Calibration, Validation, Qualification and System Suitability Tests in the Electrochemistry

Ghazanfar Abbas

Content
q q

q q q

Introduction, Definitions Validation of the dosing unit (DosingTest) Validation of a titrating system Validation of a coulometer Summary

Calibration
q

Determination of the function between the measuring value and the result.
Kalibration
8 7 6 5 4 3 2 1 0 0 1 2 M e ssw e rt 3 4

Ausgabewert

Reihe1

Validation
q

Error calculations in a analysing system using chemical, physical and mathematical basics.

Important points: linearity, selectivity, correctness, accuracy

Qualification
q

Validation to check general quality characteristics of a measuring system compared to the technical specifications.

System Suitability Tests
q

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:
q

q q q

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 Vreal : mabgel. : rF : rL : rS : * 1 / rF * ( 1 + rL / rF rL / rS )

real volume in ml, calculated from the weighing result mass reading from the balance density of the dosed solution density of the air in g/ml density of the standard used for the calibration of the balance

Validation of the dosing unit
Evaluation
q

(using statistics) difference real volume to read volume correlation, slope, y-axis

rel. error :

q

linear regression: trendline Vreal/Vread

q

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:
q

q q q

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
q

Standarddeviation: (Results) linear regression: trendline correlation, slope, y-axis

q

q

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 q Check the different components (balance, measuring unit, electrode, dosing unit) q Titration parameters, mode, calculation
q

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:
q q q q q

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:
q

preparation realization -- according to the instruction evaluation -- using statistics Opinion and conclusion -- ok or error search

q

q

q

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
q q q q q q q q q q

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?

Sign up to vote on this title
UsefulNot useful