Calibration of FTIR

PROCEDURE :
PRECAUTIONS:
Place the instrument as far as possible away from any strong magnetic or electric field or any electrical appliances generating a high frequency.
Avoid placing it where severe vibrations exist.
Place the instrument free from dust and corrosive gases.
To extend the life of the source lamp, have them powered only when required.
OPERATION:
The operations of Keys are as follows :
Switch on the main and then switch on the power supply of FTIR.
LED will glow with middle one will blinking, wait till all will continuous green.
Switch on the PC.
Open the software.
Click on connect to instrument,
Check all parameters like Acquisition, parameter. Resolution                        4 Scan                                16 Measurement                    1 Interval                              0 min. Acquisition mode                                          Single beam (for reference) Transmittance (for sample) Display full spectral range unclick Start wavelength           600 Stop wavelength           4000 Reference files              Default Detector parameter (optimum) 81 [Check the single strength in the range of 25 to 85 %]0 Data saving parameter Sample name                Default Generic name                Default Current name                Default Show sample name    Click Save to Project           Click Project                         Select appropriate project.
Clean the ‘Miracle’ surface with isopropyl alcohol; also clean the pressure tips of ‘Miracle’ with cotton swab of isopropyl alcohol.
To create project, go to project, click on new project, enter the project name then click on save.
For Reference: Change the Acquisition mode for single beam.
Click on the reference.
Wait till remaining time complete, after finishing reference it will show measure on left down corner of the monitor, as measurement finished.
For Sample: Change the Acquisition mode to transmittance.
Put the sample in mounting ring.
If the sample is volatile, put the volatile cover.
Rotate the pressure clamp till one click.
Click on measure.
After completion of measurement, monitors shows message enter object information.
Change Standard/Sample with your Standard/Sample name then click on OK.
For comparing two spectra, open two spectra which are to compare
For opening spectra go to file then open the respective file, and then double click on spectra.
Click on merge view.
Right click on the spectra.
Go to  set visible area – x axis and put the 2000 to 600 range and click OK.
For peak peaking go to mathematics and click on pick picking & click on calculate.
Printing : Open the spectra which is to be printed, then click on file, click  on print preview then click on print icon.
CALIBRATION:
Change the assembly for calibration instead of assembly for analysis for the calibration.
Handle the calibration assembly very carefully.
Handle the polystyrene film very gently and avoid direct contact to the film.
Verification of Wave Number Scale :
Measure the spectrum of polystyrene film 4000 cm-1 to 650 cm-1 after the routine Background correction.
Following bands should appear at the frequencies indicated below and
should not deviate from the designated frequency by more than the  tolerance indicated.
Sr. No. Wave-number (cm-1) Acceptable Tolerance (cm-1) 01. 3060.0    ± 1.0 3059.0 –3061.0 02. 2849.5    ± 1.0 2848.5 – 2850.5 03. 1942.9    ± 1.0 1941.9 – 1943.9 04. 1601.2    ± 1.0 1600.2 – 1602.2 05. 1583.0    ±  1.0 1582.0 –1584.0 06. 1154.5     ± 1.0   1153.5 – 1155.5 07. 1028.3    ±  1.0 1027.3 – 1029.3
Control of Resolution Performance:
Expand the recorded polystyrene spectrum in the region 3200 cm-1 to 2600 cm-1.
Note down the absorption at wave numbers 2870 cm-1 (tolerance ± 1 cm-1)
and 2849.5 cm-1  (tolerance ± 1 cm-1).
The  difference of between the absorbances at the absorption minimum at
2870 cm-1 and absorption maximum at 2849.5 cm-1  should be greater than 0.33.
Expand the polystyrene spectrum in the wave number region 1800 cm-1 to 1400 cm-1.
Note down the absorption at wave numbers the difference the absorption
at 1583 cm-1 (tolerance ± 1 cm-1) and 1589 cm-1 (tolerance ± 1 cm-1).
The difference of between the absorbances at the absorption maximum at
1583 cm-1 and the absorption minimum at 1589 cm-1  should be greater  than 0.08.