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:
- Ensure that all connections of the instrument are properly connected.
- Ensure the sample compartment area is empty and the beam path is not obstructed.
- Go to the set-up and select instrument, verify or set the below-given setting (Table 1) as per requirement.
- Select ‘Setup Instrument Advanced’ and select ‘Apodization’ as ‘None’.
- Go to the ‘Setup Instrument Beam Path’ option and select “None’ from the filter wheel icon.
- Take background by keeping the scan type as ‘Background’.
- Verify the basic instrument setting and enter the performance verification parameter details in ‘Sample ID’ and ‘Description’.
- GO to the ‘Setup’ and then select ‘Peak Detection’ and enable ‘Basepoint’.
- Place the certified polystyrene film, in the sample holder in the sample compartment.
- Select the ‘Scan’ from the workspace menu.
- After the completion of scanning, spectra will be generated.
- To get the peak table, go to the ‘process’ menu and select ‘peak table’.
- 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).
Range | 4000 to 600cm-1 |
Scan Type | Sample |
Unit | Absorbance |
Scan Number | 16 |
Resolution | 4 cm-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:
- Ensure that all connections of the instrument are properly connected.
- Ensure the sample compartment area is empty and the beam path is not obstructed.
- Go to the set-up and select instrument, verify or set the below-given setting (Table 2) as per requirement.
- Follow the procedure given in the Resolution parameter form point no. 4 to 12
- 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 Type | Sample |
Unit | % T |
Scan Number | 16 |
Resolution | 4 cm-1 |
Acceptance Criteria:
Wavenumber (In cm-1) | Acceptable tolerance (In cm-1) |
906.6 | 905.6 – 907.6 |
1028.3 | 1027.3 – 1029.3 |
1154.5 | 1153.5 – 1155.5 |
1583.0 | 1582.0 – 1584.0 |
1601.2 | 1600.2 – 1602.2 |
1942.9 | 1941.9 – 1943.9 |
2849.5 | 2848.5 – 2850.5 |
3060.0 | 3059.0 – 3061.0 |
Calibration Frequency:
Frequency for Calibration of FTIR spectrophotometer is 6 month or major maintenance job is performed.
Also Read:
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- FAQ on FDA’s Data Integrity
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- Understand 14 ICH guidelines in short
- What is Form 482, 483 and 484?
- What are stability chambers in pharma?
- Correction, Corrective action and preventive action
Refer YT Channel: Pharmabeej