Sample Preparation Procedure

The sample was thoroughly dried in the solid state to avoid damaging the equipment. Weigh The sample being tested was weighed to 2 mg in a Tzero hermetic aluminum pan. It is best to place the sample directly in the pans, transferring the sample from the weigh paper to the pan can lead to a loss in material. The lid was placed on the pan. It was ensured to place the lid with the indention facing down then the covered pan was placed in the blue holder, assuring that the lid is flush with the top of the holder.

The holder was then placed under the press with lid flushed with the top of the holder. Then the handle was pulled down, thus sealing the pan and lid. Repeat with an empty pan to be used as a reference.

DSC Procedure

The sealed pans were placed in the sample tray, taking note of the slot number and the reference pan was placed in a reference slot also noting the slot number. The reference pan was an empty sealed pan and was used for multiple runs. The power to the cooler was turned on and was ensured to be on event mode.

The software was opened, TA Universal Analysis on the desktop of the computer. In the Control tab, down to event and press the ‘On’ was clicked. This will start the cooler. The ‘Go to standby temp’ was pressed so that the cell does not freeze. The temperature of the cell indicated in the status bar.

The nitrogen gas tank was turned on, and held at 20 psi and the sample purge flow was set at 50 ml min-1.

On the program in the center panel named “ ” the data for the sample that was running was entered. and all the information needed were filled out which includes: sample name, sample weight, sample slot number, reference slot number, and data storage location.

On the second tab, Procedure, the parameters for the operating procedure were entered.

To adjust the procedure type, Test wa clicked and from on Editor to set the temperatures, ramp rates, holding times, cycle names, etc.

At this time the procedure was saved to be used in further experiments. On the far right panel, Experiment, runs was added. After inserting all of the sample information and the runs are in the appropriate order the program was started. There was an arrow next to the run that will begin first.

When the program ends, the cooling system was automatically turn off. However, the nitrogen tank was turned off after the test.