CHEM 261 Lecture Note 1

Kwame Nkrumah University of
Science & Technology, Kumasi, Ghana
CHEM 261
TITRIMETRIC METHODS OF ANALYSIS
Prof Godfred Darko

Department of Chemistry
Faculty of Physical and Computational Sciences
COURSE OUTLINE
a) Basic concepts of analytical chemistry:
i. Introduction and treatment of analytical data
ii. Statistical treatment of analytical data
b) Titrimetric analysis
iii. Acid-Base titration
iv. Complexometric titration
v. Precipitation titration
vi. Redox titration
References
 Harris, D.C. Quantitative Chemical Analysis. 6 th Edition
 Miller, J.C. and Miller, J.N. Statistics for Analytical Chemistry. 3 rd Edition
 Harvey, D. Modern Analytical Chemistry. 1st Edition.
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COURSE MATERIALS
Lecture notes (DropBox)
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Lecture via ZOOM
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Introduction Basic concepts
Chemical analysis includes any aspect
of the chemical characterization of a
sample
Analytical Chemistry?
◦ “Science of Chemical Measurements”
Characterization analysis
An analysis in which a sample’s chemical or physical properties are
evaluated
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Areas of chemical analysis and
questions asked
Quantitation:
◦ How much of substance X is in the sample?
Detection:
◦ Does the sample contain substance X?
Identification:
◦ What is the identity of the substance in the sample?
Separation:
◦ How can the species of interest be separated from the sample
matrix for better quantitation and identification?
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What is analytical chemistry
Analytical Chemistry provides the methods and
tools needed for insight into our material
world…
for answering four basic questions about a
material sample?
o What?
o Where?
o How much?
o What arrangement, structure or form?
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What do Chemical Analyst Do?
• Research Analytical Chemist:
Creates and /or investigates novel
techniques or principles for chemical
measurements
or
Conducts fundamental studies of
chemical/physical phenomena
underlying chemical measurements
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Role of analytical chemistry
Analytical chemists work to improve the reliability of
existing techniques to meet the demands of for better
chemical measurements which arise constantly in our
society
o They adapt proven methodologies to new kinds of

materials or to answer new questions about their
composition
o They carry out research to discover completely new

principles of measurements and are at the forefront
of the utilization of major discoveries such as lasers
and microchip devices for practical purposes
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History of analytical chemistry
Classical methods: early years (separation of analytes)
via precipitation, extraction or distillation
o Qualitative: recognized by color, boiling point,
solubility, taste
o Quantitative: gravimetric or titrimetric
measurements
o Instrumental Methods: newer, faster, more
efficient
o Physical properties of analytes: conductivity,
electrode potential, light emission absorption, mass
to charge ratio and fluorescence, many more…
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Numbers in Analytical Chemistry
Measurements usually consist of a unit and a number
expressing the quantity of that unit
Many different units may be used to express the same
physical measurement
For consistency, scientists use a common set of
fundamental units
These units are called SI units after the Système
International d’Unités
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Fundamental SI Units
Measurement Unit Symbol
mass kilogram kg
volume litre L
distance metre m
temperature kelvin K
time second s
current ampere A
amount of substance mole mol
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Other SI and non-SI Units
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scientific notation
A shorthand method for expressing very
large or very small numbers by indicating
powers of ten; for example, 1000 is 1 × 103
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Common Prefixes for Exponential Notation
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Significant Figures
Recording a measurement provides information
about both its magnitude and uncertainty (error
associated with the measurement)
It is assumed that all digits, except the last,
are known exactly
Significant figures indicate the uncertainty
associated with a measurement
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Significant Figures
Significant figures indicates the uncertainty
associated with a measurement
The number of significant figures is equal to
the number of digits in the measurement, with
the exception that a zero (0) used to fix the
location of a decimal point is not considered
significant
1 × 102 has one significant figure
1.0 × 102 has two significant figures
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Significant Figures
For measurements using logarithms, such as pH,
the number of significant figures is equal to the
number of digits to the right of the decimal,
including all zeros
Digits to the left of the decimal are not included
as significant figures since they only indicate
the power of 10
A pH of 2.45, therefore, contains two significant
figures
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Significant Figures
Exact numbers, such as the stoichiometric coefficients
in a chemical formula or reaction, and unit conversion
factors, have an infinite number of significant figures
A mole of CaCl2, contains exactly two moles of chloride

and one mole of calcium
CaCl2 Ca + 2Cl
both have an infinite number of significant figures
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Significant Figures
For mathematical operations involving addition and
subtraction, the last digit that is significant for all
numbers included in the calculation
3.63 cm
13.129 cm
+123.1 cm
139.859 cm = 139.9 cm
significant to the 0.1

place
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Significant Figures
All non-zero digits are significant
Zeros at the end of a measurement?
scientific notation:
5000 5 x 103
5000 5.0 x 103
5000 5.00 x 103
5000
5.000 x 103
5000.0
5.0000 x 103
5000.00
5.00000 x 103
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Significant Figures
1. Retain the least significant figure if it and the digits that
follow are less than halfway to the next higher digit; thus,
rounding 12.442 to the nearest tenth gives 12.4 since 0.442 is
less than halfway between 0.400 and 0.500
2. Increase the least significant figure by 1 if it and the digits

that follow are more than halfway to the next higher digit;
thus, rounding 12.476 to the nearest tenth gives 12.5 since
0.476 is more than halfway between 0.400 and 0.500
3. If the least significant figure and the digits that follow are
exactly halfway to the next higher digit, then round the least
significant figure to the nearest even number; thus, rounding
12.450 to the nearest tenth gives 12.4, but rounding 12.550 to
the nearest tenth gives 12.6. Rounding in this manner prevents
us from introducing a bias by always rounding up or down
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Concentration expressions
An expression stating the relative amount of solute

per unit volume or unit mass of solution
Concentration is a general measurement unit stating

the amount of solute present in a known amount of
solution
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Molarity and Formality
Molarity
Concentration of a particular chemical species in solution
The number of moles of solute per liter of solution (M)
Formality
a substance’s total concentration in solution without
regard to its specific chemical form
The number of moles of solute, regardless of chemical
form, per liter of solution (F)
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There is no difference between a substance’s molarity
and formality if it dissolves without dissociating into ions
For example, the molar concentration of a glucose solution

the same as its formality because glucose does not ionize
upon dissolution in solution
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For substances that ionize in solution, such as NaCl,
molarity and formality are different
For example, dissolving 0.1 mol of NaCl in 1 L of water

gives a solution containing 0.1 mol of Na+ and 0.1 mol of Cl–
The molarity of NaCl, therefore, is zero since there is
essentially no undissociated NaCl in solution
The solution instead, is 0.1 M in Na+ and 0.1 M in Cl–. The

formality of NaCl, however, is 0.1 F because it represents
the total amount of NaCl in solution
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Common Units of Concentration
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Normality
The number of equivalents of solute per litre of solution
(N)
=
Normality makes use of the chemical equivalent, which is

the amount of one chemical species reacting
stoichiometrically with another chemical species
Normality is a function of the chemical reaction in which

the species participates
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Normality
The number of equivalents, n, is based on a reaction unit,
which is that part of a chemical species involved in a
reaction
In a precipitation reaction, the reaction unit is the
charge of the cation or anion involved in the reaction;
thus for the reaction
n for Pb2+ =2; n for I- = 1
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Normality
In an acid–base reaction, the reaction unit is the number
of H+ ions donated by an acid or accepted by a base
n for H2SO4 =2; n for NH3 = 1
For a complexation reaction, the reaction unit is the

number of electron pairs that can be accepted by the
metal or donated by the ligand
n for Ag =2; n for NH3 = 1
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Normality
in an oxidation–reduction reaction the reaction unit is
the number of electrons released by the reducing agent
or accepted by the oxidizing agent
n for Fe3+ =1; n for Sn2+ = 2
Clearly, determining the number of equivalents for a

chemical species requires an understanding of how it
reacts
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Normality
Normality is the number of equivalent weights (EW) per
unit volume and, like formality, is independent of
speciation
An equivalent weight is the ratio of a chemical species’
formula weight (FW) to the number of its equivalents
Thus, normality and molarity relate as:
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For phosphoric acid, the number of equivalents is the
number of H+ ions donated to the base
For the reactions in (a), (b), and (c) the number of
equivalents are 3, 2, and 1, respectively
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Weight, Volume, and Weight-to-Volume Ratios
Weight percent (% w/w), volume percent (% v/v) and

weight-to-volume percent (% w/v) express
concentration as units of solute per 100 units of sample
weight percent = Grams of solute per 100 g of solution

(% w/w)
weight-to-volume percent = Grams of solute per 100 mL
of solution (% w/v)
Eg., A solution in which a solute has a concentration of
10% w/v contains 10 g of solute per 100 mL of solution
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Weight, Volume, and Weight-to-Volume Ratios
parts per million = Micrograms of solute per gram of

solution; for aqueous solutions the units are often
expressed as milligrams of solute per liter of solution
(ppm)
parts per billion = Nanograms of solute per gram of

solution; for aqueous solutions the units are often
expressed as micrograms of solute per litre of solution
(ppb)
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Converting Between Concentration Units
Example,
A steel that is 450 ppm in Mn contains 450 µg of Mn for
every gram of steel
A helium concentration of 6.3 ppm means that one liter of

air contains 6.3 µL of He
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A concentrated solution of aqueous ammonia is 28.0%
w/w NH3 and has a density of 0.899 g/mL. What is
the molar concentration of NH3 in this solution?
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The maximum allowed concentration of chloride in a
municipal drinking water supply is 2.50 × 102 ppm Cl–.
When the supply of water exceeds this limit, it
often has a distinctive salty taste. What is this
concentration in moles Cl–/litre?
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p-Functions
When working with concentrations that span many
orders of magnitude, it is often more convenient to
express the concentration as a p-function
The p-function of a number X is written as pX and is

defined as
pX = –log(X)
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p-Functions
the pH of a solution that is 0.10 M H+ is
pH = –log[H+] = –log(0.10) = 1.00
and the pH of 5.0×10–13 M H+ is
pH = –log[H+] = –log(5.0 × 10–13) = 12.30
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Question
What is pNa for a solution of 1.76×10–3 M Na3PO4?
Solution
and pNa is
pNa = –log[Na+] = –log(5.28 × 10–3) = 2.277
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Basic Equipment and Instrumentation
Measuring Mass
An object’s mass is measured using a balance
A balance determines mass by

balancing an unknown mass against
a known mass
Modern balances usually use a
force restoration mechanism that
creates a force to balance the
force exerted by the unknown
mass
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Measuring Mass
sample is placed on the sample pan, displacing the pan
downward by a force equal to the product of the
sample’s mass and the acceleration due to gravity
The balance detects this downward movement and
generates a counterbalancing force using an
electromagnet
The current needed to produce this force is
proportional to the object’s mass
A typical electronic balance has a capacity of 100–200 g
and can measure mass to the nearest ±0.01 to ±1 mg
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Measuring Mass
If the material being weighed is not moisture-sensitive,

a clean and dry container is placed on the balance
The mass of this container is called the tare
Most balances allow the tare to be automatically

adjusted to read a mass of zero
The sample is then transferred to the container, the
new mass is measured and the sample’s mass determined
by subtracting the tare
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Measuring Mass
For samples that absorb moisture from the air;
The sample is placed in a covered weighing bottle and

their combined mass is determined
A portion of the sample is removed, and the weighing
bottle and remaining sample are reweighed
The difference between the two masses gives the mass
of the transferred sample
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Measuring Mass
For samples that absorb moisture from the air;
The sample is placed in a covered weighing bottle and

their combined mass is determined
A portion of the sample is removed, and the weighing
bottle and remaining sample are reweighed
The difference between the two masses gives the mass
of the transferred sample
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Precautions Measuring Mass
Balances should be placed on heavy surfaces to minimize
the effect of vibrations in the surrounding environment
and should be maintained in a level position
Materials placed on a balance should normally be handled
using tongs: analytical balances are sensitive enough that
they can measure the mass of a fingerprint
Volatile liquid samples should be weighed in a covered
container to avoid the loss of sample by evaporation
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Precautions Measuring Mass
Air currents can significantly affect a sample’s mass. To
avoid air currents, the balance’s glass doors should be
closed, or the balance’s wind shield should be in place
A sample that is cooler or warmer than the surrounding
air will create convective air currents that adversely
affect the measurement of its mass
Samples dried in an oven should be stored in a desiccator
to prevent them from reabsorbing moisture from the
atmosphere
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Measuring Volume
The type of glassware used depends on how exact

the volume needs to be
Beakers, dropping pipets, and graduated cylinders are
used to measure volumes approximately, typically with
errors of several percent
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Measuring Volume
The type of glassware used depends on

how exact the volume needs to be
Beakers, dropping pipets, and graduated
cylinders are used to measure volumes
approximately, typically with errors of
several percent
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Measuring Volume
Pipette
Volumetric flask
Measuring cylinder
A pipette is used to deliver a specified volume of solution

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Measuring Volume
Measuring pipette
Transfer pipette Digital pipette
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CHEM 261 Lecture Note 1

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Kwame Nkrumah University of

Science & Technology, Kumasi, Ghana

TITRIMETRIC METHODS OF ANALYSIS

Prof Godfred Darko

Meeting ID: 666 0943 3307

o They adapt proven methodologies to new kinds of

o They carry out research to discover completely new

A mole of CaCl2, contains exactly two moles of chloride

both have an infinite number of significant figures

significant to the 0.1

2. Increase the least significant figure by 1 if it and the digits

An expression stating the relative amount of solute

Concentration is a general measurement unit stating

For example, the molar concentration of a glucose solution

For example, dissolving 0.1 mol of NaCl in 1 L of water

The solution instead, is 0.1 M in Na+ and 0.1 M in Cl–. The

Normality makes use of the chemical equivalent, which is

Normality is a function of the chemical reaction in which

n for Pb2+ =2; n for I- = 1

n for H2SO4 =2; n for NH3 = 1

For a complexation reaction, the reaction unit is the

n for Ag =2; n for NH3 = 1

n for Fe3+ =1; n for Sn2+ = 2

Clearly, determining the number of equivalents for a

Thus, normality and molarity relate as:

Weight percent (% w/w), volume percent (% v/v) and

weight percent = Grams of solute per 100 g of solution

parts per million = Micrograms of solute per gram of

parts per billion = Nanograms of solute per gram of

A helium concentration of 6.3 ppm means that one liter of

The p-function of a number X is written as pX and is

the pH of a solution that is 0.10 M H+ is

pH = –log[H+] = –log(0.10) = 1.00

and the pH of 5.0×10–13 M H+ is

pH = –log[H+] = –log(5.0 × 10–13) = 12.30

A balance determines mass by

If the material being weighed is not moisture-sensitive,

Most balances allow the tare to be automatically

For samples that absorb moisture from the air;

The sample is placed in a covered weighing bottle and

For samples that absorb moisture from the air;

The sample is placed in a covered weighing bottle and

The type of glassware used depends on how exact

The type of glassware used depends on

A pipette is used to deliver a specified volume of solution

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