Perkin Elmer DSC-6 Thermal Analyzer

Prepared by:

J. Scanlon

Location:

Dow 2224

Hazards:

The following materials and equipment associated with this procedure present exposure or physical health hazards. Safety precautions are prudent and mandatory.



Controls:

Prior to performing this procedure, the following safety equipment must be accessible and ready for use: (e.g. chemical fume hood, biological safety cabinet, laminar flow hood, chemical spill kits)



Protective Equipment:

Prior to performing this procedure, the following personal protective equipment must be obtained and ready for use: (e.g. acid resistant gloves, safety eyewear, lab coat, chemical splash apron)



Waste Disposal:

This procedure will result in the follow regulated waste which must be disposed of in compliance with environmental regulations.



Spill:

In the event that a hazardous material spills during this procedure, be prepared to execute the emergency procedure below.


Instructions:


 

Contact Ying Qi or Justin Scanlon for training. For booking go here. You will need an MSE user account. Please fill out the MSE form in the attachments and bring the original copy when you come for your training. Fill out the user section and have your advisor fill out the section provided. An account shortcode and account contact will be required as well. ALL TRAINING MUST BE GIVEN BY MSE TECH STAFF.

 

Operation of the DSC 6
(Please see Ying Qi or Justin Scanlon for instruction before use)

  1. Make sure that the pump is submerged in water. Place ice from ice machine (also located in 2224 HH Dow) in the cooler with the pump and water. Plug in the cooling water pump.
  2. Turn on the gas tank.
  3. Click on the DSC 6 Icon under Pyris.
  4. If you need to run a background scan (only necessary daily, not for every sample) place an empty pan with lid on each side of the machine (in both the sample and reference holder). Make sure that you use forceps to remove the furnace lids and place them only on the metal ring surrounding the sample holder.
  5. On the outer window decide what temp. you want to start at and enter this value. Hit the "go to temp." button.
  6. Within the method editor (either the screen will be available or you will have to click on the icon in the upper left hand corner) several items need to be entered:
    • in the SAMPLE INFO window make sure that the "sample weight" item is ZERO, enter a filename for your background and any comments
    • in the INITIAL STATE window enter the initial temperature, initial Y (20 is fine) and purge gas is nitrogen at 20ml/min. Leave "baseline file" info blank for this run.
    • in the PROGRAM window design your run. Isothermal steps (hold for 1-5 minutes) and temperature scan steps (10 °/min. is good for up ramps, 40 °C/min. for down ramps)
    • click on END CONDITION
    • go to 30 °C is good, ignore box on bottom right
    • Push "start" – the icon on the outer window that shows a picture of the DSC with a scan in the background.
  7. The scan can be seen in "real time" in the INSTURMENT VIEWER and data analyzed in the DATA ANALYSIS package. (Both found in the upper left of the screen).
  8. After running a background scan you can now test your sample. While the background scan is running, prepare your sample and reference pan. Make sure to note the weight of your sample (without the pan).
  9. Remove the two DSC furnace lids using forceps. PLACE THESE ON THE METAL RING SURROUNDING THE SAMPLE HOLDER.
    Using forceps, place the sample (left) and reference pan (right) into the DSC. Replace the two furnace lids using forceps.
  10. Below the "go to temperature" button on the outer screen, type in the initial desired temperature. Hit the "go to temperature" button in order for your sample to equilibrate at that temperature while you are setting up the run.
  11. Within the method editor (either the screen will be available or you will have to click on the icon in the upper left hand corner) several items need to be entered:
  • in the SAMPLE INFO window enter the weight of your sample without the pan, enter a filename for your scan and any comments
  • in the INITIAL STATE window enter the initial temperature, initial Y (20 is fine) and purge gas is nitrogen at 20ml/min. Enter the baseline file that you will be using and check the box to subtract it from your data.
  • in the PROGRAM window design your run. Isothermal steps (hold for 1-5 minutes) and temperature scan steps (10 °/min. is good for up ramps, 40 °C/min. for down ramps)
  • click on END CONDITION
  • go to 30 °C is good, ignore box on bottom right
  • Push "start"
  • the icon on the outer window that shows a picture of the DSC with a scan in the background.
12.  After you are done please turn off the gas tank, unplug the circulating pump and remember to log your time into the logbook.

 

 

Instructions for the Perkin Elmer Auto Balance AD6 can be found on top of the scale.

 

Instructions used for MSE 365 are located here (pdf)


Equipment:


Last Revision:

Oct 01, 2020