic (aluminum) 90µL cups must be used. For TGA-DTA experiment, the ceramic (40µL or 90 µL) or platinum (40 µL or 110 µL) cups are acceptable alternatives. Platinum is generally prepared for TGA-DTA work. All cup types are reusable.
10. Loading and taring the sample cup (and a reference cup) on the balance. Taring the cups ensures that the weights measured by the balance reflect the weight of the sample only. This should be done before each experiment with the furnace closed. When you tare a cup and than the SDT read the weight of the empty cup and store the weight as an offset, which is subtracted from subsequent weight measurements.
11. Entering experimental information through the TA controller. Select the desired technique to set up your experiment by accessing the Experimental View or starting the Wizard functions. You also can use procedure file (.prc).
12. Creating and selecting the thermal method on the controller, and schedule the run. If you have method files from experiments that were done before the Advantage software became available, you can still use these files. Otherwise, You can set up your experimental parameters by clicking the Editor button on the Procedure Page to display the Method Editor window.
13. Setting up any external accessories, such like Air Cool Option, a Purge Gas, and Gas Switching Accessory.
14. Starting the experiment by selecting Control/Start or click the Start button on the tool bar.
15. As results from the measurements, you can monitor the real-time signals, plot, and method progress. An example for DSC-TGA plots of AgGaTe2 the same as in the Figure for DSC measurement.