Definition of calibration & validation and calibration of IR

1. Presented By:
Netra Prasad Neupane
17BPH080
B.Pharmacy (8th semester)
Presented To:
Prof. (Dr.) P. Malairajan
FHS, SIHAS
SHUATS
Presentation on:
SAM HIGGINBOTTOM UNIVERSITY OF AGRICULTURE
TECHNOLOGY AND SCIENCES, PRAYAGRAJ
ADVANCED INSTRUMENTATION TECHNIQUES
BP811ET
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2. INTRODUCTION
Validation:
 Validation of an analytical procedure is the process by
which it is established, by laboratory studies, that the
performance characteristics of the procedure meet the
requirements for the intended analytical applications.
Equipment validation:
 Demonstrate that equipment used in validation studies is
suitable for use and is comparable to equipment used for
routine analysis Calibrated (as applicable) Qualifications
should have been performed.
•Installation Qualification
•Operation Qualification
•Performance Qualification
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3. Method validation:
Process Validation:
It is documented program which provides a high
degree of assurance that a specific process will
consistently produce a desired result/ product
meeting its predetermined specifications and
quality characteristics.
It is the process of demonstrating that analytical
procedures are suitable for their intended use.
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4. DEFINATION
According to ICH :
Calibration: It demonstration that a particular
instrument or device produces results within specified
limits by comparison with those produced by a reference
or traceable standard over an appropriate range of
measurements.
Validation: Validation of an analytical procedure is the
process by which it is established, by laboratory studies,
that the performance characteristics of the procedure
meet the requirements for the intended analytical
applications.
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5. Why should be Calibrated?
These should be calibrated for the following ways.
To ensure the Reliability of the instrument.
To determine the accurancy of the instrument.
To ensure the Reading are consistent with other instrument.
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6. Need for calibration
Calibration can be called for:
• With a new instrument
• When a specified time period is elapsed.
• When a specified usage (operating hours) has
elapsed.
• When an instrument has had a shock or
vibration which potentially may have put it
out of calibration.
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7. • Sudden changes in weather.
• Whenever observations appear questionable.
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8. IR Spectrophotometer
• IR spectroscopy is the spectroscopy that deals with the infrared
region of the electromagnetic spectrum, that is light with a longer
wavelength and lower frequency than visible light.
• Infrared spectroscopy (IR) measures the bond vibration
frequencies in a molecule and is used to determine the functional
groups.
• The infrared region of the spectrum encompasses radiation with
wave numbers ranging from about 12,500 to 50 cm -1 (or)
wavelengths from 0.8 to 200 µ.
• Infrared region lies between visible and microwave region.
• Infrared spectroscopy is the analysis of infrared light interacting
with a molecule.
• It is based on absorption spectroscopy.
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9. Infrared Region
Near infrared region 0.8- 2.5 µ (12,500-4000 cm-1)
Main infrared region 2.5-15 µ (4,000-667 cm-1)
Far infrared region 15-200 µ (667-100 cm-1)
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10. Calibration of IR spectroscopy
• Wave number verification
• Resolution performance
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11. Wave number verification
• Prepare polystyrene film with thickness 0.04 mm
and verify the wave number.
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Observed wavenumber Minimum tolerance Maximum tolerance
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

12. Resolution performance
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
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13. Application of IR spectroscopy
Structure determination
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14. Identification of substances
Determination of molecular structure.
Detection of impurities
Progress of reactions
Presence of water in sample
Application in industry
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15. REFERENCE
1. Aparna C, Gowrisankar D. a Review on Calibration of
Analytical Instruments. Int J Pharm Chem Biol Sci.
2015;5(3):573–82.
2. Günzler, Helmut, and Hans-Ulrich Gremlich. "IR
spectroscopy. An introduction." (2002).
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16. 9 March 2021 16
Thank you