Calibration, Validation, Qualification

and System Suitability Tests in the

Electrochemistry

Ghazanfar Abbas
 Content

 Introduction, Definitions
 Validation of the dosing unit (Dosing-
Test)
 Validation of a titrating system
 Validation of a coulometer
 Summary
 Calibration
 Determination of the function between the
measuring value and the result.

Kalibration

8
7
6
Ausgabewert

5
4 Reihe1
3
2
1
0
0 1 2 3 4
Messwert
 Validation
 Error calculations in a analysing system using
chemical, physical and mathematical basics.

Important points:
linearity, selectivity,
correctness, accuracy
 Qualification

 Validation to check general quality

characteristics of a measuring system compared
to the technical specifications.
 System Suitability Tests

 Test of an instrument or a method for the

analysis of a certain sample.
 Validation of the dosing unit
Dosimat test according to AB 238
 Validation of the dosing unit
Realization:

Dose 10 different volumes between 0.1 und 1 cylinder

into a bottle on an analytical balance.

accidently sequence

accidently volumes (except 0.1 and 1 cylinder)

 Validation of the dosing unit
Importent points:

 Density must be known on a constant temperature

(no sunbeam, no draught or wind)
 The Burette tip has to be fixed above the balance
 no micro-valve can be used.
 The air in the balance should be saturated with the
solvent used, to get a stable reading.
 Validation of the dosing unit
Calculation
Vreal = mread * 1 / rF * ( 1 + rL / rF - rL / rS )

Vreal : real volume in ml, calculated from the weighing result

mabgel. : mass reading from the balance
rF : density of the dosed solution
rL : density of the air in g/ml
rS : density of the standard used for the calibration of the balance
 Validation of the dosing unit
Evaluation (using statistics)

 rel. error : difference real volume to read volume

 linear regression: correlation, slope, y-axis

 trendline Vreal/Vread
Validation protocol
Validation protocol
Opinion and Conclusion
 Metrodata "Dosing-Test"
It is possible to automate this procedure

Therefore the windows software

Metrodata "Dosing-Test" (6.6025.000) is necessary.

Additionally the cables: - balance - pc

- dosing unit - pc
Metrodata "Dosing-Test"
 Validation of a Titration System

Titrator test according to AB 252 (KF AB 255)

 Validation of a Titration System

Realization:

10 Titrations with the same parameters but

different sample sizes are done.
The consumtion has to be withinl 0.2 - 0.9 cylinder
volumes.
Sample : Titer substance or Standardsample
 Validation of a Titration System

Important points:

 Constant temparature (no sunbeam, no draught

or wind)
 Electrode and burette tip in correct positions
 Electrode condition (electrode test necessary ?)
 correct sample size (balance and cylinder)
 Validation of a Titration System

Evaluation using statistics

 Standarddeviation: (Results)

 linear regression: correlation, slope, y-axis

 trendline titer / consumption

 Opinion and Conclusion
Are all the values and parameters within the limits?

Yes ----- The system is o.k. for a certain periode !

No ------ Additional checks are necessary,

-------------------------- error search!!
 Opinion and Conclusion
Error search :

 Repeat the validation, maybe an other user

 Check the different components

(balance, measuring unit, electrode, dosing unit)

 Titration parameters, mode, calculation
 Validation of a KF Titrator

The validation of KF titrator is simular to a normal

Titration system.

Different standards can be used:

- Certified standards
- Defined samples
- Water (ul Syringe)
 Validation of a KF Coulometer

For the coulometeric water determination, no dosing

unit is used.
The method normally works for samples containing
0.05 to 10 mg water

The validation should be done for the range which is

used for real samples in the certain laboratory.

(e.g. 0.2 to 2 mg or 0.05 to 0.5 mg with the limits for this range)
 Validation of a KF Coulometer

Important points:

 dry cell
 tightness of the cell ( drift below 20 ug/min.)
 new reagent
 handling of the standard (rinse the syringe)
 clean electrodes
 Summary
A Validation can be separated into different steps:

 preparation

 realization -- according to the instruction

 evaluation -- using statistics

 Opinion and conclusion -- ok or error search

 Summary

Experience from the validation should

influence the daily routine !

Experience from the daily routine should

influence the instructions for a validation
and also the periode for the validations!
 Support from Metrohm
 Metrohm is ISO 9000 certified
 Selftest of the instrument on start up.
 Diagnosis in the instructions for use
 Different application bulletins (238, 252, 255)
 pH- electrode test in the pH-Meter 713 and 692
 Metrodata "Dosing-Test" Software
 "GLP- page" in the 726 Titroprocessor
 Certified buffers und electrodes
 Seminars for customers, sales and service people
 CH Service contracts
 Discussion

Do you have additional wishes from Metrohm?