Monday, December 13, 2010

Operation And Calibration Of Fourier Transform Infrared Spectrophotometer (Ftir

1.0.            OBJECTIVE:

The objective of this SOP is:
1.1               To ensure that the FTIR performs satisfactorily and gives accurate and reproducible data. 

2.0.            RESPONSIBILITY:

2.1               The Officer - Quality Control shall be: 

2.1.1.        Responsible for operating the FTIR as per the SOP.
2.1.2.        Responsible for timely calibration of FTIR System as per the SOP.

2.2               The Executive - Quality Control shall be:

2.2.1          Responsible for ensuring the adherence of SOP.

3.0.            ACCOUNTABILITY:
          
Head - Quality Control

4.0.            PROCEDURE:

4.1              OPERATING PROCEDURE:

Ø      Check the cleanliness of sample chamber
Ø      Check the condition of bags of Silica granules
Ø      Turn the power switch of F.T.I.R.- 8300 `ON’
Ø      ON Online computer system display on screen FTIR 8300.
Ø      Double click FTIR 8300. Loading is start wait till loading. After loading is complete Hyper IR is display on screen click OK wait till the instrument starts initialization, and displays ‘Normal’ if the initialization is OK online FTIR is activated click maxima Shimadzu FTIR 8000 SCSI (default) screen on.
Ø      After initialization main menu is displayed; wait for 30 min. to stabilize the system.
Ø      SPECTRUM MEASUREMENT
Ø      Measurement menu displayed on screen
Ø      Press `MEASUREMENT’ mode
Ø      Measurement screen (Spectrum) displayed on it.
Ø      In measuring mode click T% or as per specified monogram.
Ø      Set parameters in help of crusher.
Ø      Click BKG start. Scanning “MEASURE BKG’. Wait till window on the screen disappears.
Ø      After ‘Bkg scan’, put the sample disk in the sample chamber, with the help of sample holder and close the chamber immediately.
Ø      Click sample start for ‘measure sample’
Ø      Wait for scanning, till the window on screen disappears and actual sample IR scan displayed.
Ø      Compare the Spectrum by help of menu bar in computer screen (PEAK TABLE)
Ø      If comparison with standard and sample then click file and open file as required. Then by help of menu-bar click joined visible.
Ø      For printing of spectrum click file go with print desk for adjustment of graph
Ø      Record all analysis in log book

4.2              Calibration of F.T.I.R
Ø      Scan the polystyrene film (0.05 mm) and go to menu
Ø      Select ‘Data Processing’ mode and select function no. 3. (peak pick)
Ø      Load the Spectra of Polystyrene film `S’.
Ø      Select the appropriate threshold value & select the Wave number from 4700  to 370 cm-1.
Ø      For resolution follow the same procedure and appropriate range wave numbers
Ø      Control of wave number
Ø      Place the poly-styrene film (0.05 mm thick) and scan it and check the maximum at following wave numbers (cm-1)
1. 3027.1        5. 1181.4
2. 2850.7        6. 1069.1
3. 1601.4        7.   906.7
4. 1583.1

Ø      Resolution
Ø      Check the resolution performance of the apparatus by recording the spectrum of polystyrene film (0.05 mm thick).
Ø      Measure the depth of the trough from, the maximum absorption at 2851 cm-1 (3.51um) to the minimum at 2870 cm – 1  (3.48um).
Ø      The depth must be greater than 18 % transmittance
Ø      Measure the trough from maximum at 1583 cm-1 (6.32um) to the minimum at 1589 cm-1 (6.29um), which must be greater than 12% transmittance. And record in Annexure – 1.
Ø      Affix a calibration status label on the instrument containing “Calibrated On”, “Due On” and “Signature”.
Ø      If the calibration is not within the specified standards, check the cleanliness of polystyrene film again and repeat the calibration
Ø      Report to Head – QC, if any discrepancy observed during calibration or operating the instrument and affix ‘Under Maintenance’ label on the instrument.
   
                             UNDER MAINTENANCE
        EQUIPMENT             :

        SINCE             :

SIGNATURE:

In case of calibration failure, follow the procedure given in SOP.

ANNEXURE – 1

FORMAT FOR CALIBRATION RECORD OF FTIR

       REF. SOP NO.: 
       Revision No.:  01
    Page No.: 1 of 1
      Effective from: 



Calibration Record     :           FTIR 
Instrument Sr. No.                  :
Make And Model       :
Calibration Date         :
Calibration Due On    :
Frequency                   :           Monthly 

Wave no.
Result
Limit
3027.1

± 3 nm
2850.7

± 3 nm
1601.4

± 1 nm
1583.1

± 1 nm
1181.4

± 1 nm
1069.1

± 1 nm
906.7

± 1 nm
Acceptance criteria:

1)      Resolution ________________________ (NLT 18% Transmittance)
2)      Resolution ________________________ (NLT 12% Transmittance)

Conclusion:  The Instrument is Qualified / Not Qualified for Use.





Calibrated By:                                                            Checked By:  
Date :                                                                          Date:

2 comments:

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    ReplyDelete
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