Krishnan basics of calibrations and pv non analytical instruments
1. Basics of calibrations &
performance verification
of non analytical instruments
Dr K Krishnan
2. 5.3.1.4 Equipment calibration and
metrological traceability
The laboratory shall have a documented procedure for the calibration of
equipment that directly or indirectly affects examination results. This
procedure includes:
a) taking into account conditions of use and the manufacturer’s
instructions;
b) recording the metrological traceability of the calibration standard and
the traceable calibration of the item of equipment;
c) verifying the required measurement accuracy and the functioning of
the measuring system at defined intervals;
d) recording the calibration status and date of recalibration;
e) ensuring that, where calibration gives rise to a set of correction
factors, the previous calibration factors are correctly updated;
f) safeguards to prevent adjustments or tampering that might
invalidate examination results.
22/02/2014 FQI ISO 15189 IA & QMS certificate
course
3. • Metrological traceability shall be to a reference material or
reference procedure of the higher metrological order available.
• NOTE Documentation of calibration traceability to a higher order
reference material or reference procedure may be provided by
an examination system manufacturer. Such documentation is
acceptable as long as the manufacturer’s examination system
and calibration procedures are used without modification.
• Where this is not possible or relevant, other means for providing
confidence in the results shall be applied, including but not
limited to the following:
— use of certified reference materials;
— examination or calibration by another procedure;
— mutual consent standards or methods which are clearly
established, specified, characterized and mutually agreed
upon by all parties concerned.
22/02/2014 FQI ISO 15189 IA & QMS certificate
course
4. Equipments that indirectly affect
results
• Parts of Analyzer which may / may not be integrated
but contribute indirectly to results:
• Pre Analytical Phase
– Centrifuge
– Water bath
– Autoclave
– Pipette
– Storage chambers, Environment
– HIT indices measuring component
• Automation of non – analyzer component
– Engen™
5. Calibration requirements - general
• Appropriate to the
equipment
• SOP of calibration defined
• Certification a must
• Signed off by the qualified
engineer / agency
• Traceability certificate copy
required for the instrument
used for any calibration
6. Calibration certificate contents
The calibration certificates issued by external agency must be checked for
following details:
• Name of Certificate issuing agency
• Date of issuance
• Description of the equipment under calibration
• Standards / Calibrators used for the calibration of the reference
• Date of Calibration
• Calibration results
• Acceptance criteria
• Next calibration due date
• Traceability to national/international standards
• Copies of calibration certificate of the standard / calibrator with traceability
to national / international standards (if applicable).
7. Centrifuge
• Indicators on the instruments
– Speed
– Temperature ?
• Calibration of speed
– Tachometer ( Traceability to reference standard and calibrated)
• Indicator display should match the actual reading with
tolerance limits prescribed by the manufacturer
• Frequency : every PM event / as required
• Centrifuge should be fully loaded
• Speed requirement specific for the tests done
• Speed required for tests defined:
– as per tests
– As per type of tubes used
– Temperature:
• Calibrated thermometer equipment used for calibrating temp
display
• Tolerance limit defined
9. Water baths calibration
• Correction Factor = the difference in the NIST traceable
thermometer and the Observed Temperature measured
by the NIST traceable thermometer. This is calculated
and reported during the annual certification of the
thermometers
• The True Temperature measured by the laboratory
thermometer = the Observed Temperature plus the
correction factor for that thermometer
• Equipment used: NIST traceable thermometer
• Frequency: Annual
Source: EPA/OPP MICROBIOLOGY LABORATORY
ESC, Ft. Meade, MD
Standard Operating Procedure for
Calibration of Thermometers
10. Autoclave calibration
Frequency of controls:
• With chemical Indicator : Every load
• With Biological indicator: Every month
Calibration Procedure:
• Temperature indicator, Pressure gauge and probe
should be calibrated quarterly / on extensive
maintenance
– Temperature gauge: Benzoic acid Grade AR: melts at 121°C:
– Pressure: A standard calibrated gauge attached to a T
connection and pressure compared – Limits: +5 % psi,
– Temperature indicator calibrated using silicon oil bath and std
thermometer at 100° C and 125° C (Limit: + 1°C)
Source: S S Jadiya, School of Pharma Sciences,
RGTU UIT, Bhopal
11. Calibrating a pipette for actual
volume
VOLUME
Pipette :
Water Temperature:
Density From Table: 0.9982
Technicia
n:
Date :
Balance :
Measure
Actual
Volume Weight Volume calc. Limits
No (µl) (g) (µl) (%)
1 1000 0.988 989.8 -
2 0.0 -
3 0.0 -
4 0.0 -
5 0.0 -
°C Density
18 0.9986
19 0.9984
20 0.9982
21 0.998
22 0.9978
23 0.9975
24 0.9973
25 0.997
26 0.9968
27 0.9965
28 0.9962
12. Storage chambers:
calibration and validation
Specify range of temperature for storage
The objectives:
• To calibrate temperature display with calibrated
equipment (as for water baths with NIST
thermometers)
• To identify the hot and cold zones in storage chambers,
• To challenge the storage temperature by keeping the
chambers open for fixed time
• To find the maximum time allowable for power shut
downs
13. Calibrating storage chambers
Three types of validation to be
conducted with the sensors
located at different places:
• The Static Mapping
• The Dynamic mapping
• The Power cut-off and
recovery mapping
Equipment ID Accuracy Calibration
validity
Data Logger
(36 CH)
Make: Chino
+ 0.5 °C 31st Oct
2014
RTD Pt-100
Sensor 4
wire
+ 0.5 °C 24th Nov
2014
Characterization of equipment
used to calibrate storage
14. Measuring HIT indices
• Manual inspection
– Color index grade I to IV
– Visual grading as per a given chart
– Range of hemolysis, turbidity and icterus to be determined for
each grading using dedicated reagents
• Automated Systems
– Integrated with Analyzer
• Usually done with dedicated reagents for measuring
hemolysis, turbidity and Bilirubin
• Throughput may be affected
– VITROS Microsensor technology is unique method
• No reagents used
• Hence Throughput not affected
16. MicroSensor™ - How it Works
Reflectometer
Spectrophotometer
Grating &
Photodiode Array
Electronics
A/D, DSP,
S/W
Collect Light from
Reflectometer
Lamp
Shine Light
Through Patient
Sample
Measure Spectrum
of Transmitted
Light
Master
Computer
Software
Communicate
Absorbance
Spectrum
Convert Spectra a
to Semi-
Quantitative
Indice Values
17. Absorbance Spectrum
0
0.5
1
1.5
2
400 450 500 550 600 650 700 750 800
Wavelength
Absorbance
Bilirubin
Turbidity
Hemoglobin
Absorbance Spectrum is acquired for each sample.
Spectrum is used to make predictions for the three indices.
Controls to be run weekly to cross check
No calibration required as no reagent used
18.
19. Cost of not calibrating non- analytical
equipments
20. Automation of pre analyticals
enGen™
•Sample processing – decapping, centrifugation
•Sample transport with intelligent routing
•Rules-based reflex & repeat testing
•Result verification
The only calibration required is for the
centrifuge
