Calibration of FTIR Spectrophotometer : Pharmaceutical Guidelines

Calibration of FTIR Spectrophotometer

Know the procedure to calibrate the FTIR 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 up > validation > System suitability. 
  • The 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 > scan > Instrument > Advanced.
  • Keep Apodization ‘none’ & scan speed 0.1cm/s.
  • The instrument may ask for collecting new background, then click OK.
  • Go to Instrument > Validate > system Suitability & click OK.
  • The instrument should display ‘System suitability test pass’.
  • Scroll the report from the 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 wavenumbers & find out the difference between two %T.
  • The 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.
  • The difference should be not less than 18%T.
  • Then adjust the scale to 4000 to 450 cm-1 & take printouts.
  • Verification of wave number scale.
  • Go to Process > Peak table & take its print.
  • Peaks (transmission minima) should be observed at the wave numbers as follows, within 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. 
  • The instrument should display ‘System suitability test passes. 
  • The report will be displayed, click print icon & take print out.

Maintenance/ Repairs

Whenever the 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.
.moc.enilediugamrahp@ofni :liamENeed Help: Ask Question


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1 comment: Post Yours! Read Comment Policy ▼

  1. Anonymous5/5/11 02:15

    This is exactly what I've been looking for.

    Thanks!

    ReplyDelete


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