Temperature Control with Manual Proton Spectra

 

STATUS

NOT Finished yet... Dean W.

Written by Dean Waldow

Updated Nov. 16, 2013


Safety and Precautions!

  • MAKE SURE YOU CAREFULLY USE THE CERAMIC SPINNER!
  • Do NOT use the plastic spinner.
  • Make sure your sample tube is able to handle the high temperatures.
  • Make sure your sample will not undergo a phase change to a gas the temperatures you are interested in.
  • The upper limit is set to 105°C currently though higher temperatures are possible. Consult Dean Waldow, Craig Fyhle, or Neal Yakelis, if higher temperatures are needed.

Procedure:

To take a series of proton spectra as a function of temperature, you can use the following procedure.

Temperature control is handled by the EDTE function. 

> edte

You should likely tune the controller for your situation. There are configurations saved. Here is what worked well for 35°C to about 105°C.

First proton spectra, get the sample from the sample changer.

  >  sx 'sample number'

Then get ready to take the proton spectrum.

 > new

> rpar (then choose PROTON)

> atma

> lock (then choose your solvent)

> getprosol

Then when the sample is equilibrated issue the following:

 > rga

> zg 

when finished 

 > ft

> apk

then change set point to new temp and when equilibrated

 > new

> rga

> zg

when finished

 > ft

 apk

and repeat until finished.

Set temperature back to 23 °C and when sample is cooled then send the sample back to the sample changer.

sx  ej