To lay down a procedure for operation and calibration of FTIR.
This procedure is applicable for procedure for operation and calibration of FTIR.
QC Officer/ QC Executive
- 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.
- > 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
- Operation Procedure:
- 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.
Trainer : Manager – Quality Control
Trainees : Staff of the QC departments
Master Copy : QA Department
Controlled Copy : QC Department
Display Copy : QC Department
|SOP||Standard Operating Procedure|
|Sr. No.||Serial Number|
|FTIR||Fourier transform Infrared|
- REVISION HISTORY OF CHANGE:
|Sr. No.||Date||Revision Details||Revision No.|