SOP for Operation & Calibration of FTIR

1. OBJECTIVE:

To lay down a procedure for operation and calibration of FTIR.

• SCOPE:

This procedure is applicable for procedure for operation and calibration of FTIR.

• RESPONSIBILITY:

QC Officer/ QC Executive

• ACCOUNTABILITY:

QC Manager.

• PROCEDURE:
  • Operation Procedure:
    • Login to the computer using your ID and password.
    • Turn on the FTIR machine (the power button is in the front)
    • Start software. Start
    • A window may pop up asking to remove marked data. Click yes.
    • Another window may pop up saying “Autoadjust required. Perform autoadjust now?” Click yes.
    • This may take several minutes
    • On the top toolbar, click on Measurement –EasyScan
    • A window will pop up with some options. Typically nothing needs to be adjusted, but you can select the range of wavenumbers scanned (in cm-1).
    • Name the data file and add any comments. Then click ok.
    • It will ask to execute BKG (background) measurement. Click yes.
    • It will ask to execute BKG measurement again. Click no.
    • Now it is time to place the sample in front of the beam. There is a triangular sample holder that can be used. Tape can also be used to hold the sample in front of the beam. (The beam is red; make sure it is going through the part you want to test).
    • Once the sample is in place, close the chamber and click ok.
    • The spectrum will be acquired.
    • It will ask “Are you all right?” Click ok.
    • Save the XPS file if desired. It contains the spectrum and lists peaks in a table.
    • Now, you can export the data to a text file for use in Excel or other software if desired.
    • File
    • > Export. Save as (ASCII) which will make a .txt file.
    • See the figure below to see what the screen should look like.
    • A peak or spectrum search can now be performed by clicking on search.
    • a. It is recommended to try both as one may find a better match than the other.
    • The Y-Axis can be changed to absorbance or % transmission by clicking Graph > Y-axis mode – > Tra or Abs
    • The blue –red = green button (circled in the image below) will put both the acquired spectrum and the matched spectrum on the same graph.
    • The matched spectra will be given a score out of 1000 on how well it matches the acquired spectra.
    • When finished
    • Close the software
    • Remove the sample and wash with methanol by tissue papar.
    • Turn off the power
    • Log off

• Calibration Procedure:
• Operate the instrument as per its standard operating procedure.
• Ensure that before performing the calibration instrument is clean.
• Use reference standard polystyrene film for calibration along with its certificate traceable to NIST (5) standards.       
•  Thickness of the polystyrene film is 38 µ (micron) or 0.038 mm.
• Polystyrene film used for calibration of FTIR because it shows absorption bands covers the complete range of IR region.
• Polystyrene film is made up of polymers of styrene and stable at any temperature and highly durable.
• Set the polystyrene film in a sample chamber of an instrument and set the instrument parameters as mentioned below :

Resolution : 2 cm-1

Measurement mode : % transmittance & ratio

No. of scans : 1 to 20

Scanning range : 4000 to 400 cm-1 or as per requirement.

• Verification of the wave number scale:
• The wave-number scale may be verified using a calibrated polystyrene film, which has transmission minima (absorption maxima) at   the wave numbers (in cm^–1) shown in below:

Standard wave number ( cm^-1)       Tolerance

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

• Control of resolution performance: Record the spectrum of a polystyrene film approximately 35 µm in thickness. The difference  between the percentage transmittance at the transmission maximum A at 2870  cm^-1 (3.48 µm) and that at the transmission minimum B at 2849.5 cm^-1 (3.51 µm)  must be greater than 18. The difference between the percentage transmittance at  the transmission maximum C at 1589 cm^-1 (6.29 µm) and that at the transmission  minimum D at 1583 cm^-1 (6.32 µm) must be greater than 10.After calibration, affix the label” CALIBRATED” on the instrument.Frequency of calibration is in every three month.
• TRAINING:

Trainer   : Manager – Quality Control

Trainees : Staff of the QC departments

• DISTRIBUTION:

Master Copy                  :           QA Department

Controlled Copy            :           QC Department

Display Copy                 :           QC Department

• ATTACHMENTS:

NA

• REFERENCES:

In-House

1. ABBREVIATIONS:

Abbreviations	Extended Form
SOP	Standard Operating Procedure
NA	Not Applicable
QC	Quality Control
Sr. No.	Serial Number
QA	Quality Assurance
DEPT.	Department
FTIR	Fourier transform Infrared

1. REVISION HISTORY OF CHANGE:

Sr. No.	Date	Revision Details	Revision No.
01	17/01/2020	NEW SOP	00