Installation and Operational
Qualification of Titration Equipment
(IQ/OQ-Protocol)
Com-300A Titration System
INTRODUCTION
This Installation and Operational Qualification Protocol, called IQ/OQ-Protocol, documents the
essential steps of the Com-300A Titration System installation and certifies its correct execution.
The instruments operating manuals are used as reference for detailed installation instructions and
default settings.
Purpose
The IQ-Protocol certifies the proper installation and calibration of all components according to the
specifications to be met.
The OQ-Protocol certifies that the whole set of equipment and its accessory work according to its
specification.
Scope
This Qualification Protocol applies to a new set of equipment and its accessory
This Qualification Protocol applies to a modified and previously qualified set of equipment and its
accessory
This Qualification Protocol serves as a requalification for a previously qualified set of equipment
and its accessory
Hirunama IQ/OQ Protocol for Titration Equipment 1
Installation and Operational
Qualification of Titration Equipment
(IQ/OQ-Protocol)
QUALIFICATION PROTOCOL
Date of installation: ______/_______/_______
CUSTOMER
Company: __________________________________________
Address: __________________________________________
Employee responsible: __________________________________________
SUPPLIER
Company: __________________________________________
Address: __________________________________________
Technician responsible: __________________________________________
EQUIPMENT
Instrumentation
Com-300A: __________________________________________
Serial Number: __________________________________________
Exchangeable units
Interchangeable unit: __________________________________________
Serial Number: __________________________________________
Electrodes
Electrode (p/n): __________________________________________
Batch Number: __________________________________________
ACCESSORY
Printer
Model: __________________________________________
Serial Number: __________________________________________
Balance
Model: __________________________________________
Serial Number: __________________________________________
Hirunama IQ/OQ Protocol for Titration Equipment 2
Installation and Operational
Qualification of Titration Equipment
(IQ/OQ-Protocol)
Installation Qualification
UNPACKING
1 All instruments and accessory were inspected. No physical damage was observed.
2 All items were delivered according to the shipping list.
EQUIPMENT INSTALLATION
3 All instruments incl. sample changer, if applicable, were installed in the working place and fits into
the provided space.
4 All instruments started properly.
5 The internal keyboards, if applicable, worked properly.
6 The exchangeable heads were mounted on the instruments and were detected properly.
7 Reagents were filled into the exchangeable heads and required data stored on the head.
8 The stirrers were installed incl. stand rods and titration clamps and connected to the instruments.
The stirrers worked properly according to its specifications.
9 The electrodes were connected to the instruments and were detected, if applicable, properly.
10 The pH electrodes, if applicable, were calibrated. The obtained data are attached and within
specification.
ACCESSORY INSTALLATION
11 The RS232 port was installed. A RS232 por stick was connected and detected by the titrator.
12 The Printer was installed. A method print out (default method) worked properly.
13 The Balance was connected to the equipment. A weight was successfully transmitted from the
Balance to the Titrator.
KARL FISCHER INSTALLATION
14 The Karl Fischer Titration vessel, if applicable, was installed properly. This includes all tubes,
drying flasks, waste bottles and electrodes. The solvent was filled into the titration vessel.
15 The KF, if applicable, was used to fill and empty the titration vessel. The pump worked properly.
16 The generator electrode, if applicable, starts the conditioning after complete installation. The drift
goes down to a value below 10 µg/min.
17 A Karl Fischer method was started and worked as specified in the instruments manual.
Hirunama IQ/OQ Protocol for Titration Equipment 3
Installation and Operational
Qualification of Titration Equipment
(IQ/OQ-Protocol)
CALIBRATION SPECIFICATIONS
The following specifications have to be met if a pH calibration is performed. For the calibration
technical buffer 4.0 , 7.0 and 10.0 are used.
Charge Buffer 4.0: __________________________________________
Expire Date: __________________________________________
Charge Buffer 7.0: __________________________________________
Expire Date : __________________________________________
Charge Buffer 10.0: __________________________________________
Expire Date : __________________________________________
Reference Value Slope: 95 %_____________________________________
Actual Value Slope: __________________________________________
Calibration report
Reference value Indication value Error Expanded uncertainty
Hirunama IQ/OQ Protocol for Titration Equipment 4
Installation and Operational
Qualification of Titration Equipment
(IQ/OQ-Protocol)
The installation is completed without any deviation from the requirements as specified in
the Installation Protocol. The criteria for the following Operational Qualification are fulfilled.
Deviations with no subject to release are stated under description.
The following deviations from the requirements as stated in this Installation Protocol were
observed. The installation is not completed, a requalification is required.
Description: ________________________________________________________
________________________________________________________
________________________________________________________
________________________________________________________
________________________________________________________
________________________________________________________
________________________________________________________
________________________________________________________
Employee Responsible: _______________________________
Date: _______________________________
Signature: _______________________________
Technician Responsible: _______________________________
Date: _______________________________
Signature: _______________________________
Hirunama IQ/OQ Protocol for Titration Equipment 5
Installation and Operational
Qualification of Titration Equipment
(IQ/OQ-Protocol)
Operational Qualification
The Operational Qualification Protocol certifies, that the set of equipment and its accessory works
according to the specification of the manufacturer and that all operators defined by the customer
are trained on the equipment. CRM materials are used to show that the criteria as follows are
fulfilled.
The Qualification procedure is divided into 3 steps.
1. Standardization of the Titration reagent using the specific CRM material three times.
2. Linearity test using the specified CRM material by titrating 6 different amounts of the CRM
material.
3. Calculation of the statistical values to show that the whole set of equipment is able to
produce consistent results over the operating range of the Titrator.
The criteria which shall be fulfilled are as follows.
1. The standardization gives a relative standard deviation (RSD) of <0.5 %.
2. The Linearity test gives a recovery rate (mean value) of 6 sequential measured titrations of
100 ± 2 %.
3. The correlation factor of the linearity test is better than or equal to 0.99.
4. The ordinate intercept of the linearity test is smaller than or equal to 0.05 ml or, in case of
coulometric Karl Fischer titrations, smaller than or equal to 5 µg water.
The balance used for this Qualification provided by the customer should have at least 4 digits with
a resolution of 0.001 g.
All methods used as well as calculation results and used formula are attached to this protocol.
Hirunama IQ/OQ Protocol for Titration Equipment 6
Installation and Operational
Qualification of Titration Equipment
(IQ/OQ-Protocol)
VOLUMETRIC TITRATION
OQ Titration number:
Instrumentation
Com-300A: __________________________________________
Serial Number: __________________________________________
Interchangeable unit: __________________________________________
Serial Number: __________________________________________
Electrode (p/n): __________________________________________
Batch Number: __________________________________________
Balance (Model): __________________________________________
Serial Number: __________________________________________
Reagents
Reagent/Manufacturer: __________________________________________
Batch number: __________________________________________
CRM Material
Reference Material: __________________________________________
Manufacturer: __________________________________________
Certified value: __________________________________________
Drying procedure: __________________________________________
Procedure Description
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
Hirunama IQ/OQ Protocol for Titration Equipment 7
Installation and Operational
Qualification of Titration Equipment
(IQ/OQ-Protocol)
Repeatability
Mass of standard, g Titration volume,ml Content, mg/g or %
Average, mg/g or %
% RSD, %
Uncertainty , %
Ratio of Recovery
Mass of standard, g Titration volume,ml Content, mg/g or % Ratio of Recovery, %
Average, mg/g or %
Uncertainty , %
Hirunama IQ/OQ Protocol for Titration Equipment 8
