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Using Nicolet FTIR |
- Sign in on the log sheet, record you full name, Advisor's name,
the start time, and your Recharge #
- Log into your personal IR account, Launch Omnic E.S.P. 5.1
(double clicking the icon) on Desktop.
- Chose the DEFUALT TRANSMISSION from the Experiment
popup menu right below the top menu. All the parameters for routine FTIR
experiments are already set there.
Make sure: Sample chamber is empty, the door is closed and the shutters
to source and detector are open (down).
Cover the window in the sample port with the dark screen (if not
already in place, it can be found in top righthand draw of desk).
- Make sure in:
Collect > Experiment Setup >Bench
DETECTOR=DTGS KBr
BEAM-SPLITTER=KBr
Collect > Experiment Setup >Diagnostics
red interferogram should appear in window with Max: ~7.5 and Min.:
~-2.8 (Location around 1024). Otherwise hit Align…
button to optimize the intensities.
- If doing Align…, wait until the Align Bench comment
box has disappeared from the screen.
- Exit from the optical bench setup by pressing OK.
- Collect Spectrum
- Get background spectrum for each day used.
Purge chamber. Collect>Experiment Setup > Background
Handling (set 600 for Collect Background After). Wait for
about 2-5 minutes (same time to be used for sample); Then
Collect>Collect Background.
Note: CO2 should be visible at around 2300 wave # and
H2O should be visible at 1400 and 1800.
- Collect Sample. Place sample in chamber. Make sure
the target beam hits the sample and goes to receiver. Purge for the
the same amount of time as used above and acquire the same number of
scans using Collect>Collect Sample.
- To save data, highlight the data, i.e. click on the spectrum with
the left mouse button. The desired spectrum will turn red.
- Open: File>Save (change to your own directory, i.e. for
ABC the directory is c:\users\ABC, type in the name of file in File Name
box, keeping the .spa extension, i.e. data.spa, press OK).
- Or use Save As feature to save in CSV format that is accessible by
Excel and other programs.
- Open: File > Exit ( to quit ONMIC)
- Log Off your account: Click START in the top left corner of9
the screen and chose LOGOFF, then YES.
- Leave spectrometer with all sample chambers closed, and the
shutters open (down). Please put back, in the correct place, any
equipment that you have used. Don't leave samples in the lab.
- Complete the log sheet with your stop time and the actual time you
consumed. Include any problems that you have had with the instrument, and
if you solved these problems, how you did it.
Manual for FTIR and for the OMNIC software are very clear and in details,
and can be found in hardcopy on the bookshelf behind the lab door or through
online help. Please DON'T REMOVE ANY MANUALS or EQUIPMENT FROM THE IR/RAMAN
LAB. Thanks for your corporation.
Detector Options
Standard IR Detector
Near IR Detector
Far IR Detector
Photo Acoustic Detector. Kept in left hand desk drawer. Dave Margolese uses
it regularly.
ATR Accessory: Measure the reflected spectrum of liquid and solids without
special sample handling. Please contact Nomar Alcantar at x8407.
Make a pellet and use in beam path.
DRIFTS Cell. Reflection cell. ( In a Wood Box labeled DRA.)
*Load powder into call ( may have to add KBr.)
*Have to align 2 small mirrors every time.
*Harrick Cell is used with the DRIFTs Cell to control the atmosphere around
the sample.
Liquid Cell. Sample sandwiched between plates.
May have to vary the mix of KBr and sample to get good transparence. To
start try ~5 parts dry KBr and 1 part sample. Grind together in a mortar
with pestle.
Load into the press cell 1/3rd or 1/4th full. May want to pull a vacuum on
this to get water out.
Align this cell in the Carver Press and compress to about 10,000 PSI on the
press pressure gauge. (Do not exceed 12,000 PSI!) (Do not extend the
stroke of the press pass about 5 inches, use spacers if necessary.) Leave
under pressure for at least 2 minutes. The final pellet should be about 0.5
to 1 mm thick.
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