Chapter 5 P1_Volumetric titration NTLP

CHAPTER 5

VOLUMETRIC TITRATIONS

Contents
5.1. Principles of the volumetric analysis
5.2. Reactions used in volumetric titration
5.3. Titration curves and equivalence point
5.4. Indicators
5.5 Volumetric calculations
5.6 Application in food analysis

1
Chapter 5 P1_Volumetric titration NTLP

5.1. Principles of the volumetric

analysis
 Volumetric titration involve measuring the
volume of a solution of known concentration that
is needed to react completely with the analyte.
 Titration (analyte / titrand)
 Standard solution (standard titrant)
 Indicators
 Titration curve; Equivalence point ; End point
 Titration error

Volumetric Titration
• Adding slowly a standard reagent,
called the titrant C (known
concentration, CC) into a controled
volume of sample solution
containing the analyte or titrand X
(VX mL), allow them to react, until
an obvious sign occurs (usually a
change in the color)
•  Stop adding the titrant then read
the used-volume of C (VC mL).
• Calcultate the concentration of X
(CX) following stoichiometrically
equivalent amount of titrant and
titrand.

2
Chapter 5 P1_Volumetric titration NTLP

Types of reactions in titration

 Neutralization reaction/titration (acid/base

reaction)
 Complexation reaction/titration
 Precipitation reaction/titration
 Redox reaction/titration

Reactions in titration
 Titration reactions

 Indicator reactions

At the equivalence point,

=

Cc.Vc = Cx.Vx

3
Chapter 5 P1_Volumetric titration NTLP

Types of titration curves

 provides a visual picture of how a property of the titration
reaction changes as we add the titrant to the analyte

Titration curves – example (cont.)

 (a) Complexation titration of 25.0 mL of 1.0 mM Cd2+ with 1.0 mM

EDTA at a pH of 10 (titrand’s equilibrium concentration as pCd).
 (b) Redox titration of 25.0 mL of 0.050 M Fe2+ with 0.050 M Ce4+ in 1
M HClO4 (titration mixture’s electrochemical potential, E, through the
Nernst equation is a logarithmic function of concentrations.
 (c) Precipitation titration of 25.0 mL of 0.10 M NaCl with 0.10 M
AgNO3. (titrant’s equilibrium concentration as pAg).

4
Chapter 5 P1_Volumetric titration NTLP

Titration Modes
 Titration curves define the properties required of an
indicator or instrument and allow us to estimate the error associated
with titration methods.

Titration Modes
 Equivalent point (EQP) is a theoretical point in
a titration when the amount of added standard
reagent is equivalent to the amount of analyte.
 Veq (theoretical)
 Example:
 Titration of NaCl with AgNO3 occurs after exactly 1
mole of Ag+ has been added for each mole of Cl- in
the sample.
 Titration of H2SO4 with OH- is reached after
introducing 2 moles of base for each mole of acid.

5
Chapter 5 P1_Volumetric titration NTLP

Titration Modes
 End point (f) is the point in a titration when a
physical change occurs that is associated with
the condition of chemical equivalence.
 Vf (practical)
 Ensure that any volume or mass difference between
the equivalence point and the end point is small.
 The accuracy of titration will be high when the end
point is quite close to the equivalence point

Titration Modes
 Vf = Veq; Vf > Veq; Vf < Veq
 Stop the titration at equivalence point: Vf = Veq

 Stop the titration near equivalence point (before or after)

 Titration error, the difference in volume or mass

between the equivalence point and the end point.
Et = Vf – Veq

 Vf: the actual volume of reagent required to reach the end point
 Veq: the theoretical volume necessary to reach the equivalence
point.

6
Chapter 5 P1_Volumetric titration NTLP

Titration Modes

Determination of the end point:

 Visual (Using indicator – Classical method)

 Instrument (Modern method) potentiometric

titration

Indicators

 Redox indicators
 Acid-base indicators
 Complexation indicators
 Precipitation indicators
 Adsorption indicators

7
Chapter 5 P1_Volumetric titration NTLP

Some common titration techniques

 Direct titration

 Back titration

 Indirect titration

 Blank compensated titration

DATA CALCULATION

 Stoichiometry and equivalent number

 Liquid sample:
• Vx ml sample soln. titrate with VC ml of titrant (CC)

CC .VC
C N (X) 
VX

CC .VC
C g/L(X)   Eq X  C N (X) .Eq X  C M (X) .M X
VX

8
Chapter 5 P1_Volumetric titration NTLP

DATA CALCULATION
Solid sample:
 a (g) of sample, dilution and titration with a titrant
C (VC (ml), known CC)

100
%X  CC .VC .10 3. .Eq X
a

Volumetric calculations
 mol, mmmol, eq., mmeq

mol A 
amount A (mol) Vsolution ( L)C A  
 L 
mmol A 
amount A (mmol) Vsolution ( L)C A  
 L 

9
Chapter 5 P1_Volumetric titration NTLP

Application to food analysis

 Kjeldahl Method – Protein analysis
 Calculation of titratable acidity
 Mineral analysis

10