How to do Calibration of FTIR Spectrophotometer?

FITR is one of the instrument used in pharmaceuticals for the identification of the material.

Here is the procedure for Calibration of FTIR spectrophotometer in pharmaceuticals.

Calibration Of FTIR Spectrophotometer:

Calibration of FTIR spectrophotometer can be performed through two parameters: 1. Resolution and 2. Accuracy of wavenumber

Resolution:

  1. Ensure that all connections of the instrument are properly connected.
  2. Ensure the sample compartment area is empty and the beam path is not obstructed.
  3. Go to the set-up and select instrument, verify or set the below-given setting (Table 1) as per requirement.
  4. Select ‘Setup Instrument Advanced’ and select ‘Apodization’ as ‘None’.
  5. Go to the ‘Setup Instrument Beam Path’ option and select “None’ from the filter wheel icon.
  6. Take background by keeping the scan type as ‘Background’.
  7. Verify the basic instrument setting and enter the performance verification parameter details in ‘Sample ID’ and ‘Description’.
  8. GO to the ‘Setup’ and then select ‘Peak Detection’ and enable ‘Basepoint’.
  9. Place the certified polystyrene film, in the sample holder in the sample compartment.
  10. Select the ‘Scan’ from the workspace menu.
  11. After the completion of scanning, spectra will be generated.
  12. To get the peak table, go to the ‘process’ menu and select ‘peak table’.
  13. Record the difference between the absorbance values at the absorption minimum at 2870 cm-1 (A) and the absorption maximum of 2849.5 cm-1 (B), and the difference between the absorption values, and absorption minimum at 1589 cm-1 (C) and absorption maximum at 1583 cm-1 (D).
Range4000 to 600cm-1
Scan TypeSample
UnitAbsorbance
Scan Number16
Resolution4 cm-1
Calibration of FTIR spectrophotometer: Table 1

Acceptance Criteria: The difference between A and B should be greater than 0.33 and the difference between C and D should be greater than 0.08.

Accuracy of Wavenumber:

  1. Ensure that all connections of the instrument are properly connected.
  2. Ensure the sample compartment area is empty and the beam path is not obstructed.
  3. Go to the set-up and select instrument, verify or set the below-given setting (Table 2) as per requirement.
  4. Follow the procedure given in the Resolution parameter form point no. 4 to 12
  5. After completion of the test, verify the test results for transmission minima (absorption maxima) at the required wave number ( in cm-1) against acceptable tolerance (in cm-1).
Range 4000 to 600 cm-1
Scan TypeSample
Unit% T
Scan Number16
Resolution4 cm-1
Calibration of FTIR spectrophotometer: Table 2

Acceptance Criteria:

Wavenumber (In cm-1)Acceptable tolerance (In cm-1)
906.6905.6 – 907.6
1028.31027.3 – 1029.3
1154.51153.5 – 1155.5
1583.01582.0 – 1584.0
1601.2 1600.2 – 1602.2
1942.91941.9 – 1943.9
2849.52848.5 – 2850.5
3060.03059.0 – 3061.0
Calibration of FTIR Spectrophotometer
FTIR spectrophotometer

Calibration Frequency:

Frequency for Calibration of FTIR spectrophotometer is 6 month or major maintenance job is performed.

FTIR Talk Letter by Shimadzu

Also Read:

Refer YT Channel: Pharmabeej

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