Calibration

2016
BY HIDAYATH UNNISA
M.PHARM 1ST YR
SULTAN-UL-ULOOM COLLEGE OF
PHARMACY, HYD,TS, INDIA.
21-Apr-16
ADVANCED PHARMACEUTICAL
ANALYSIS-II

April 21, 2016 [ADVANCED PHARMACEUTICAL ANALYSIS-II]
HIDAYATH UNNISA, SULTAN-UL-ULOOM COLLEGE OF PHARMACY, BANJARA HILLS, HYDERABAD, TS,INDIA. PAGE 2

UNIT-I
Calibration and qualification of equipment
CALIBRATION
Calibration is the process of finding a relationship between two quantities that are unknown (when the
measurable quantities are not given a particular value for the amount considered or found a standard for the
quantity).
Calibration of an instrument is the process of determining its accuracy. The process involves obtaining a
reading from the instrument and measuring its variation from the reading obtained from a standard instrument.
Calibration of an instrument also involves adjusting its precision and accuracy so that its readings come in
accordance with the established standard.
What is Equipment Calibration?
Calibration of equipment needs to be carried out on a regular basis. This is because instruments tend to deviate
owing to hard operating conditions, mechanical shocks or exposure to extreme temperature or pressure.
Frequency of calibration would depend on the tolerance level. When the objective of the measurement is critical
calibration would need to be carried out more frequently and with great accuracy.
Definition of Calibration: ICH The 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.
Qualification: Action of proving and documenting that equipment or ancillary systems are properly installed,
work correctly, and actually lead to the expected results. Qualification is part of validation, but the individual
qualification steps alone do not constitute process validation.
QUALIFICATION OF EQUIPMENT:

Qualification of analytical instrumentation is essential for accurate and precise measurement of analytical data.
If the instrumentation is not qualified, ensuring that the results indicated are trustworthy, all other work based
upon the use of that instrumentation is suspect. For the purposes of this article, the assumption will be made that
the foundation of validation and verification work to follow is based solidly upon well-qualified
instrumentation.
Difference between calibration and qualification
You can see by my definition above that I consider calibration to be
something you do in relation to measurement. Qualification proves
suitability in all relevant areas, not just measurement. However, if,
for example, you have a process component that functions only to measure
a critical process parameter (and cannot impact product quality in any
way through its measurement function), you may be able to prove it is
suitable (qualified) through calibration alone.
CALIBRATION STANDARD
Definition
A recognized objective standard of quality for a business process output or characteristic. Calibration standards
may be established through internal research or with the help of external process improvement consultants, and
are used to make adjustments to other areas of the enterprise to achieve a uniform high standard of measurable
quality.
CALIBRATION STANDARDS AND PREPARATION
TEMPERATURE
Type: Mercury in glass or other reference thermometer with Accuracy: ±0.02ºC Resolution: ±0.01ºC
CONDUCTIVITY 1413 us/cm referred to 25ºC
A solution preparation is based on the procedure in the HANDBOOK OF CHEMISTRY AND PHYSICS 1963
Chemical Rubber Publishing Company. Conductivity of Standard Solutions using KCl. Preparation: Dissolve
0.7459 grams of potassium chloride (KCl) in distilled water made up to one litre of solution. At 25ºC this has a
conductivity of 1413 us/cm.
SALINITY 35ppt

Preparation: Obtain clean seawater and standardise using a laboratory salinometer (eg Yeo-Kal Model
601MKIV) whose accuracy is: Accuracy: 0.003ppt Resolution: 0.001ppt Standardise against I.A.P.S Standard
seawater service P101 and use the measured salinity of the clean seawater as the calibration solution.
Alternatively, dissolve 32.4356 grams of KCl in 1 kg of solution for a 35 ppt salinity. Conductivity is very
dependent upon temperature. This solution of KCl will only give sufficiently accurate results when its
temperature is within about 0.1deg C of 15degC.
pH
Buffers 4.00 and 10.01 prepared using Standard Methods., Ref: Durst, R.A. 1975 Standard Methods; Reference
Materials: Standardisation of pH Measurements NBS Spec Publ. 260-53, National Bureau of Standards,
Washington D.C.
pH Weight of Chemicals needed/1000mls solution @ 25ºC
4.004 10.12gm KHC8H4O4 (potassium hydrogen phthalate)
10.014 2.0992 gm NaHCO3 (sodium bicarbonate)
2.640gm Na2CO3 (sodium carbonate)
Alternatively, a chemical supply company can provide standard buffer solutions.
ORP STANDARD
Reference: Innovative Sensors Inc. Technical Bulletin. ORP or REDOX potential can be reported as either the
direct potential or alternatively it can be reported as referred to the hydrogen electrode. Prepare pH buffers of
4.0 and 7.0. Add a "pinch" of quinhydrone crystals to each of the buffers until saturated and stir for 30 seconds
to obtain the two calibration points. Buffer 7.0 with quinhydrone crystals gives a probe output of 86mV (or
295.2 mV when referred to the hydrogen electrode). Buffer 4.0 with quinhydrone crystals gives a probe output
of 263mV (or 472.2 mV when referred to the hydrogen electrode).
DISSOLVED OXYGEN
When a new probe is installed it is advisable to do a two point calibration at 0% and 100%. Once this has been
done correctly it is only necessary to calibrate the 100% point for field calibrations. The zero point will rarely
change. To obtain 0% use either nitrogen gas in a container (i.e. purge oxygen out) or dissolve 26gm of sodium
sulphite and add 0.2 gm of cobalt chloride in 500mls of water. Discard solution oafter 30 minutes as it will not
keep. To obtain 100% saturated water aerate a sample of fresh water for about 2 hours. A fish tank air pump and
aerator stone is ideal. Note: Be sure that the 100% sample is not contaminated with the 0% solution. Wash the
sensor before placing it in 100% saturated water.
TURBIDITY

FOR MAIN STANDARD 200 ntu's
Preparation for 200 ntu using Standard Methods. Solution 1: 10gm Hexamethylenetetramine C6H12N4
(analysis quality) is dissolved in distilled water. This solution is made up to 100mls with distilled water.
Solution 2: 1.0gm Hydrazinium sulphate N2H6SO4 (analysis quality) is dissolved in distilled water. This
solution is made up to 100mls with distilled water. Procedure: Mix 5mls of solution 1 with 5mls of solution 2.
Allow to stand for 24 hours at 25 ± 3ºC, then make up this solution to 200mls with distilled water. This is 200
ntu. This solution has a shelf life of 4 weeks if kept in a dark place.
The activity of qualifying systems and equipment is divided into a number of subsections including the
following:
• Design qualification (DQ)
• Component qualification (CQ)
• Installation qualification (IQ)
• Operational qualification (OQ)
• Performance qualification (PQ)
Design qualification (DQ): It should ensure that instruments have all the necessary functions and
performance that will enable them to be successfully implemented for the intended application and meet
business requirements. It also verifies that the equipment has been developed in a quality control
environment.
The main purpose of DQ is to ensure that
The right type of equipment is selected for specific tasks.
The equipment will have the right functional and performance specification.
The vendor meets the user firm’s qualifications and support criteria.
DQ should be performed – when
A new instrument is being purchased or
An existing instrument is being used for a new application not previously specified.

Installation qualification (IQ):- It establishes that the instrument is delivered as designed and specified,
that it is properly installed in the selected environment and that this environment is suitable for the
operation and use of instrument.
The main purpose of IQ are to ensure that the-
Equipment has been received as purchased.
The equipment meets the physical hardware specification.
Individual hardware modules and all accessories are properly installed and connected to each other.
The software is completely installed on the designated storage device.
The instrument functions in the selected environment.
Operational qualification (OQ): - Operational qualification is process of demonstrating that an
instrument will function according to its operational specifications in the selected environment. The
main purpose of OQ is to ensure that the equipment’s hardware as well as software meets functional and
performance specifications as required for the intended application and as specified in the DQ
document.
Performance qualification (PQ):- It is actual demonstrations during the course of the validation program
show that the facility, support system or piece of modular equipment perform according to a predefined
protocol and achieve process reproducibility and product acceptability.

THANK YOU.... . . . .

Calibration

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