First, prepare before starting

Before using the scanning calorimeter, check the appearance of the instrument for damage and confirm that the power connection is stable. Turn on the supporting cooling system to ensure that the temperature is stable within the set range. Generally, it needs to be run 15-20 minutes in advance. At the same time, prepare dry and clean sample crucibles and reference crucibles to avoid impurities affecting the test results.

Second, the sample loading operation

Grind the sample to be tested into a uniform powder, accurately weigh 5-10mg and put it into the sample crucible, paying attention to not too much or too little sample. The reference crucible is filled with an equal amount of inert material, such as empty crucible or alumina powder. After filling, use tweezers to smoothly place the two crucibles into the designated slot of the instrument furnace body to ensure accurate placement and avoid tilting or shifting.

III. Key points of parameter setting

Open the instrument control software and enter the parameter setting interface. Set the heating rate according to the characteristics of the sample. The normal range is 5-20 ° C/min. It is recommended to choose a slower rate for samples with poor thermal stability. At the same time, set the test temperature range to cover the temperature range where the sample may undergo thermal changes, such as from room temperature to sample decomposition temperature. After confirming that the parameters are correct, click Save and start the test program.

IV. Testing process monitoring

After the test is started, observe the temperature curve and heat change data of the software interface in real time. If the curve fluctuates abnormally, the test should be suspended immediately to check whether it is caused by improper sample filling and instrument failure. During the test process, keep the surrounding environment of the instrument stable, avoid vibration and strong magnetic field interference, and ensure accurate and reliable data.

Data storage and shutdown

After the test, when the temperature of the instrument drops to room temperature, save the test data and derive the original map and analysis report. Take out the sample crucible and reference crucible, and clean the residual impurities in the furnace body. Finally, turn off the power supply and cooling system of the instrument, organize the experimental table, and complete the entire operation process. Mastering these steps will enable the standard and efficient use of scanning calorimeters to carry out thermal analysis experiments.