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Annex 4 Qualification of IR Spectrophotometers
Annex 4 Qualification of IR Spectrophotometers
QUALIFICATION OF EQUIPMENT
QUALIFICATION OF IR SPECTROPHOTOMETERS
Introduction
The present document is the fourth Annex of the core document “Qualification of
Equipment”, and it should be used in combination with it when planning, performing and
documenting the IR spectrophotometer qualification process.
The core document contains the Introduction and general forms for Level I and II of
qualification, which are common to all type of instruments.
For FTIR spectrometers, an example has been added to give instrument-specific proposals
that may be used in combination with the general requirements presented in the core
document “Qualification of Equipment”, when drawing up a Level I checklist.
TABLE I
Manufacturer:
Provider/Distributor:
Notes:
- This check-list, containing examples of technical attributes that can be taken into
account in the selection of an instrument and supplier, can be used in combination
with the general check-list presented in Level I in the core document “Qualification of
Equipment”.
- For Table II (Level II of Equipment Qualification: Installation and release for use)
please refer to the core document.
TABLE III
TABLE IV
ANNEX I
This Annex contains practical examples of tests and their associated tolerance limits for
several parameters related to the performance of an IR spectrophotometer.
These examples can be considered by the OMCLs as possible approaches to perform the
Level III of the equipment qualification process: “Periodic and motivated instrument checks”.
Note: If available and judged appropriate, the use of the automatic internal calibration
function of the instrument is encouraged. Please refer to the manufacturer instructions.
1. WAVE-NUMBER SCALE
Method:
Record the minimum energy ratio value for at least one of the following measurement points
and compare it to the vendor’s specifications:
Limits:
Energy ratio test specifications vary for each spectrometer configuration. Refer to the
manufacturer’s specification.
3. SIGNAL/NOISE RATIO
Method:
Record the maximum noise level for each of the following regions:
Limits (% T):
Noise level test specifications vary for each spectrometer configuration. Refer to the
manufacturer’s specifications.
4. RESOLUTION
Materials:
Certified polystyrene film of approximately 35 µm in thickness.
Method:
- For instruments having a monochromator, record the spectrum of the polystyrene film.
- For Fourier-transform instruments, use suitable instrument resolution with the appropriate
apodisation prescribed by the manufacturer. The resolution is checked by suitable means,
for example by recording the spectrum of a polystyrene film approximately 35 µm in
thickness.
Limits:
Monochromator instruments:
- Difference x 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) > 18.
- Difference y 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) > 10.
Fourier-transform instruments:
- Difference between the absorbances at the absorption minimum at 2870 cm-1 and the
absorption maximum at 2849.5 cm-1 > 0.33.
- Difference between the absorbances at the absorption minimum at 1589 cm-1 and the
absorption maximum at 1583 cm-1 > 0.08.
5. ZERO TEST
Method:
When using a polystyrene film of approximately 35 µm in thickness as standard at the
wavelength of 2925 cm-1 and 700 cm-1, almost complete absorption of the irradiated energy
can be observed. With this test, the remaining transmission is measured. As the maximum
absorption can be observed at 700 cm-1 negative values may be observed. The objective of the
test is to evaluate if, despite the fact that there is almost complete absorption, energy is still
detectable.
Non-valid results are an indication of a non-linear behaviour of the detector and the electronic
system.
Limits (%T):
See manufacturer’s specification.
Note: if an automated system is available, this test can be run more frequently or it can be
transferred to Level IV, to be run before each analysis.
Method:
This test checks the presence of peaks that signal a contamination problem.
Use the automated function of the instrument (if available) to perform this test. If not
available, record a background spectrum.
Limits:
Note: if an automated system is available, this test can be run more frequently or it can be
transferred to Level IV, to be run before each analysis.
Method:
This test checks for an unexpected reduction of the transmittance. An instrument specific
automated test can be used.
A background spectrum is recorded and the transmittance is measured at 3 wave numbers e.g.
4000, 2600 and 1000 cm-1.
Limits:
The lower limit of the transmittance for the 3 wave numbers must be 80 %.
8. SPECTRAL LIBRARY
It is recommended to record the spectrum of a newly acquired polystyrene film and to save it
in a spectra library.
Electronic libraries for checking the identity of unknown substances should be examined from
time to time by using selected examples of well-known reference substances.
Requirements:
The substances are unambiguously identified by the electronic library search.
ANNEX II
This Annex contains practical examples of tests and their associated tolerance limits for
several parameters related to the performance of an IR spectrophotometer.
These examples can be considered by the OMCLs as possible approaches to perform the
Level IV of the equipment qualification process: “In-use instrument checks”.
Note: If available and judged appropriate, the use of the automatic internal calibration
function of the instrument is encouraged. Please refer to the manufacturer instructions.
Method:
This test should be performed according to Ph. Eur., the MAH dossier or a suitably validated
in-house method.
Note: regeneration or replacement of the desiccant should be done in case of failure of the
system suitability test (e.g. by drying it for 8-12h at 250°C, then flushing with N2).
REFERENCES