This document details the procedure for the Operation and Calibration of FTIR. It is the policy of XYZ Limited that the written procedure shall be followed for the operation and calibration of FTIR and its use monitored to ensure that the instrument gives consistently accurate and reproducible results in compliance with regulatory requirements.
This procedure is to be applied at the time
of the Operation and Calibration of FTIR.
RESPONSIBILITY & ACCOUNTABILITY
Persons along with their responsibilities
and accountabilities are given below:
Executive -Â Corporate Quality Assurance:- To prepare SOP.
Trainee Analyst/ Jr. Analyst/ Analyst/ Sr. Analyst:- To follow the SOP accordingly
Manager-Corporate Quality Assurance:-To ensure implementation of SOP.
Manager -Â Technical:-To ensure implementation of SOP.
FTIR Standard Operating Procedure
General Instructions
5.0.1Â Â Â Ensure that system is
initialized before operation.
5.0.2Â Â Â Ensure that KBr used
for sample preparation should be free from moisture.
5.0.3Â Â Â Pellet formation
should be thin and transmittance should not be less than 80%.
5.0.4Â Â Â Report any discrepancy
observed during operation and calibration of instrument to Section In-charge or
his representative for corrective and preventive action.
5.0.5Â Â Â Section In-charge or
his representative will take the necessary action and report the same to the Manager
– Quality Assurance.
5.0.6  Affix ‘Under Maintenance’
label on the FTIR
PRECAUTIONS FOR FTIR
Ensure that the instrument is clean and free from dust and kept
comfortably on a table & a proper stabilized supply of 220V.
Ensure that there is no vibration-forming device kept near to the
instrument.
Check the temperature and humidity of that area.
Never shut down the power of the instrument.
Avoid touching the KBr window or exposing it to moisture-containing
solvent. (As it can damage the KBr window permanently)
Please make sure that the desiccant indicator should be a dark blue color.
If it becomes pink change the desiccant packs immediately from the
desiccant compartment.
You can regenerate the packs by pulling them into the oven at 105°C for drying
5.1 PROCEDURE
(operation)
5.2.1Turn ‘ON’ the RESUME
switch followed by Power Switch when a beep is heard indicating the end of
initialization.
5.2.2 Switch on the computer attached to FTIR,
the system is set up window automatically.
5.2.3 Enter User Name and Password.
5.2.5 Again Double click the Icon Spectra measurement to perform the measurement. It displays the following Icons
          Menu                  Settings                      View                    Help
5.2.6Â Â Click settings will display Background Measurement.
5.2.7 Confirm that the sample holding cell
is empty, then execute (parameter + background) from the measure menu of the
spectra measurement program.
5.2.8 To analyze a sample in FTIR, it is converted in pellet by mixing it with Kbr
5.2.9 Set (Sample) in the(Y-axis) group to % T and (Background) to single.
5.2.10 Verify the Spectrum Profile on
(Background Preview). Click the OK button in the (Parameters/ Background
measurement) dialog box to start measurement  Â
5.2.11 Background Measurement is now completed.
Proceed to sample measurement
5.2.12 Sample measurement
5.2.13. Prepare
the sample as per the pharmacopeia instructions and place the sample in the sample
chamber.
5.2.14 Execute
(Parameter sample) from the (measure) menu of the spectra measurement program
5.2.15 Verify
the spectrum profile on (Sample Preview) and click the <OK> button when
OK to start measurement.
5.2.16 When
the measurement is completed, the spectra analysis program starts automatically
and this completes the sample measurement.
5.2.17 Saving a Spectrum Execute (Save as) from the (File) menu. Specify the file type as [Jasco Std (JSW)] from (list files of type)
5.2.18 Select
the destination directory and enter the file name. Click <OK> button.
This
completes the saving spectrum data in a file
Maintain Log Book of FTIR on XYZ/CQA/SOP-040/FR-01 LOGBOOK OF FTIRÂ (Appendix I)
5.3Â Calibration of FTIR as per USP
CALIBRATION
FREQUENCY: QUARTERLY
5.3.1Â Wave NUMBER Verification (USING
POLYSTYRENE FILM)
5.3.1.1 Operate the Instrument as per the operating procedure shown above.
5.3.1.2 Ensure that the instrument is clean and free from dust and kept comfortably on a table.
5.3.1.3 Ensure power supply 220 V.
5.3.1.4 Ensure that there is no
vibration-forming device kept near to the instrument.
5.3.1.5 Carry out a background as per
Operation of FTIR.
5.3.1.6 Now put polystyrene film 1.5 Mil in
sample compartment and click ok. After competition the scanning click Yes and
mark the peak from the Analyze menu and click the find peak, then verify the
Wave number.
                              3060.0 (+1.0)
cm¯1
                              2849.5 (+1.0)
cm¯1
                              1942.9 (+1.0)
cm¯1
                              1601.2 (+1.0)
cm¯1
                              1583.0 (+1.0)
cm¯1
                              1154.5 (+1.0)
cm¯1
                             1028.3 (+1.0)
cm¯1
5.3.1.7After Saving the calibration and
take the print from the file menu and click the Print options.
5.3.1.8Record the Calibration Data on APL/CQA/SOP-040/FR-02
Calibration Data Sheet (Appendix II)
5.3.2 RESOLUTION PERFORMANCE
5.3.2.1 Check the Resolution performance of the polystyrene film of thickness approximately 35µm, by clicking on ‘’zoom’’ and zooming in the area around 1500 cm-1  to 1600 cm-1  and with the use of the ‘cursor’ click on the peak at 1583±1.0 cm-1 and valley 1589±1.0 cm-1. Again, zoom in area 2900 to 2800 and with the use of cursor click peak 2849.5±1.0 cm-1 and valley on 2870±1.0 cm-1.
5.3.2.2 Find out the difference of Transmittance
between the depth of the trough from the minimum transmission at 1589±1.0 cm-1 to maximum transmission at 1583±1.0 cm-1.
Acceptance criteria: The difference should be greater than 10%Transmittance.
5.3.2.3 Find
out the difference of Transmittance between the depth of the trough from the
minimum transmission at 2870 ±1.0 cm-1 to maximum transmission at 2849.5±1.0 cm-1
Acceptance criteria: The difference should be greater
than 18%Transmittance
Note:Â Note down the values from the screen only as printouts are not possible for the same
5.4 GENERATION OF INSTRUMENT CALIBRATION NUMBER
Generate Instrument Calibration number on the calibration data sheet as INSCALXXYYZZZ. Where INS denotes Instrument, CAL denotes Calibration. XX denotes the year, YY denotes Month ZZZ denotes sequence number.
5.5Â ABBREVIATIONS
INS CAL: Instrument Calibration
Download:- Logbook and AppendixÂ
