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Calibration of FT-IR Spectrophotometer


Learn how to calibrate the FT-IR Spectrophotometer used in identification of Pharmaceutical products.


  • Check that all the connections of the instrument are proper.
  • Ensure that printer is attached to the instrument.
  • Attach sample compartment.
  • Log in the software.
  • Go to Set upÞ validation Þ System suitability.
  • Instrument may ask for gathering the configuration, then click OK.
  • System suitability set up will appear.
  • Go to checks & select only Abscissa, screen report.
  • Go to archive & set archive prefix as required & click OK.

Resolution


  • Go to Instrument Þ scan Þ Instrument Þ Advanced.
  • Keep Apodization ‘none’ & scan speed 0.1cm/s.
  • Instrument may ask for collecting new background, then click OK.
  • Go to Instrument Þ Validate Þ system Suitability & click OK.
  • Instrument should display ‘System suitability test pass’.
  • Scroll the report from original path for display, click print icon & take print out.
  • Abscissa spectrum of polystyrene film will be displayed.
  • Go to graph format icon & select the range 1600 to 1580.
  • Zoomed spectrum will appear, then collect the continuous curser & label at about 1583 cm-1 & 1589 cm-1, find out %T at these wave numbers & find out the difference between two %T.
  • Difference should be not less than 12%T.
  • Similarly zoom between 2840 cm-1 to 2880 cm-1 & label at 2851 cm-1 & 2870 cm-1, find out %T at these wave numbers & find out difference.
  • Difference should be not less than 18%T.
  • Then adjust the scale to 4000 to 450 cm-1 & take print outs.
  • Verification of wave number scale
  • Go to Process Þ Peak table & take its print .
  • Peaks (transmission minima) should be observed at the wave numbers as follows, with in the tolerance limit.

Wave number  cm-1     Minimum Tolerance cm-1     Maximum Tolerance cm-1
3060.0                            3058.5                                     3061.5
2849.5                            2848.0                                     2851.0
1942.9                            1941.4                                     1944.4

1601.2                            1600.2                                     1602.2
1583.0                            1582.0                                     1584.0
1154.5                            1153.5                                     1155.5
1028.3                            1027.3                                     1029.3

  • Remove sampling compartment.
  • Attach the diffuse reflectance sampling accessory.
  • Collect the background with KBr.
  • Go to Set up Þ validation Þ system suitability.
  • Set up will appear.
  • Go to checks & select only Abscissa, screen report.
  • Go to archive & set archive prefix as required & click OK.
  • Go to Instrument Þ validate Þ system suitability.
  • Click OK.
  • Instrument should display ‘System suitability test passes.
  • Report will be displayed, click print icon & take print out.

Maintenance / Repairs

Whenever instrument is out of order, then put the tag as ‘Out of Calibration’ & get it repaired.
After repair calibrate the instrument before use.

Frequency

Once in three months.
Attachments
Enclose following attachments with the calibration report.

  • System suitability check report for slide holder instrument configuration.
  • Abscissa spectrum of polystyrene film with identified peaks’ table for wave number calibration.
  • Abscissa spectrum of polystyrene film (showing %T at 2851cm-1, 2870cm-1, 1583 cm-1, 1589 cm-1).
  • System suitability check report for diffuse reflectance instrument configuration.
  • Note : Words in italics stand for instrument tabs.  

                     CALIBRATION REPORT OF FT-IR SPECTROPHOTOMETER

Reference –
Date -
Frequency - Once in three Months.
Instrument No. -
Make – 

  Model – 

1.0
Resolution:
 
Difference Between % T at 2851 cm-1 and 2870 cm-1
Difference Between % T at 1583 cm-1 and 1589 cm-1
Limit
NLT 18%
NLT 12%
Actual
2.0
Verification of Wave Number Scale -
Observed Wave Number cm-1
Minimum Tolerance
cm-1
Maximum Tolerance
cm-1
3058.5
3061.5
2848.0
2851.0
1941.4
1944.4
1600.2
1602.2
1582.0
1584.0
1153.5
1155.5
1027.3
1029.3
3.0
System suitability after attachment of diffuse reflectance sampling accessory : Complies / Does Not Comply.
4.0
Conclusion : Calibration is satisfactory / Not satisfactory.
5.0
Next Calibration Due On :
Done  By :
Date :
Checked By :
Date :









Ankur Choudhary is India's first professional pharmaceutical blogger, author and founder of Pharmaceutical Guidelines, a widely-read pharmaceutical blog since 2008. Sign-up for the free email updates for your daily dose of pharmaceutical tips. Email: .moc.enilediugamrahp@ofni



1 Comment so far : Add yours...

Anonymous said...

This is exactly what I've been looking for.

Thanks!

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