Manual for Netzsch DSC 214 Polyma

Password computer: LatitudeE5550

Open shortcut «DSC 214 Polyma»

Check which gases in indicated in the program

“MFC Gas extended”
Purge 1 synthetic air (normally 30ml/min)
Purge 2 nitrogen (normally 40 ml/min)
Protective gas nitrogen (normally 60 ml/min)

Do NOT exceed 0,5 BAR pressure on gas out from the wall!!!! With a higher pressure, the valves in the gas flow box will be broken.

Prepare your sample(s) by:

  • Weigh the crucible and lid empty (remember not to touch the lid and crucible with your fingers – use a tweezer)
  • Fill in your sample in the crucible (10-20 mg) and weigh it with 3 decimals accuracy.
  • If you want to use a closed crucible, close the crucible by using the pressing tool
  • Remember not to fill the crucible with too much powder. If there is a lot of gas evaporating from the sample during the analysis, the crucible can burst from the pressure.
  • If you have samples you know will evolve a lot of gas, you can either run the sample with an open crucible or use a pierced lid.


How to program an analysis:

Open Method – Create new method

(Alternatively, open a previous one if you want to use the same temperature program and conditions as for samples you have run before)

 

Setup:

  • Select correct crucible type
    For ordinary samples in aluminum crucible with lid – choose “Concavus Pan, closed (610 degrees)”
  • If you want to run a sample without lid – choose “Concavus Pan, open (610 degrees)”
  • For references or if you use pierced lids – choose “Concavus Pan, pierced lid (610 degrees)”

 

Header:

  • Choose measurement type (correction is only used for CP measurements)
  • Write in your project number
  • Write in your name (operator)
  • Write in which material or composition you are running the analysis on
  • Write in the crucible and lid mass.
  • Check gases

Temperature program:

Create your own program

  • Step 1 is the starting conditions: check the starting temperature for the instrument indicated in the software, mark in the gases you want to use and fill in the flow/min. Purge 1 synthetic air (normally 30ml/min), Purge 2 nitrogen (normally 40 ml/min), Protective gas nitrogen (normally 60 ml/min)
  • When you are finished press “Add”
  • Add the steps you need
    • End temperature – The temperature (T)  you want to go up to. Maximum T is 600 degrees.
    • Heating rate is normally 10K/min
    • Aquistion rate will come up automatically
    • Dynamic step – heating or cooling step
    • Isothermal step – dwell time
    • Final step – the program will automatically add 10 degrees more than the highest T in the program. (If the T goes above this temperature, the instrument will cut of the power to the heating, preventing the heating elements to be destroyed)
    • Take out the marking of the gas flow in the Final step, then you will not use more gas than necessary

Calibrations

  • Will not be used

 

Press Forward. Write in the file name for your method, press Save

 

To load your sample or samples:

  • Open autosampler and press Start
  • Click on Position 1, and define step . Open the method you want to use, fill in what material you are analyzing, the identity (what material or sample), name and mass of the sample. Give it a filename and save the analysis file in your folder.
    Repeat this procedure if you have several samples, starting with the next sample in position 2. Please remember to give this sample a different filename.
    Press OK when you are finished filling in information about the samples you want to run.

 

 

  • Position 0 is the empty reference crucible with mass 51,85mg. This crucible is already inside the instrument and shall not be taken out. The reference is placed on the left side of the platform.
    If you are doing CP measurements, it is important that the reference crucible is the same type as the sample crucible you are using. That is if you are running analysis with an open crucible, the reference crucible should be open. In addition, it should be closed if the sample crucible is closed.
  • When you have filled in information about the samples you want to run, press Start and then OK, and the instrument will start the analysis. The instrument will first check if the reference crucible is inside the furnace, check that the information about the reference crucible is correct when the message window appears, and then press OK
  • When your analysis is done, stop auto measurements, and press NO
  • Remember to turn the gas off when you are finished with the analysis, and take your samples with you.

 

If there is something wrong with the autosampler, press the emergency button on top of the furnace. This will stop the robot immediately. Contact the apparatus responsible person.

If you want to stop your measurement, go into the program and press stop measurement .

How to take out your data

  • Open Proteus
  • File- open
  • Look up your data file
  • Mark the red temperature curve
  • Go in to Extras in the menu. And open Export Data
  • Mark in Single point, full range
  • Check that the file is defined as an Ascii file, Column should be Tab and decimal symbols should be Comma.
  • Press Export , find your memory stick and save the file
  • If you want to save the curves, go in to File in the menu, choose Print analysis to pdf