CHAPTER 1

INTRODUCTION:
ANALYTICAL CHEMISTRY

OUTLINE
Review the type and steps in analysis
Review the terms: Moles, molarity and
concentration.
Review other forms of expressing
concentration:
[ppm, ppb, ppt, %(w/w), %(w/v), %(v/v)]

LEARNING OUTCOME
In this chapter, you should be able to:
Differentiate between qualitative &
quantitative analysis
Explain the steps involve in quantitative
analysis
Calculate the concentration of solution
Explain the preparation of solution

IMPORTANCE OF
ANALYTICAL CHEMISTRY
Analytical chemistry is used to collect necessary data to
solve problems throughout many fields of science such
as:
Industry, Medicine, Environmental Studies, Chemistry,
Biology, Agriculture, Materials Science, Archeology,
Forensic Science, Geology, Physics, Engineering, etc.

WHAT IS ANALYTICAL
CHEMISTRY ?
Provides the methods and tools needed for insight into
our material world and answering four basic questions
about a material sample:
What? Where?
How much? What arrangement, structure or form?

The technique used to identify the substance which

may be present in a material and to determine the
exact amount of the identified substance

DISCIPLINE OF ANALYTICAL
CHEMISTRY
QUALITATIVE

QUANTITATIVE

To detect the presence of a Is the determination of that

substance in the sample
substances
Finding out what substances Finding the amount
present
(quantity) of substances
present
WHAT?

HOW
MUCH
?

QUALITATIVE vs QUANTITATIVE
Identification of elements,
ions, compounds present in a
sample (what is it).
Qualitative
tests
may
performed by selective chemical
reactions or with use of
instrumentation.

Determination of how
much of one or more
constituents
present
(how much)
A history of the sample
composition will often
be known

Achieved by:
Sample preparation:
extraction, precipitation
Instrumentation (selective
detectors)
Target analyte derivatization
Chromatography: separation

The
analyst
will
performed qualitative
test prior to perform
the
more
difficult
quantitative analysis

METHOD OF CHEMICAL ANALYSIS

To estimate the concentration of an analyte may require
both measurement of the mass or volume of the sample
and some physical quantity that is related to the
concentration of the element or compound.

This quantity can be classified as:

Gravimetric [mass of a precipitate]
Volumetric [volume of a titration]
Electroanalytical [voltage, current, amount of charge]
Spectroscopic [absorbance, fluorescence, emission]
Miscellaneous [radioactivity, reaction rate, refractive
index]

STEPS IN ANALYTICAL CHEMISTRY

Defining the problem
Selecting the method
Obtain a representative sample

Prepare the sample for analysis

Eliminating interferences
Performing the measurements
Calculating the results and reporting the data

STEP 1

DEFINING THE PROBLEM

To obtain required information within a

period of time
Know what information is needed, by whom,
what purpose & what type of sample is to be
analyzed.
Depend on equipment available, cost, time
involved

STEP 2

SELECT A METHOD

Factors to select a method:

Sample type
Size of sample
Level accuracy
Sample preparation needed
Transportation or storage of sample

Complexity of sample & no of components in sample

influence the choice of method applied.

Analysis size of
sample is classed
as meso,
semimicro or
ultramicro

STEP 3

OBTAIN A REPRESENTATIVE
SAMPLE

Chemical analysis performed on only small

portion of the material
Sample (Solid/Liquid/Gas) may be homogeneous or
heterogeneous
Gross sample:
consist several portions of tested material
must be reduced in size to gain laboratory sample
Laboratory sample:
small portion, crushing or sieving to form homogeneous
or uniform powder for analysis
the analysis sample that actually analyzed

STEP 4

PREPARING THE SAMPLE FOR

ANALYSIS

Preparing laboratory samples

SOLIDS : grinding, mixing, storage to avoid changes (water
content, oxidation).
LIQUIDS : solvent & analyte evaporation, settling of
solids,storage to minimise chemical changes (refrigeration,
freezing, deoxygenate, dark)

Replicates samples
Will improve the quality of the resultsand provide a measure
reliability

Preparing and storage the solutions

Physical & chemical changes, what suitable solvent used to
dissolve entire sample
(acid, base, oxidant, reductant, organic solvent) .

STEP 5

ELIMINATING INTERFERENCES

Perform necessary chemical separation to

remove interference
Impurities may decrease the spectroscopic signal used
to calculate the concentration
Separation step include precipitation, extraction,
chromatography, distillation

INTERFERENCE
Species other than analyte
that can cause error and
affect the final measurement

STEP 6

PERFORMING THE
MEASUREMENTS

Gravimetric analysis
Involve separation of analyte by precipitation followed by
measurement of mass
Volumetric analysis
the analyte reacts with a measured volume of reagent of
known concentration, in a process called titration

STEP 6

PERFORMING THE
MEASUREMENTS
Instrumental techniques
More selective and sensitive
than volumetric & gravimetric
Instrumentation must be
calibrate
Calibration is accomplished by
preparing a series of standard
solutions of the analyte at
known concentrations
A calibration curve is the
instrument response as a
function of concentration

STEP 7

CALCULATING THE RESULTS

AND REPORTING THE DATA

Calculate & Evaluate the results

To estimate whether results are reliable or not
Precision is estimated using the standard deviation using
replicate measurements
Accuracy is best evaluated by including standard
materials close in nature & composition to the unknown
samples

Precision and accuracy is very important in analytical

chemistry and referred as quality control
or quality assurance

UNITS FOR QUANTITY & CONCENTRATIONS

1.
2.
3.
4.
5.

Mole and milimoles

Concentrations & its Definition
Density and Specific Gravity
Molarity, Molality
Percentage Concentration:
%w/w, % w/v, % v/v
6. ppm, ppb, ppt

UNITS FOR QUANTITY & CONCENTRATIONS

MOLE and MILIMOLES
MOLE
The mole (mole) is the SI unit for the amount of a
chemical species
One mole (mol) is the amount of a substance that
contains as many entities (atoms, molecules or ions)
as there are in 12.0 g of C-12 atoms.
The mass in grams of 1 mole of a substance is
called its molar mass.

MOLE

RELATIONSHIP BETWEEN
MOLE AND NUMBER OF
ENTITIES

1 mole of atoms/molecules/ions of any element will

contain Avogadros number of atoms/molecules/ions or
6.022 x 1023 atoms/molecules/ions of that element.
For example:
1 mol of Mg atom contain 6.022 x 1023 Mg atom
1 mol of H2O molecules contain 6.022 x 1023 H2O
molecules
1 mol of Na+ ions contain 6.022 x 1023 Na+ ions

Number of entities = number of moles x 6.022 x 1023

EXERCISE
1. Calculate the number of atoms in 1 mol of aluminium atoms
(6.02 x 1023)
2. Calculate the number of atoms in 0.5 mol of aluminium atoms
(3.02 x 1023)
3. If a container has 12.0 x 1023 atoms of magnesium, determine
number of moles of magnesium atoms
(2.0 moles)
4. How many molecules of CO2 are found in 3.5 moles of CO2?
(2.1 x 1024)
5. How many Cl- ions are present in 0.25 moles of CaCl2?
(3.0 x 1023)

MOLE and MILIMOLES

MOLE VS. Milimole

1 g= 1000 mg
1 mol = 1000 mmol
1 L = 1000 mL

EXAMPLE

EXAMPLE

FORMULA

EXERCISE
1. Calculate the number of moles for 3.4 g of carbon atoms
(0.28 moles)
2. What is the mass of 0.30 moles of CH4?
(4.8 g)
3. How many moles of Cl- is present in 0.34 moles of CaCl2?
(0.68 moles)
4. What is the mass of H in 2.5 moles of H2O?
(5.0 g)
5. What is the mass of O in 3.0 moles of CO2?
(96.0 g)

CONCENTRATION

WHAT IS SOLUTION
CONCENTRATION?

Concentration is the amount of solute in a given volume of

solution.
Solution
:A homogenous mixture of two or more
substances, consisting of solvent and
solute
Solute
:The substance present in a smaller
proportion of the solution. It can be
solid, liquid or gas.
Solvent
:A substance that generally a liquid
present in the larger proportion of the
solution.
Water is considered a universal solvent for most solutions.

DENSITY

DENSITY AND SPECIFIC

GRAVITY OF SOLUTION

Density of a substance is the mass per unit

volume.
In SI unit, density is expressed in unit of kg per
liter, (kg/L) or in metric system the unit use is
gram per milliliter, (g/mL)
Density of water = 1 g/ mL
Specific gravity is the ratio of the mass of an equal
volume of water at 4oC.
Specific gravity is dimensionless.

MOLARITY

MOLARITY / molar
concentration

Molarity : no of moles of the solute in 1 L (dm3) of solution

Molar mass (atomic mass) - the mass of 1 mole of a
substance in unit gram. (Unit for molar mass is g/mol)
Unit for Molarity (mol/L), (M), (mmol/mL)

FORMULA!!
M = no of mol of solute
volume of solution (L)

or
Mmol= Molarity x mL

M = no of mmol of solute
volume of solution (mL)

EXAMPLE
Calculate the molar concentration of ethanol in aqueous
solution that contains 2.30 g C2H5OH (46.07 g/mol) in 3.50
L of solution

No of mole C2H5OH = 2.30 g

46.07 g/mol

Molarity = 0.04992 mol

3.5 L
= 0.0143 M

= 0.4992 mol

EXAMPLE

Try this!!

1. Sea water contains roughly 28.0 g of NaCl per liter.

What is the molarity of sodium chloride in sea water?
No of mole NaCl = 28.0 g
58.44 g/mol

= 0.4791 mol

Molarity = 0.47909 mol

1L
= 0.4791 M

EXAMPLE
2. What is the molarity of 5.30 g of Na2CO3 dissolved in
400.0 mL solution?
No of mole Na2CO3 = 5.30 g
106 g/mol
Molarity = 0.05 mol
0.4 L
= 0.125 M

1 L = 1000 mL
1 dm3 = 1000 cm3

= 0.05 mol
Remember!!
convert volume
to L or dm3

MOLALITY

MOLALITY

Number of moles of solute that dissolved in 1000 g of solvent, m

Preferred expression of concentration involving colligative
properties
(b.p elevation, freezing point depression, osmotic pressure)
Unit for molality (mol/kg)

FORMULA!!

m = no of mol of solute
1 kg of solvent

EXAMPLE
If you have 10.0 grams of Br2 and dissolve it in 1.00 L of
cyclohexane, what is the molality of the solution? The
density of cyclohexane is 0.779 kg/L at room temperature.
Mol of Br2

= 10 g
(159.8 g/mol)

= 0.063 moles Br2

Next, convert the volume of solvent to the weight of solvent

using the density
= 1.00 L x 0.779 kg/L = 0.779 kg
Now just divide the two to get the molality
Molality, m = 0.063 moles Br2
0.779 kg cyclohexane
= 0.080 molal

Try this!!

EXAMPLE

1. A sulfuric acid solution containing 571.4 g of H2SO4 per

liter of solution has a density of 1.329 g/cm3. Calculate
the molality of H2SO4 in this solution
No of mol H2SO4 =

571.4 g
(98.0768 g/mol)

= 5.826 mol

Mass of solvent
1 L of solution = 1000 mL = 1000 cm3
1.329 g/cm3 times 1000 cm3 = 1329 g (the mass of the entire
solution)
1329 g - 571.4 g = 757.6 g = 0.7576 kg (the mass of water in the
solution)
Molality, m = 5.826 mol / 0.7576 kg = 7.690 m

% CONCENTRATION

PERCENTAGES

Concentration can be described in term of %

concentrations
% concentrations (% w/w, w/v, v/v),
Number of parts in 100 parts
eg. Gram of A in 100 grams of sample.
% of A =

number of parts of A
x 100
number of parts of sample

% WEIGHT/WEIGHT

%(w/w)

Percent weight in weight concentration which is weight

in 100 g of sample.
Weight percent (w/w) = weight solute (g) x 100
weight of sample (g)
To express the
concentration
of commercial
aqueous
reagents

% WEIGHT/WEIGHT

%(w/w)

% WEIGHT/VOLUME

% w/v

Percent weight in volume concentration which is weight in 100 ml of sample.

Weight percent (w/v) = weight solute (g)
x 100
volume of sample (mL)
To indicate the
composition of
dilute aqueous
solution of solid
reagents

% VOLUME/VOLUME

% v/v

Percent volume in volume concentration i.e. volume in 100 ml of sample.

Weight percent (v/v) = volume solute (mL) x 100
volume sample (mL)
To specify the
concentration of a
solution prepared by
diluting a pure liquid
with another liquid

ppm and ppb for solid

and liquid

ppm = parts per million (106)

ppb = parts per billion (109)
ppt = part per trillion (1012)
parts of a substance present in one million (or 1 billion) parts of
solvent (water)
If we use gram as the unit, 1ppm means we have 1 g of
substance in 1,000,000 g solvent.

ppm, ppt, ppb

ppt = grams of analyte x 103
grams of sample
ppm = grams of analyte x 106
grams of sample
ppb = grams of analyte x 109
grams of sample
1. What is the w/v in ppm of sodium in a
solution containing 2.500mg of Na+ in 500
mL of solution.
ppm (w/v) = mg of analyte = 2.500 mg = 5 ppm
L of solution
0.5 L
ppm (w/v) = g of analyte x 106
ml of solution
= 2.5 x 10-3g
x 106
500mL
= 5 ppm

2. An analysis for cadmium in water give a value

of 1.20 ppb (w/v). What mass of cadmium is
contained in 1.00 L water?
ppb = g/mL x 109

3. Determine the ppm of ferrous ion, Fe2+, in a solution known

to be 1.2 10-6 M Fe3(PO4)2.8H2O (RMM=501.61)

4. Describe the preparation of 1L 0.1 M HCl

from concentration HCl 37% w/w and with
density 1.18 g/mL

Using 2 formula:
1. Molarity (concentrated) = percentage (%) x (density/RMM) X 1000
2. M1V1 (concentrated) = M2V2 (diluted)

5. Describe the preparation of a 250 mL 50 ppm solution

of AgNO3 from solid chemical.

6. Describe the preparation of 0.5 L 50 ppm of Cl- from solid KCl.

7. How many gram of Ba(NO3)2 is needed to prepare a 50 mL

solution containing 100 ppm NO3-?

How many milliliters of concentrated sulfuric acid, 94.0%

(g/100 g solution), density 1.831 g/cm3, are required to prepare
1 L of 0.100 M solution?

EXERCISE

SELF TEST

1. Define:
a) Parts per million
b) Molality
c) Molarity
d) Percentage
2. Calculate the number of mole in the following:
i) 250 ml, 0.150 M HCl (Ans: 0.0375 mole)
ii) 6.72 liter H2 at STP. (Ans: 0.3 mole)
Hint: 1 mol of H2 at STP contain 22.4 L

EXERCISE
3. How many mole of solute present in the following
solutions:
i) 16.3 liter solution 0.113 M (Ans: 1.8419 mole)
ii) 15.6 ml solution 0.025 M (Ans: 0.0039 mole)
4. Calculate the molar concentration of ethanol in an aqueous
solution that contains 2.30 g of C2H5OH (46 g/mol) in 3.5 L
of solution (Ans: 0.0143 M)
5. Calculate the molarity of 15.0 g ammonia in 750 mL
solution. (Ans: 1.1765 M)
6. Briefly explain how to prepare the following solutions; 500
mL 6.50 % (w/v) aqueous ethanol, C2H5OH.