Basics of titration &

Introduction to GTP™
 Agenda

 Welcome
 Definition of Titration
 Chemical reactions for Titration
 Measurement Techniques
 Titration Types
 Titration Techniques
 Introduction to GTP™
 Summary

Basics of titration 2 GTP™

 What isTitration?

Definition of Titration

Determination of the quantity of a chemical substance in a sample ...

by controlled addition

of a reagent (titrant) of known concentration ...

based on a complete chemical reaction between

substance and reagent ...

to an endpoint, which is appropriately detectable.

Basics of titration 3 GTP™

 Manual Titration – Automatic Titration

Burette

Titrant

Indicator
(Sensor)

Result Sample
calculation Automatic evaluation &
Result calculation
Basics of titration 4 GTP™
 Agenda

 Welcome
 Definition of Titration
 Chemical reactions for Titration
 Measurement Techniques
 Titration Types
 Titration Techniques
 Introduction to GTP™
 Summary

Basics of titration 5 GTP™

 Chemical reactions for titrations

Requirements for the chemical reactions

 High reaction rate at ambient conditions

(short titration time)
 Simply controlled experimental conditions
(temperature, pressure, solvent, pH, etc.)
 Specific reaction
(no side reactions with other components)
 Strictly stoichiometric course of reaction
 Traceable course of reaction

Basics of titration 6 GTP™

 Types of chemical reactions for titration
Acid / Base titration

HCl + NaOH → NaCl + H2O

Examples
 Acid content in wine, milk
 Acid content in oranges juice
 Assay determinations (Aqu. & Non-aqu.)

METTLER TOLEDO Electrodes: pH sensitive membrane

Basics of titration 7 GTP™

 Types of chemical reactions for titration
Precipitation titration

NaCl + AgNO3 → AgCl (s) + NaNO3

Examples
 Chloride Content
 Sodium chloride content in food:
ketchup, chips, cheese, eggs
 Chloride content in water and waste water
 Silver content in coins and jewelry

METTLER TOLEDO Electrode: Silver ring electrode

Basics of titration 8 GTP™

 Types of chemical reactions for titration
Complexometric titration

Mg2+ + EDTA4- → [Mg-EDTA] 2-

Examples
 Total hardness in water (Ca & Mg)
 Calcium content in cheese and milk
 Cement Analysis (Al, Fe, Mg, Ca)
 Electroplating bath (Cu, Zn, Cd)

METTLER TOLEDO Sensor: Phototrode

Basics of titration 9 GTP™

 Types of chemical reactions for titration
Karl Fisher titration for water determination
I2 + SO2 + 2 H2O 2 HI + H2SO4

A special type of titration

 Specific for water, which is in many samples
 Fast (1 – 2 minutes)
 No decomposition
 Wide measuring range (0,001% – 100 %)
METTLER TOLEDO Electrode: Pt pin electrode
For Karl Fisher titration a separate generation of instruments exist. For more
information take a look to the Karl Fisher presentation or to our specific brochures.

Volumetric KF- Coulometric KF-

titration titration

Basics of titration 11 GTP™

 Types of chemical reactions for titration
Precipitation for surfactant determination

[surfactant] – + [surfactant] + → Complex

anionic surfactant cationic surfactant colloidal complex

Clear solution → turbid solution

Examples
 Washing powder
 Softener
 Toothpaste Colloidal complex
 Cosmetics (cross section)

 Paper

 METTLER TOLEDO Sensors: Phototrode

Basics of titration 12 GTP™

 Major titration reactions

Titration reactions

Acid / Base
Oxidation / Reduction
Aqueous
(Redox)
Non-aqueous
Diazotizations
Manganometry
Complexometric Precipitation Iodometry
Turbidimetry Cerimetry
Karl Fischer

Basics of titration 13 GTP™

 Agenda

 Welcome
 Definition of Titration
 Chemical reactions for Titration
 Measurement Techniques
 Titration Types
 Titration Techniques
 Introduction to GTP™
 Summary

Basics of titration 14 GTP™

 Monitoring of Titration
Major measurement techniques

Electrochemical Conductimetric
Potentiometric (pH/mV)
Voltametric (Ipol)
Amperometric (Upol)

Photometric
Colorimetric (color change)
Turbidimetric
Basics of titration 15 GTP™
 Agenda

 Welcome
 Definition of Titration
 Chemical reactions for Titration
 Measurement Techniques
 Titration Types
 Titration Techniques
 Introduction to GTP™
 Summary

Basics of titration 16 GTP™

 Types of titrations

There are two titration modes which

can be distinguished:

 Endpoint titration EP

 Equivalent point titration EQP

Basics of titration 17 GTP™

 Endpoint titration (EP)

E (mV, pH)
9

7 Endpoint

Volume (mL)
Basics of titration 18 GTP™
 Equivalence point titration (EQP)

Volume Vs dE/dV plot

E (mV,pH)

Equivalence point

Volume (mL)
Basics of titration 19 GTP™
 Agenda

 Welcome
 Definition of Titration
 Chemical reactions for Titration
 Measurement Techniques
 Titration Types
 Titration Techniques
 Introduction to GTP™
 Summary

Basics of titration 20 GTP™

 Titration techniques

Three main titration techniques are used

 Direct titration

 Direct titration with blank

 Back titration

Basics of titration 21 GTP™

 Direct titration – the optimal case
Conditions
 Solvent is inert
 Fast reaction, clear endpoint
Performance
 Direct titration of sample and solvent to EP or EQP
Example
 Titration of NaOH with HCl
Result
 Result = titrant consumption

titrant
sample mL
Basics of titration 22 GTP™
 Direct titration with blank
Conditions
 Solvent is not inert
 Fast reaction, clear endpoint
Performance
 Blank: Titration of solvent to EP or EQP
 Sample: Direct titration of sample and solvent to EP or EQP
Example
 Determination of acid number (AN) in Oils
Result
 Result = titrant consumption – blank value

blank titrant
solvent sample mL
Basics of titration 23 GTP™
 Back titration
Conditions
 Solvent is inert
 Slow reaction and / or weak endpoint
Performance
 Back value: Add excess of titrant A which reacts with the sample
 Sample: Titration of the excess of titrant A with titrant B
Example
 Saponification value of edible oils
Result
 Result = back value (titrant A consumption) – titrant B consumption
Back value (titrant A; acid)

titrant B (base)
sample mL
Basics of titration 24 GTP™
 Titration applications for various samples

Electroplating
Pharma

Food

Mineral oil Cosmetics

Plastics Detergents

Basics of titration 25 GTP™

 Agenda

 Welcome
 Definition of Titration
 Chemical reactions for Titration
 Measurement Techniques
 Titration Types
 Titration Techniques
 Introduction to GTP™
 Summary

Basics of titration 26 GTP™

 Good Titration PracticeTM

Approach

 Validation approach is designed to find best possible

Establishing documented evidence which provides a high degree of assurance that a specific
process will consistently produce a product meeting its pre-determined specifications and quality
attributes
(FDA definition of process validation on
http://www.fda.gov/Drugs/GuidanceComplianceRegulatoryInformation/Guidances/
ucm124720.htm)

 Aims for most suitable system for intended use (“fit for purpose”)
 Is applicable to the process of purchasing, installing and using analytical
systems
 It is based on your requirements, circumstances, risks etc. and takes the
whole life time of the analytical system into consideration

Basics of titration 27 GTP™

 Good Titration PracticeTM

GTPTM is based on validation principles

 Same goal
- Establishing documented evidence which provides a high degree of
assurance that a specific titration system will consistently produce results
meeting their pre-determined specifications and quality attributes
 Risk-based approach
- Risks are inherent in every process, also in the generation of titration results
- Risks are identified and addressed
 Life-cycle approach
- Includes the first idea to buy a titration system until its replacement / disposal
- Considers the complete process, from receiving and preparing the sample till
the integration of the analysis result into your data system
- Takes total costs of ownership into account, not just initial investments

GTP
TM

Good Titration PracticeTM

Basics of titration 28 GTP™
 Good Titration PracticeTM

GTPTM is based on a defined set of activities

Disposal / Replacement
Need for analytical system

Evaluation / Selection

Oper ation

Ready for use Purchase / receive

titration system
Installation / Qualification

 5 stages over the whole life cycle of the titration system

(evaluation, selection, installation, qualification, routine operation)

Basics of titration 29 GTP™

 5 Stages of GTPTM

Evaluation and selection

 Specify and document your requirements

 Find suitable technique ( titration)
 Find most suitable titration supplier in terms of
- Competence and experience (reference customers, installed base)
- Quality standards applied during development and production
- Quality of offered products and services
 Find most suitable titration system based on your requirements on
- Result quality (accuracy, precision, trustworthiness, reliability)
- Compliance (regulations and guidelines)
- Safety (for human and environment)
- Costs (total cost of ownership)
 And proof it with suitable documentation
 At the end of this stage, the titration system is purchased and delivered
Basics of titration 30 GTP™
 5 Stages of GTPTM

Installation and qualification

 Make sure
- System is installed as specified
- System is qualified as specified
- SOPs are written
- Training as specified is provided to users
- Other activities are performed if specified (examples)
 Method development / validation
 Evaluation of measurement uncertainty

 And proof it with suitable documentation

 At the end of this stage, the titration system and its environment is ready
for routine use

Basics of titration 31 GTP™

 5 Stages of GTPTM

Routine operation

 Make sure
- System is used as specified
- Re-qualification is performed as specified
- Maintenance is performed as specified (user)
- Maintenance is performed as specified (supplier)
- Other activities are performed if needed (examples)
 Repairs
 Exchange consumables
 Development of new applications
 More training

 And proof it with suitable documentation

 At the end of this stage, the titration system is retired or replaced

Basics of titration 32 GTP™

 Agenda

 Welcome
 Definition of Titration
 Chemical reactions for Titration
 Measurement Techniques
 Titration Types
 Titration Techniques
 Introduction to GTP™
 Summary

Basics of titration 33 GTP™

 Summary

GTP™ to your benefit

 Helps you to find suitable titration system for you
- Makes you aware of possible risks and provides you with suggestions to address
these risks
- Helps you to reduce overall costs
- Helps you in your efforts to become compliant
- Helps you to increase operator safety
- Helps you to achieve high result quality

 Helps you to install and qualify the titration system professionally

- Saves you time from the purchase to the release for routing operation by providing
appropriate documentation and services like e.g. training

 Helps you to get maintain high-quality during routine use

- Provides practical tips and tricks
- Provides suitable services like maintenance Summary

Basics of titration 34 GTP™

 Questions

Basics of titration 35 GTP™