SOP for Calibration of Shimadzu IR Spirit-X FTIR Spectrophotometer

PURPOSE

To lay down a procedure for the Calibration of the FTIR Spectrophotometer, Model: IRSpirit-X, Make: Shimadzu

SCOPE

This SOP applies to the Calibration of the FTIR spectrophotometer, with the model IRSpirit-X and the make Shimadzu.

RESPONSIBILITY

• QC Analyst: Calibration of an instrument as per SOP.
• Senior Analyst: Reviewing of recorded data and implementation of the SOP.
• Manager QAD/QCD: Approval and responsible for implementing the SOP.

PROCEDURE

Handling of polystyrene film

• Polystyrene film thickness should be approximately 35µm.
• Ensure that the polystyrene film is within its validity.
• After completion of calibration store the polystyrene film in a self-sealed polyethylene bag/ box and keep it in a desiccator.
• Label the polystyrene film with the following information from its certificate of analysis.

Polystyrene film
Lot No.
Calibrated on
Valid till
Sign & Date

Calibration Procedure

FTIR is calibrated by using polystyrene film for the following parameters,

1. Verification of wave number accuracy.
2. Control of Resolution performance of the instrument.

• Click on the ‘Macro’ tab in the LabSolutions IR launcher, following window appears.

• Click on ‘JP Validation’, and the following screen appears.

• Click on ‘Run’, the following screen will appear.

• Select ‘Measurement’, and the following screen appears.

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• Set the parameters as follows:

• Click on ‘OK’, and the following screen appears.

• Click on ‘OK’.
• After the power spectrum measurement, the following screen appears.

• Put the polystyrene film in the sample compartment and click on ‘OK’.
• When the measurement is finished the calculation for inspection is done automatically. The validation program inspects 5 tests. When all tests pass, the validation is passed. The judgment dialog box shows ‘Pass’ and a validation report is printed out.
• Then close the program by clicking on ‘close’ / ‘Program end’.
• Repeat the same procedure for ‘EP Validation’.
• The spectrum shall give the wave number accuracy at the wavelength mentioned below. Record the observation in the Calibration report as per ‘CALIBRATION REPORT OF FTIR SPECTROPHOTOMETER’ Annexure 01.

ALSO READ: SOP for Calibration of Shimadzu IR Affinity-1S FTIR

• Similarly, check the performance of ATR (Attenuated Total Reflection) mode by selecting ‘ATR’ in the EP Validation parameter setting.
• Acceptance criteria: The wave number accuracy obtained with the polystyrene film shall be within the range specified in the Calibration compilation report as per ‘Calibration Compilation Report for FTIR’.
• Verification of Wave Number for Transmission mode as per the following table.

Wave Number	Tolerance Limit	Acceptance Criteria
3060.0	± 1.0 cm-1	3059.0 – 3061.0
2849.5		2848.5 – 2850.5
1942.9		1941.9 – 1943.9
1601.2		1600.2 – 1602.2
1583.0		1582.0 -1584.0
1154.5		1153.5 – 1155.5
1028.3		1027.3 – 1029.3
906.6		905.6 – 907.6

• Verification of Wave Number for ATR mode as per the following table.

Wave Number	Tolerance Limit	Acceptance Criteria
3059.7	± 1.0 cm-1	3058.7 – 3060.7
1601.0		1600.0 – 1602.0
1027.7		1026.7 – 1028.7
906.1		905.1 – 907.1

• Control of Resolution Parameter by Absorbance as per the following table.

Absorbance difference between (cm-1)	Tolerance Limit
2870.0 – 2849.5	NLT 0.33 ABS
1589.0 – 1583.0	NLT 0.08 ABS

• Frequency of Calibration: Once in 6 months or after any major maintenance job.
• Calibrate the instrument on or before the calibration due date.
• After completion of the calibration activity, affix the calibration status label on the instrument.
• If any calibration result is found to not meet the acceptance criteria specified in SOP, this shall be considered out of calibration.
• If calibration complies, update an instrument's current calibration status label with all relevant details indicating the calibration status as ‘PASSED’.

ANNEXURES

Calibration Report for FTIR Spectrophotometer

REVISION HISTORY

Nil

ALSO READ: SOP for Operation of Shimadzu IRSpirit-X FTIR Spectrophotometer