TCNJ Chemistry Instrumentation

Operating Instructions

Pyris 6 DSC

General Instructions

1) Make sure the DSC unit is on. The red light on the front of the instrument display should be on, and the display should read 'standby'.

a. If the unit is off, turn it on using the black switch on the back of the DSC.

b. If the display reads 'heat' followed by a temperature value or the temperature value is not between 20-25°C, STOP! Someone else is probably using the instrument. Check the instrument sign-in sheet.

2) Turn on the temperature controller that is directly behind the DSC. Do not change the temperature settings on the controller.

3) At the top of the computer screen, there should be a toolbar (Pyris Manager). Click on the button corresponding to the DSC instrument to open the DSC application window. Wait a few seconds for the instrument software to open (it's SLOW!).

4) If you know the initial temperature that you will be using for your analysis, enter it in the box in the control panel on the right side of the screen and click the 'Go to Temp' button (second from the top in the control panel, just above the temperature value).

Loading the Sample

1) Select two sample pans of the same size and two corresponding lids.

2) Add your sample to one of the pans (about 5-15mg), place a lid on top of the pan, and attach the lid using the crimper.

3) Place the other lid on top of the second (empty) sample pan, and attach the lid using the crimper.

4) Remove both lids that are covering the DSC sample chamber using tweezers.

5) Place the empty sample pan ("reference pan") on the right side of the chamber using tweezers. Place the pan containing your sample on the left side of the chamber using tweezers. (NOTE: The pan containing your sample and the "reference pan" MUST be the same size!)

Creating/Editing a Method

1) If the Method Editor does not open when you open the DSC application window, click on the Method Editor icon (second from the left in the application window toolbar).

2) The first tab in the Method Editor is the Sample Info page. Enter your operator ID, sample name, sample weight, and data file name. (The sample weight should be roughly 5-15mg.)

3) The second tab is the Initial Stage page. Enter the initial temperature of your analysis. Make sure that Y initial=0.00. Do not change the pre-run actions. Do not check the baseline subtraction box. If you think that baseline subtraction is necessary, see Alyza for instructions.

4) The third tab is the Program page. Enter your temperature program. The temperature program usually has three steps: heat, hold, and cool. A final hold step at the initial temperature is recommended to make sure that the instrument temperature stabilizes. Do not change the data sampling option or the selected value.

5) The fourth tab is the View Program page. Verify that your program is correct. If you would like to edit a segment in the program, double click on it. This will bring you back to the Initial State or Program page, where you can edit the desired segment(s).

Saving the Method

1) To save your method, click File, then choose Save As.

2) Type the desired name for your method and hit enter.

Starting the Run

1) Click on the 'Start/Stop' button located on the right side of the screen in the control panel (top button, looks like the DSC instrument with a spectrum behind it).

Monitoring Data Collection

1) The Instrument Viewer should already be open when you start your run. If not, click on the Instrument Viewer icon (leftmost icon in the application window toolbar). The Instrument Viewer displays the real-time signals from the instrument as data are collected during your run.

2) If you would like to monitor the status of your run, you can open the Status Panel by clicking on the View menu and selecting Status Panel. Choose the parameter that you would like to monitor from the drop-down list.

3) The DSC instrument button in the Pyris Manager toolbar also shows the instrument status. A green LED means that the analyzer is on but no method is running. Red means that a method is running, and the analyzer is heating. Yellow means that a method is running, and the analyzer is holding. Blue means that a method is running, and the analyzer is cooling. Dark Gray means that the analyzer is off.

Looking at Your Data

1) Open the Data Analysis window by clicking on the 'Start Pyris' button in the Pyris Manager toolbar (at the top of the screen) and selecting Data Analysis.

2) Click on File, then choose Open. Select your data file, then click Open.