Precipitation Titration by Sitesh

Precipitation titration/Argentometric Titration
DEPT. OF PHARMACY
Qualifications- Presented by-

Sitesh sah
GPAT(All India rank-154)
M. Pharmacy(Pharmaceutical Analysis)
NIPER JEE(All India rank-75)
NIPER-Ahmedabad
Working at Deurali Janta Pharmaceuticals
INTRODUCTION FLOW OF PRESENTATION
BASIC TERMINOLOGIES IN TITRATION
TYPES OF PRECIPITATION TITRATION
MOHR’S METHOD
VOLHARD’S METHOD
FAJANS’S METHOD
ADVANTAGE & LIMITATION

2
Some important terms in titration process:
1. Analyte/Titrand: The solution of unknown concentration but known

volume put in conical flask.
2. Titrant: The solution of known concentration put in burette.
3. Equivalent Point: It is a theoretical point where the amount of two
reactants are just equivalent.
4. End point: It is a practical point at which the reaction is observed to be
complete, this point is usually observe with the help of indicator.
5. Indicator: An conducive material used to identify the outcome of the
titration process. They change color in a pH range.
3
PRINCIPLE & INTRODUCTION
 Principle
Those titration in which chemical reaction takes place and they will form precipitate
Also called as argentometric titration because of use of AgNO 3 as titrant.(Latin name for silver, argentum)
Used for analysis of:
Halides (Cl- , Br- , I- )
Pseudo halides (S 2- , HS- , CN- , SCN- )
Example; NaCl + AgNO3 →AgCl( )+ NaNO3
In Above reaction: Ag+ • Is precipitating Agent
Cl- • Is Analyte
• Is
AgCl precipitate
4
Basic requirement
 Precipitate must be practically insoluble.

 Precipitation must be rapid and stoichiometric
 Suitable method should be there to determine end point.
5
TYPES OF PRECIPITATION TITRATION
Mohrs method : Colored ppt. is formed

Is direct method
Use chromate as indicator
Fajans method : Use Adsorption indicator

Is direct method
Volhards method : Colored Solution is formed

Indirect method
Excess of silver ion is added to sample
and remaining silver ion is back titrated.
6
Mohr’s Method
 This is direct method uses potassium chromate as an indicator in the

titration of (Cl- , Br- , and CN- )ions (analyte) with a silver nitrate
standard solution (titrant).
 Iodides cant be determined by Mohr's method because iodide itself
produce colour precipitate with silver ions.
 After all the chloride has been precipitated as white silver chloride, the first
excess of titrant results in the formation of a silver chromate precipitate
(brick red color precipitate).
 Example: Titration of NaCl by using AgNO3 in presence of K2CrO4 as
indicator
 Principle
1. NaCl + AgNO3 →AgCl+ NaNO3
2. K2CrO4 + 2AgNO3 →Ag2CrO4+ 2KNO3
7
Conditions for Mohr’s method
 The titrations Cant be performed in basic medium because Ag+ will be

precipitated as silver hydroxide.
 It cant be carried out in presence of ammonium ion because ammonia
acts as chelating agent and ligand formation takes place.
 It cant be carried out in presence of reducing agent because CrO42- will
be reduced as Cr3+ .
 It cant be carried out in presence of anions like Po43- ,S2- because it will
give colored precipitate.
8
Volhard’s Method
 The volhard method is an indirect or back titration method in which an

excess of a standard solution of silver nitrate is added to a chloride
containing sample solution.
 The excess silver is then back titrated using a standardized solution of
potassium or ammonium thiocyanate with ferric ion as an indicator.
 The reaction between the silver ions and thiocyanate ions produces a
complex ion, silver thiocyanate (AgSCN), which is soluble in water and has
a red color.
 Indicator; Iron alum or Ferric ammonium sulphate
 This method is carried out in acidic medium because in basic medium Fe 3+
may form ferric hydroxide.
 Principle Ag+ + Cl- ⇾ AgCl
Ag+ + SCN- ⇾ AgSCN

9
- 3+ 2+
Modified Volhard’s Method
 Chloroform or nitrobenzene or other wetting agent is added after addition of

excess silver nitrate.
 These agents will form a layer surrounding the precipitate of silverchloride ,
preventing solubility of AgCl.
10
Fajans’s Method
 Fajans method is based on mechanism of adsorption.

 It is used to determine chlorides, bromides and iodides.
 Titrant; Standardized AgNo3
 Indicator;
1. Acidic dye-Fluorescien and eosin
2. Basic dye-Rhodamine, phenosafranine
 Principle NaCl + AgNO3 →AgCl+ NaNO3
AgCl + AgNO3 + Fluorescein-⇾ AgCl Ag+ Fluorescein-
(Complex of pink color)
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Fajans’s Method
 Mechanism:
Before equivalence point At end point
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Effect on solubility of Precipitate
1. Effect of acids: Solubility of salt will be increased by decrease in pH

value
2. Effect of Temperature: Solubility of most inorganic salt will be increased
by increase in temperature.
3. Effect of Solvent: Most of the inorganic solvent are more soluble in
water because it shows dipole moment and attracts cations as well as
anions. These cations and anions are converted into hydrated form
because of water.
13
Advantage of precipitation titration
 Has high precision and accuracy.

 Simple and easy to use, doesn’t require complex instrumentation.
 Low cost method
 Used to determine wide range of analyte including Halides, Sulfates and phosphates .
Limitation of precipitation titration
 Precipitation titration can be affected by presence of interfering ions.

 Precipitation titration requires large sample size.
 It is very difficult to detect end point.
14
15
TENTATIVE TIMELINE
2018(third semm) 2019(fourth semm.)
JUN JUL AUG SEP OCT NOV DEC JAN FEB MAR APR MAY
Literature survey
Characterization
of drug
Bioanalytical
method
development &
Selection of
sample extraction
technique
Bioanalytical
method
Validation COMPLETED
In vivo
pharmacokinetic
study
REMAINING 20
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Precipitation titration/Argentometric Titration

Qualifications- Presented by-

BASIC TERMINOLOGIES IN TITRATION

TYPES OF PRECIPITATION TITRATION

ADVANTAGE & LIMITATION

1. Analyte/Titrand: The solution of unknown concentration but known

Example; NaCl + AgNO3 →AgCl( )+ NaNO3

In Above reaction: Ag+ • Is precipitating Agent

 Precipitate must be practically insoluble.

Mohrs method : Colored ppt. is formed

Fajans method : Use Adsorption indicator

Volhards method : Colored Solution is formed

 This is direct method uses potassium chromate as an indicator in the

 The titrations Cant be performed in basic medium because Ag+ will be

 The volhard method is an indirect or back titration method in which an

Ag+ + SCN- ⇾ AgSCN

 Chloroform or nitrobenzene or other wetting agent is added after addition of

 Fajans method is based on mechanism of adsorption.

Before equivalence point At end point

1. Effect of acids: Solubility of salt will be increased by decrease in pH

 Has high precision and accuracy.

Limitation of precipitation titration

 Precipitation titration can be affected by presence of interfering ions.

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