Protocol Twin-Jet Set-Up
Carolina Garcia
July 11, 2009
Contents
1 Matrix Formation 2
2 Annealing process 4
3 Cleaning up 5
1
Chapter 1
Matrix Formation
1. Close the vacuum of the lines
2. Preparate the samples.
(a) Preparation of Ozone In lab the ozone if made from Oxygen (O2 )
and an electric discharge at the boiling point of Liquid Nitrogen
(N2 ) i.e. at a temperatur of 77K, the procedure is:
• open the sample container
• Be sure that you have enough N2 and prepare it the two
cylinders
• Put the electric discard wire inside the sample tube and one
cylinder under the sample tube.
• Be sure the black stuff is close enough to the cylinder1 and
under the cylinder border
• Fill that cylinder with N2 up its border
• Slowly open the Oxygen valvule until the desire inches (The
usual amount is 3 main lines)
• to start the Ozone creation turn on the voltage source
• The main gauge should decrease (lineally) as the Ozone is
produced.
(b) Preparation of 1,3 cyclohexadiene
• If it is the first time
• Use one of the cylinders
• Let the liquid sample to warm i.e. expand the molecules so
gas is produced
3. Measure the diseare amount of sample by open the can, open the
sample valvule and watching the gauge of the line to the desider value.
1
The end of the black stuff brings the electric discharge
2
4. Turn on the Cryostatic system!! not necessary and this point it could
be before.
• sing up in the paper
• open the water
• Turn on the refrigerator
5. Fill the rest of the Can with Ar. Open slowly the Ar valvule until 30
inches in the line gauge, close the Ar.
6. Close the can, to retain the sample.
7. Open the vacuum to clear the line remove the extra particles of Ar
8. At 200K take the Background Spectrum.
• In the program go to Instrument → Scan, and put the following
parameters
9. At 21K and after the Background collection is finished, start the de-
position. For both lines:
(a) Measure the rate of deposition
• open the can all the way
• when the gauge is steady, close the can
• open the line slowly to reach a rate of 1 in between 1 minute
12 second per minor line
(b) open the can all the way.
10. Take a spectrum every hour.
• Same procedure as Background spectrum, step 8
• For next spectrum the only change is the name of the file and in
the description the number of scan
11. After 20 hours close the line to stop deposition.
3
Chapter 2
Annealing process
Remember that you can not close the program Spectrum One during
the running of ab experiment
12. Turn on the heater to rise the temperature of the Matrix
13. Close to the desirer temperature turn off heater
14. When the matrix has th e lower temperature and it is steady it takes
time to solidify the matrix, take spectra
15. If the matrix did not evaporate you can rise the temperature again,
hence repeat procedure from step 12
4
Chapter 3
Cleaning up
16. Change the vacuum
17. Turn off Cryogen System
• sing up in the paper
• close the water
• Turn off the refrigerator
18. Turn on the Heater if you want a quickly warm up
19. Close to room temperature Turn off the Heater
20. When the temperature reader is steady at room temperature the cell
holder is ready to open
21. Hence, close the Vacuum!!
22. Open the Ozone line
23. Open the Ar valvule, this allow to move the spectrometer from the
cell holder
24. Close the Argon
25. Remove the spectrometer container
26. Use hexanol1 to clean the windows of the cell holder and the support
windows
27. Sometimes you have to put grease in the O-ring connection
28. Close the cell holder
1
The hexanol is going to evaporate
5
29. Open the initial vacuum
30. After 25 minutes change the vacuum to the Diffusion pump
31. Open the cans and the vacuum of every line
32. Let the system overnight to clean everything. And you can start again
from 1
