SOP For FTIR

FTIR Spectrometer

Standard Operating Procedure (SOP) for Operation, Calibration, Cleaning, and Maintenance of FTIR (Fourier Transform Infrared Spectrometer).

Procedure for Operation and Calibration of FTIR

1.0   PURPOSE:

  • The purpose of this Standard Operating Procedure (SOP) is to describe the start-up, operation, calibration, and maintenance procedure of the FTIR – Fourier Transform Infrared Spectrophotometer.

2.0   SCOPE:

  • This SOP is applicable to the Shimadzu make and model IRAffinity-1 FTIR- Fourier Transform Infrared Spectrometer of the quality control department at the pharmaceutical drug manufacturing plant.

3.0   REFERENCES:

  • Instrument manual of Fourier Transform Infrared Spectrophotometer (FTIR).
  • SOP for Handling of out of Calibration results (OOC)
  • SOP for Analytical Instrument Qualification.
  • European Pharmacopoeia
  1. SOP for -Instrument/Equipment usage log book.
  • SOP for –Maintenance of Laboratory Instruments.

4.0   RESPONSIBILITY & ABBREVIATIONS

  • The Analyst shall be responsible for the operate the instrument as per SOP,
  • Calibrate the instrument as per SOP and Recording all the document related to the operation, calibration, and maintenance.
  • Quality Control Head or Designee shall be responsible for give training to all the concerned persons before the implementation of SOP,
  • To ensure proper documentation as per SOP and initiate the maintenance activity white breakdown.
  • QA shall be responsible for check and ensure the implementation of the system as per SOP.
  • Quality Head and Plant Head shall be responsible for the review, approve the SOP.
  • ABBREVIATIONS:
  • FTIR: Fourier Transform Infrared Spectrophotometer.
  • KBr: Potassium Bromide
  • NA: Not Applicable
  • QA: Quality Assurance
  • QC: Quality Control
  • SOP: Standard Operating Procedure

4.0   PROCEDURE FOR OPERATION AND CALIBRATION OF FTIR:

  • Startup of FTIR Software
  • Clean the Instrument and surroundings.
  • Connect the instrument with the power supply.
  • Switch on the instrument and Computer system.
  • Double click on “IR Solution” Icon.
  • After No. of internal operation.
  • Select the “Measure” and select Measurement from the main menu, further select “ initialize” from the measurement tab.
  • Press “Yes” then following screen will appear:
  • Select File to load standard method for analysis or fill the desired parameter of the method.
  • Click on file,
  • Select the above option to enter the main window and select the standard method for analysis or prepare new method as per STP.
  • After selecting the standard method, double click on method or Open it from main window. A dialog box will appear and ask about downloading parameter of Method.
  • Press “OK” to download the method parameters
  • After completion of method downloading,
  • Click on “BKG” for background correction. A dialog box will appear.
  • Press “OK” if the Sample compartment is ready for Background.
  • Select measure from the above screen window, fill all the required (sample/standards information) in comment/Date file and select sample for sample analysis.
  • For the Sample Analysis click on the Data path file and give the appropriate file path for saving the data.
  • Copy the file name and paste the data in the comment and click on the sample tab.
  • After scanning the sample click on “Calculate” and then “OK” on the Peak Table.
  • The number of peaks in the Peak Table must be between 15 to 25.
  • To adjust the number of peaks click on “Calculate” and then increase or decrease the “Min Area” and then click on “OK”.
  • Click on “Window” from the main menu bar and select “Join Visible”.
  • Then click on “Manupulation 2” and select Purity.
  • Rightclick on the sample and select send to source similarly right click on the reference and select send to reference.
  • Send to reference
  • Click on “Calc”, then “OK”, select the print command from the main window.
  • Click on “OK” and select the desired report template for the Peak purity Graph as shown bellow.
  • Select the Report format and click on “Open” or double click on Report format. Press ‘OK’ for printing the document.
  • For Peak table : select the Manipulation 1 and select Peak table.
  • After selecting the peak table,
  • Click on “Calc” then “OK”.
  • Select “Print” from the above screen.
  • Select the report format as ‘peak table’ and print. As per the above described procedure.
  • Sample Preparation for FTIR Analysis:
  • Sample Preparation for solid Sample for FTIR Spectrometer:
  • Dry the KBr (Potassium Bromide –IR Spectroscopy grade) at 105°c for about 1 hour, cool it in the desiccator before use.
  • Crush the dried KBr in mortar.
  • Clean the sample holder with carbon tetrachloride or acetone to remove grease.
  • Take crushed KBr in the  “Sample Cup” and plain the surface by using sample-pressing bar.
  • Clean the excess powder that fall on the sides of the sample cup using a tissue paper and put the cup on “Sample Cup Holder” in the sample compartment of the instrument.
  • Take the background IR.
  • Weigh about 300 mg of previously dried KBr and transfer it to a clean mortar.
  • Weigh about 2 to 4 mg of previously dried sample or as per the specified specification (to make sample concentration about 1.0% w/w) and transfer to the mortar, which contained the KBr.
  • Mix the sample with KBr for homogeneous.
  • Use this sample for the sample spectrum.
  • Sample preparation (For Liquid sample) for FTIR Spectrometer:
  • Select fixed thickness cell as per the requirement or use sodium chloride cell.
  • Put the cell in cassette and take the background (Air background) or as per the requirement.
  • Suck up the liquid sample by syringe.
  • Inject the liquid sample into the cell through the one hole of cell until the liquid came out from another hole of cell and become a thin film and insert the plugin both the holes.
  • Clean the cell with tissue paper.
  • Use this sample for sample spectrum.
  • Sample Preparations – Films.
  • Use this technique for liquids or semisolids or low melting solids.
  • Put the cell in cassette and take the background (Air background) or as per the
  • A thin film can be made by dissolving a semisolid or a highly viscous liquid (such as polymers) in a minimum volume of a volatile solvent (such as chloroform, carbon tetrachloride) or the sample can be taken as such.
  • Using a clean glass capillary, place a drop or a small portion of the sample onto a clean sodium chloride cell.
  • Hold the other sodium chloride cell’s edge on the top of the sample and slide horizontally applying slight pressure so as to form a thin film on the cell.
  • In case film is to be made with a solution, evaporate the solvent to dryness using a hot air gun. Align the cell edges and assemble the two sodium chloride cells.
  • Run a Background Scan as an air blank
  • Cut the film cassette size and insert a cassette.
  • Use this sample for the sample spectrum.
  • If the sample preparation is specified in the STP/ATP or individuals monograph follow the same.
  • Calibration (Verification of the wave-number scale) of FTIR Spectrometer:
  • Follow the operational procedure and record the Spectrum of the Polystyrene film over the range of 3800 cm-1 to 650 cm-1.
  • Record the wave number in attachment no. 01.
  • The spectrum should show the Transmission minima (absorption maxima) at the wave-number given in the attachment no. 01.
  • Frequency: (Monthly± 3 days)
  • Validation Procedure of FTIR Spectrometer:
  • Ensure that, the instrument is ready for calibration and the start-up procedure is followed.
  • Calibrate the instrument for power spectrum, resolution, wave number accuracy, repeatability of wave-number and repeatability of absorbance.
  • Ensure that the Instrument is ready for the calibration and start-up the procedure is followed.
  • Initialized the instrument.
  • Click on the icon Measurement, select “EP5.0 validation”.
  • After selecting “EP 5.0 validation”.
  • Click on “Measurement”.
  • Verify the necessary information or change the details as per requirements.
  • Click on “OK” to start the background.
  • After background validation completion,“ Set polystyrene film into the sample chamber” is displayed in the screen.
  • Set the polystyrene film accordingly and click on “OK”, scanning will start.
  • After completion of the validation the report will be generated and printed automatically.
  • Compare the results for its compliance against limits given in validation format and put remark regarding validation status.
  • Make entry of the usage into the Instrument usage logbook.
  • Calibration report shall come in form of validation format at the time of printing.( Annexure-2)
  • File the validation report duly signed and checked.
  • Affix calibration label on the instrument.
  • Frequency: Monthly ± 3 days
  • Precautions/Maintenance Program of FTIR Spectrometer:
  • Precautions during FTIR Calibration :
  • Use only spectroscopic grade KBr for the sample preparation and store a dry box.
  • Clean and dry mortar and pestle immediately after the usage.
  • Check silica bag of the dry box as well as sample compartment for its effectiveness.
  • When not in use Polystyrene film should be kept in its accompanying protective cover.
  • The exposed film surface should never be touched by fingers or any other objects and Dust should be removed by blowing with clean and dry air.
  • Breakdown Maintenance of FTIR Spectrometer :
  • Put “UNDER MAINTENANCE” label on the instrument when it is under breakdown maintenance / not functioning and intimate to Head quality or designer.
  • Head quality or desginee informs to the Instrument service engineer or Utility dept.
  • Keep instrument UNDER MAINTENANCE between breakdown and service period.
  • After maintenance, calibrate the instrument to check its satisfactory functioning and record the readings. (Note: Calibrate the instrument as per the calibration schedule, this calibration is additional)
  • Retain service report copy attached in the Instrument Maintenance History File.

5.0   ANNEXURES – SOP OF FTIR SPECTROMETER:

Annexure 1: FTIR Calibration Record.

Instrument Name: FTIR
Instrument NoMake/Model
LocationCalibration frequencyMonthly±3 days
Calibrated onNext calibration due on
Sr.NoDateTransmission minimum/absorption maximum (cm-1)Observed wave number (cm-1)Calibrated byChecked byRemarks
3059-3061
2848.5-2850.5
1941.9-1943.9
1600.2-1602.2
1582.0-1584.0
1153.5-1155.5
1027.3-1029.3

Annexure 2: FTIR Validation Record.

Instrument Name: FTIR
Instrument NoMake/Model
LocationCalibration frequencyMonthly±3 days
Calibrated onNext calibration due on
1. Power Spectrum3. Wave Number Accuracy
Wave numberMeasuredStandard Not less thanWave numberMeasuredErrorTolerance
4600.03060.0±1 cm-1
4000.02849.5±1 cm-1
3000.01942.9±1 cm-1
At maximum1601.2±1 cm-1
700.01583.0±1 cm-1
500.01154.5±1 cm-1
403.01028.3±1 cm-1
351.0
2. Resolution4. Repeatability of Wave Number
Wave numberMeasuredStandardWave numberNo.1No.2ErrorTolerance
Between 2870.0-2850.0Greater than 0.332849.5±5 cm-1
1601.2±1 cm-1
Between 1589.0-1583.0Greater than 0.081028.3±1 cm-1
5.Repeatability of absorbance :
Wave numberNo.1No.2ErrorTolerance
2849.5±0.03%
1601.2±0.05%
1028.3±0.03%

Remark: The instrument is calibrated & qualified / Out of calibration & not qualified for use.

Calibration : Scheduled/Not scheduled (Reason : _________________________)
Done By: Date :Checked By: Date :Approved By: Date:

Annexure 3: Calibration Status label.

Quality Control

CALIBRATION STATUS

INSTRUMENT:

MAKE: 

MODEL  :

CALIBRATION ON :

CALIBRATION BY :

NEXT CALIBRATION DUE ON :