Unit 7 General Concept of Volumetric Titrimetry UST Template

UNIT 7 
General Concept of  
Volumetric Titrimetry
maidliu 04.25.2019
Titrimetric Method
• These include analytical methods that are based on
determining the amount of reagent of known
strength that is required to react completely with
the analyte.
Types of Titrimetry
1. Volumetric Titrimetry – the standard reagent
(titrant) is measured volumetrically
2. Gravimetric Titrimetry – the mass of standard
reagent is measured
3. Coulometric Titrimetry – the quantity of a
constant, direct electrical current of known
magnitude is measured
Definition of Terms
• Analyte: the chemical component in the sample
that is to be determined.
• Titrant: solution (usually placed in the buret)
that quantitatively reacts with the analyte.
• Standard solution: a reagent of known
concentration.
• Titration: it is based on the reaction between
the analyte and the titrant
• It is a process of measuring the volume of a solution (of
known concentration) that is needed to react
completely with the analyte.
Definition of Terms
• Equivalence point: theoretical point in
titration when the amount of titrant is
chemically equivalent to the amount of
analyte in the sample.
• Endpoint: experimental estimation of
equivalence point; point in titration when a
physical change occurs at or near the
equivalence point.
• Titration error : the difference in volume
or mass between the equivalence point and
end point.
• Indicator: substance that undergoes an
observable change when endpoint of a
titration is reached.
Basic Requirements in Titration
1. Successful titrations are based on reactions
that are stoichiometric, quantitative and
fast.
2. Titrant must be stable, of known

concentration (standard solution) and
selectively reacts with the analyte.
Properties of Standard Solution
1. It should be sufficiently stable.
2. It reacts rapidly and completely with the
analyte.
3. It undergo selective reaction with the analyte.
??? How to prepare a standard solution?

Standardization: the process of determining the
exact concentration of the solution.
Preparation of Standard Solution
1. Standardize using weighed quantity of primary
standard
Primary standard: highly purified compound that serves
as reference material for titrimetric analysis.
Requirements for a primary standard

• High purity (preferably 99.9% or better)
• Atmospheric stability
• Absence of hydrate water
• Available at modest cost
• Soluble in titration medium
• Has large molar mass to minimize relative error
associated with weighing
Preparation of Standard Solution
2. Standardize using weighed quantity of
secondary standard
3. Standardize using a measured volume of

another standard solution
Secondary standard solution: a solution that is
standardized against another standard solution
Basic Requirements in Titration
3. Endpoints of titrations must occur at or near
equivalence point.
Typical indicator changes in titration:

• Appearance/Disappearance of a color
• Change in color
• Appearance/Disappearance of turbidity
Classification of Volumetric Titrimetry
Based on the reaction involved between analyte
and titrant:
• Acid-base or neutralization titration
• Precipitation titration
• Complexation titration
• Oxidation-reduction titration
Based on how the amount of analyte is
determined:
• Direct Titration Method
• Replacement/Indirect Titration Method
• Back-titration
• Direct Titration Method: the titrant directly
reacts with the analyte.
Stoichiometric relationship can be expressed:

amountanalyte = amounttitrant X r.r.
wherein, reacting ratio (r.r.) depends on the

balanced chemical reaction;
Analyte + Titrant ! Product
The amount of analyte/titrant is expressed in

units of moles or millimoles.
Problem Set
1. A 50.00mL portion of HCl solution required
29.71mL of 0.01963 M Ba(OH)2 to reach an
endpoint with bromocresol green indicator.
Calculate the molarity of the HCl.
Ba(OH)2 + 2HCl ! BaCl2 + 2H2O
Answer: 0.02333 M
Problem Set
2. Titration of 0.2121 g pure Na2C2O4 (134.00g/
mol) required 43.31 mL of KMnO4. What is the
molarity of the KMnO4 solution?
2MnO4— + 5C2O42— + 16H+ ! 2Mn2+ + 10CO2 +
8H2O
Answer: 0.01462 M
Problem Set
3. A sample of powdered milk weighing 1.450g
was mixed with an aqueous buffer of pH 11.5. A
few drops of Calmagite indicator were added and
the solution required 31.62mL 1.538 x 10—2M
EDTA to reach the endpoint color change.
Calculate the percentage Ca in the milk.
Ca2+ + Y4— ! CaY2-
Answer: 1.344% Ca
• Replacement/Indirect titration method: the analyte is
converted to another substance by a preliminary reaction.
This new substance (X) is directly proportional to the
amount of analyte. This new substance is then determined
by titration.
Analyte + Y ! X (Reaction 1)
X + Titrant !Product (Reaction 2)
Based on balanced chemical reactions 1 and 2:
amountX = amounttitrant X r.r.2
amountanalyte = amountX X r.r.1
Combining these two equations will give:
amountanalyte = amounttitrant X r.r.2 X r.r.1
Problem Set
4. A 750.0-mg sample of iron ore was dissolved in
acid and treated to oxidize all the iron to ferric
ion. After destroying any remaining oxidizing gent,
excess KI was added. The liberated I2 required
28.50mL of 0.07500M Na2S2O3 for titration. What is
the %Fe in the sample? (AW Fe 55.85g/mol)
2Fe3+ + 2I— ! 2Fe2+ + I2
I2 + 2S2O32— ! 2I— + S4O62—
Answer: 15.92% Fe
Problem Set
5. Titration of the I2 produced from 0.1045g of
primary standard KIO3 required 30.72mL of sodium
thiosulfate. Calculate the concentration of the
Na2S2O3.
IO3— + 5I— + 6H+ ! 3I2 + 3H2O
I2 + 2S2O32— ! 2I— + S4O62—
Answer: 0.09537M Na2S2O3

• Back-titration method: the analyte is made to react with
a known amount of excess standard solution. The excess
reagent is titrated with a second standard solution.
Analyte + Titrant1 ! Product1 + excess Titrant1 (Reaction

1)
Excess Titrant1 + Titrant2 ! Product2 (Reaction 2)
To obtain the amount of Titrant1 used to react with analyte:

amounttitrant1 used = total amounttitrant1 - amountexcess titrant1
amountexcess titrant1 = amounttitrant2 X r.r.2
Finally, to calculate the amount of analyte:

amountanalyte = amounttitrant1 used X r.r.1
Problem Set
6. A antihistamine sample, brompheniramine maleate,
weighing 4.6330g was dissolved in alcohol and
decomposed with metallic sodium. The resulting solution
was treated with 10.00mL of 0.2500M AgNO3, an amount
sufficient to precipitate all of the liberated bromide ion
as AgBr. The excess AgNO3 was titrated with 0.1214M
KSCN, requiring 14.42mL to reach the endpoint.
Calculate %Br in the sample.
Br— + Ag+ ! AgBr(s)
Ag+ + SCN— ! AgSCN(s)
Answer: 1.29% Br
Problem Set
7. An 800.0mg sample of chromium ore was
dissolved and the chromium oxidized to chromate
ion. The solution was treated with 10.0mL of
0.200M AgNO3. The resulting precipitate of Ag2CrO4
was removed and discarded. The excess AgNO3
required 14.50mL of 0.1200 M KSCN. Calculate the %
Cr2O3 in the ore.
CrO42— + 2Ag+ ! Ag2CrO4(s)
Ag+ + SCN— ! AgSCN(s)
Answer: 1.29% Br
Assignment
Skoog
7-16
7-19
7-22
7-24 a
11-14
11-16 a

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UNIT 7

2. Titrant must be stable, of known

??? How to prepare a standard solution?

Requirements for a primary standard

3. Standardize using a measured volume of

Typical indicator changes in titration:

Stoichiometric relationship can be expressed:

wherein, reacting ratio (r.r.) depends on the

The amount of analyte/titrant is expressed in

Answer: 0.09537M Na2S2O3

Analyte + Titrant1 ! Product1 + excess Titrant1 (Reaction

To obtain the amount of Titrant1 used to react with analyte:

Finally, to calculate the amount of analyte:

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