9d9113d3600ba49503924d6091409a44.ppt
- Количество слайдов: 41
Basics of Titration by Michael Margreth
Basics • One of the oldest analytical methods • Based on chemical reaction • Determination of the volume of a standard solution (titrant) • Standard solution contains a defined number of molecules • Measuring volume = counting molecules • TITRATION MEANS COUNTING!
Titration Start Titrant Sample
Titration Endpoint Titrant + Sample
Titration End Titrant + Sample
Principle of a Manual Titration Titrant - optical detection - manual control - manual addition Color indicator
All in one! • Dosing • Measuring • Controlling • Evaluation
Titrations Modes • Set Endpoint Titration SET • Monotonic Equivalence point Titration MET • Dynamic Equivalence point Titration DET • Karl Fischer Titration KFT
Set Endpoint Titration Signal [p. H/m. V] endpoint volume
Monotonic Equivalence Point Titration Signal [p. H/m. V] equivalence point volume
Dynamic Equivalence Point Titration Signal [p. H/m. V] equivalence point volume
Volume increment • • In MET mode the steps are always the same In DET mode the steps are calculated by the Titrando MET Mode DET Mode p. H EP 1 V [m. L]
Karl Fischer Titration Signal [mg/min] Endpoint volume
Which mode for which titration? SET MET DET KFT defined endpoint slow reaction quick reaction Karl Fischer Titration non-aqueous titration duration has priority non S-shaped universal curve method (90%)
Endpoint evaluation tangent method circle method derivative method
Titration steps • sample preparation (homogeneity) • right electrode choice • possibly electrode conditioning • titrant preparation • titer determination • buret/ sample size choice • correct arrangement in titration vessel • stirrer rate • method parameters • results calculation • report
Arrangement stirrer electrode buret
Titer • What is a titer? Correction factor • Why do we need the titer? To know the exact concentration of the titrant • What is the unit? none • How is the titer determined? With titrimetric standards • When do I have to determine a titer? frequently
Advantages • • Absolute method Easy to carry out Carried out very rapidly Versatile method Highly reproducible and correct results Can be automated economical
Hardware definition System
Titrant definition
Sensor definition
Method definition Parameters
Titration method
Titration parameters
Sensor
Dosing device
Stirrer
Direct parameters
Direct parameters
Start conditions
Titration parameters
User defined parameters
Measurement density • • 4 0 default high density • 9 low density DET Mode 8, 5 8, 0 7, 5 p. H 7, 5 EP 1 7, 0 6, 5 6, 0 0, 5 1, 0 1, 5 2, 0 2, 5 3, 0 V [ml] 3, 5 4, 0 4, 5 5, 0 5, 5 6, 0 -0, 0 0, 5 1, 0 1, 5 2, 0 2, 5 3, 0 V [ml] 3, 5 4, 0 4, 5 5, 0 5, 5 6, 0
Stop conditions
Evaluation
Calculation
Report
Result report
Curve report
9d9113d3600ba49503924d6091409a44.ppt