INTRODUCTION

CEB4032: ANALYTICAL CHEMISTRY

DR HAYYIRATUL FATIMAH MOHD ZAID

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 Outline
▪ Analytical Objectives
▪ Qualitative Analysis
▪ Quantitative Analysis
▪ Analytical Methodology
▪ Type of equipment which includes Gravimetry,
Spectrophotometry, Spectroscopy and
Chromatography.
▪ Basic Tools and Operation
▪ Data Handling and Statistic
▪ Errors
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Learning Outcomes:
At the end of this chapter:

(1) Objectives of analytical chemistry.

(2) Definition of analytical chemistry, qualitative anlaysis

and quantitative analysis.

(3) Type of equipment and basic tools used in analytical

chemistry and laboratory safety.

(4) Basic calculation, statistical method and errors in

data handling for reliability and significant derived
results.
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 Reference Books:
▪ Gary D. Christian, 2004. Analytical Chemistry, 6th Ed., John
Wiley & Sons.

▪ Skoog, West, Holler and Crouch, Fundamentals of Analytical

Chemistry 8th Edition, International Student Edition ISBN 13:
978-0-534-41797-0.

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 Outline
▪ Analytical Objectives
▪ Qualitative Analysis
▪ Quantitative Analysis
▪ Analytical Methodology
▪ Type of equipment which includes Gravimetry,
Spectrophotometry, Spectroscopy and
Chromatography.
▪ Basic Tools and Operation
▪ Data Handling and Statistic
▪ Errors
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 What is Analytical Chemistry?

The branch of chemistry that deals with

the separation, identification and
determination of component in a sample.

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 WHY BOTHER LEARNING
ANALYTICAL CHEMISTRY??????

LETS THINK AND SHARE

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 Main Objective of Analytical Chemistry
▪ Chemicals make up everything we use or
consume, and knowledge of the chemical
composition of many substances is important
in our daily lives.

Examples:
-N content in fertilizer
-contaminants in food
-nutrients in food
-CO in air
-CO2 in NG
-glucose in blood
-carbon in steel

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 Analytical Objectives

▪ Measuring the chemical composition of

natural and artificial materials.

▪ Identify the substances which may be present

in the material.

▪ Determine the exact amounts of the identified

substance.

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 Analytical Chemist
▪ Medicine: basis for clinical laboratory tests which help
physicians diagnose disease and chart progress in
recovery.

▪ Industry: testing raw materials, assuring the quality of

products whose chemical composition is critical (household
products, fuels, paints, pharmaceuticals, etc).

▪ Environment quality: testing for suspected contamination.

▪ Nutritional value of food: major components such as protein,

carbohydrates, trace amount of vitamins and minerals,
calories.

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 Outline
▪ Analytical Objectives
▪ Qualitative Analysis
▪ Quantitative Analysis
▪ Analytical Methodology
▪ Type of equipment which includes Gravimetry,
Spectrophotometry, Spectroscopy and
Chromatography.
▪ Basic Tools and Operation
▪ Data Handling and Statistic
▪ Errors
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Qualitative and Quantitative Analysis

Discipline of
Analytical
Chemistry

Qualitative Quantitative
(What is it?) (How much is it?)

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 Qualitative Analysis
▪ Identification of elements, ions or compounds
present in a sample.

▪ The sample may be solid, liquid or gas.

Example: The presence of gunpowder residue

on a hand generally requires only qualitative
analysis.

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▪ Qualitative test may be performed by selective
chemical reactions or with the use of instrumentation.

Selective and Specific reaction:

Selective reaction
-Reaction can occur with other substances but exhibits
in degree of preference for the substance of interest.

Specific reaction
-Reaction that occur only with the substance of interest.

*few reactions are specific but many exhibit selective

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 Quantitative Analysis
▪ Determination of how much of one or more
constituents is present.

Example: Price of diesel will be determined by

the percent of sulfur impurity present

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▪ A large portion of this course deals with
methods that are used to determine how
much a material is present.

▪ We need to review the general steps that are

taken for any quantitative method.

▪ These steps are taken to insure an accurate

and reliable answer.

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 Outline
▪ Analytical Objectives
▪ Qualitative Analysis
▪ Quantitative Analysis
▪ Analytical Methodology
▪ Type of equipment which includes Gravimetry,
Spectrophotometry, Spectroscopy and
Chromatography.
▪ Basic Tools and Operation
▪ Data Handling and Statistic
▪ Errors
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 Getting Started: Analytical
Methodology/Process
1. Plan: Qualitative or quantitative or both; what kind of
information have; which technique is suitable/technique
to be used.

2. Sampling: Accuracy depends on proper sampling,

characteristic of sample is very important, required good
representative sample.

3. Sample preparation: depends on analytical techniques.

4. Analytical measurement.

5. Data Analysis: Whether the data make sense or not.

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1. Plan/Technique to be Used

1. Accuracy and sensitivity

2. Cost
3. Number of samples to be assayed
4. Number of components in a sample

The approach must produce the results in

time and cost effective.
 What type of information you need?
▪Complete analysis
- The goal is to determine the amount of each
component in a sample.

▪Ultimate analysis
- The amount of each element present without regard
to actual composition.

▪Partial analysis
- Determine one or a limited number of species in a
sample(the most common approach)
e.g. Fe in an ore sample
Presence of lead in a water sample

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 2. Sampling
1. Must be representative
-To insure the results reflect average composition.
e.g. Fe in an ore- minerals and ores are
heterogeneous → to assay any single sample
may not yield valid results for an entire sample
lot.
Proper sample selection and preparation may
help.

2. Sample selection
- Requires some knowledge as to sample source and
history, random sampling may help, powder the
sample, blend the sample, etc.
 3. Sample Preparation
One must then convert the sample to a form of suitable for
the method of analysis:

This may include:

1. Drying to insure an accurate weight
2. Sample dissolution
3. Elimination or masking of potential interferences
4. Conversion of analyte to a single or measureable
form
4. Analytical Measurement/Method
It is essential to define clearly the nature of the
analytical problem.

In general, the following points should be considered

when choosing an method for any measurement.

➢Accuracy and precision required

➢Available sample amount
➢Concentration range of the analyte
➢Interference in sample
➢Physical and chemical properties of the sample
matrix
➢Number of sample to be analyzed
➢Speed
▪ Classical Methods: Wet chemical
methods such as precipitation, extraction, distillation,
boiling or melting points, gravimetric and titrimetric
measurements.

▪ Instrumental Methods: Analytical

measurements (conductivity, electrode potential, light
absorption or emission, mass-to-charge ratio,
fluorescence etc.) are made using instrumentation.
 Type of Method/Equipment
▪ Gravimetry → Methods based on a measured weight.

▪ Titrimetry → Methods based on the measured

volume.

▪ Electrochemical → Approaches that rely on the

measurement of potential, current, resistance, charge
etc.

▪ Spectral Methods →Interaction of an analyte with

electromagnetic radiation.

▪ Chromatography →Separation of a material due to its

interaction with two different phases.

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 Different methods provide a range of precision,
sensitivity, selectivity, and speed capabilities

©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)

 Classical and Instrumentation
Methods

Gravimetric
Volumetric
Electrochemical
Spectral Methods
Chromatography
 5. Data Analysis/Results
Final step in analysis methodology:

This may include:

➢Application of the standard curve
➢Elimination of error based on replicates
➢Reporting in a standard, useable format.

Verification of method → to analyze a standard

reference material of known composition.
Summary Steps in an
Analysis

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 3. Sample
Preparation

1. Plan/
Technique to
be used

4. Analytical
Measurement

5. Data Analysis and

Results
2. Sampling
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 The way you perform an analysis
will depend on your experience, the
equipment available, the cost, and
the time involved.

Good laboratory practice

(validation) is required to assure
accuracy of analyses.

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 Outline
▪ Analytical Objectives
▪ Qualitative Analysis
▪ Quantitative Analysis
▪ Analytical Methodology
▪ Type of equipment which includes Gravimetry,
Spectrophotometry, Spectroscopy and
Chromatography.
▪ Basic Tools and Operation
▪ Data Handling and Statistic
▪ Errors
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 Safe, Ethical Handling of Chemicals
and Waste
- Safety should come first.
- Before working, familiarize yourself with safety
features of your laboratory.
- Wear goggles or safety glasses all the time → protect
your eyes.
- Wear lab coat, long pants and covered shoes.
- Rubber gloves→ protect hands from chemicals.
- Clean up any chemical spills immediately.
- Chemicals with hazardous fume should always be
used under a fume hood.
- Label all the vessels.
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What do we use in a Analytical Lab?

Basic Tools:

-Chemicals
-Balances
-Glassware
-Heating apparatus
-Instruments
-Miscellaneous: filter paper, tongs, stir rods,
beaker, etc
 Handling of Chemicals
▪ The key is to limit contamination of chemicals and
reagents.

▪ Never return excess chemicals to original bottle.

▪ Keep the workplace and balances clean.

▪ Not everything goes down the drain.

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 Analytical Balance
▪ Electronic balance→ to balance the load on the
pan.

▪ Capacity → 100-200 g

▪ Sensitivity → 0.01-0.1 mg

▪ Sensitivity → the smallest increment of mass that

can be measured.

▪ Chemical should never be placed directly on the

weighing pan.
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 Using a Balance
▪ Always weight chemicals in a clean ‘vessel’, not on
the pan!

▪ Vessel → glassware, weighing dish, or weighing

paper (put on the balance).

▪ Samples normally need to be weight at ambient

temperature (room temperature to get an accurate
reading).

▪ Balance need to be calibrated and leveled to work

properly.

▪ Using tongs, tissue or paper towel to transfer the

vessel.
 Glassware and Apparatus
▪ Burets → measure the volume of liquid precisely

▪ Volumetric Flasks → calibrated flasks to contain a

particular volume

▪ Pipets → deliver known volumes of liquid (calibrated).

▪ Syringes → dispenses tiny volumes (accuracy and

precision ~ 1%)

▪ Desiccator→ closed chamber containing a drying agent

called desiccant

▪ Filters → filter and collect precipitate

Burets

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 Manipulating
buret stopcock

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Volumetric
Flasks

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Pipets and Micropipets
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Syringes

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Desiccator

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Filter
Paper

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Washing by decantation and transferring the precipitate
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Dispensing an aliquot
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 Reading Volume
▪ Meniscus → the curved surface of a
liquid at its interface with the
atmosphere.

▪ Read the bottom of the concave of the

meniscus.

▪ Make sure your line of sight is level with

meniscus.

▪ Parallax→ apparent displacement of a

liquid level or of a pointer as an
observer changes position.

▪ Parallax occurs when an object is

viewed from a position that is not at a
correct angle to the object.
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 The Lab Notebook
▪ To record what you did and what you observed
during the experiment.

▪ Should be understandable to someone else.

▪ Contains
-Experiment objective and purpose
-List of glassware and chemicals
-Safety info on chemicals
-Flow chart of procedures
-Data
-Analysis and conclusions
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Calculation Used in Analytical
Chemistry

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 Some Important Units of Measurement

SI Units
• A standardized system of units known as the
International System of Units (SI).

• This system is based on the seven fundamental

base units.

• Numerous other useful units, such as volts, hertz,

coulombs, and joules, are derived from these base
units.

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The ångstrom unit, Å, is
a non-SI unit of length
that is widely used to
express the wavelength
of very short radiation
such as X-rays
(1 Å = 0.1 nm = 10-10 m).
Typical X-radiation lies in
the range of 0.1 to 10 Å.

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 The Mole
▪ The mole (mol) is the SI unit for the amount of a
chemical species.

▪ It is always associated with a chemical formula and

represents Avogadro’s number (6.022 × 1023) of
particles represented by that formula.

▪ The molar mass (M) of a substance is the mass in

grams of one mole, g/mol of the substance.

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 Example 1

How many mole and milimoles of benzoid acid

(MW = 122.1 g/mol) are contained in 2.00 g of
the pure acid?

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 Answer

Amount of HBz = 2.00 g / 122.1 g/mol

= 0.0164 mol

In millimoles = 0.0164 mol x (1000 mmol/1 mol)

= 16.4 mmol

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 Example 2

How many grams of Na+ (MW = 22.99

g/mol) are contained in 25.0 g of Na2SO4
(MW = 142.0 g/mol)?

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 Answer
From chemical formula, 1 mol of Na2SO4 contains
2 mol of Na+

Number of mol of Na2SO4 = 25 g / 142 g/mol

= 0.1761 mol

Number of mol of Na+ = 0.1761 mol x 2

= 0.3521 mol

Mass of Na+ = 0.3521 mol x 22.99 g/mol

= 8.10 g
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Solutions and Their Concentrations

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 Example 3

Calculate the molar concentration of ethanol

in an aqueous solution that contained 2.30 g
of C2H5OH (MW = 46.07 g/mol) in 3.50 L of
solution.

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 Answer
No of mol of C2H5OH = 2.30 g / 46.07 g/mol
= 0.05 mol

Molar concentration of C2H5OH = 0.05 mol / 3.5 L

= 0.0143 mol/L
= 0.0143 M

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• Percent Concentration
• Chemists frequently express concentrations
in terms of percent (parts per hundred).
• Three common methods are:

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• Parts Per Million and Parts Per Billion

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Cppb ppb

− parts per billion (ppb)

− parts per thousand (ppt)

• 1 ppm = 1 mg/L
• 1 ppb = 1 μg/L
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 Example 5

What is the molarity of K+ in a solution that

contains 63.3 ppm of K3Fe(CN)6 (MW = 329.3
g/mol)?

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 Answer

= 5.7669 x 10-4 mol/L

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 Chemical Stoichiometry
▪ Stoichiometry is defined as the mass
relationships among reacting chemical
species.

▪ This section provides a brief review of

stoichiometry and its applications to chemical
calculations.

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 Empirical Formulas and Molecular
Formulas
▪ An empirical formula gives the simplest
whole-number ratio of atoms in a chemical
compound.

▪ In contrast, a molecular formula specifies the

number of atoms in a molecule.

▪ Two or more substances may have the same

empirical formula but different molecular
formulas.

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• For example, CH2O is both the empirical and
the molecular formula for formaldehyde.

• It is also the empirical formula for such

diverse substances as acetic acid (C2H4O2),
glyceraldehyde (C3H6O3), and glucose
(C6H12O6).

• The empirical formula is obtained from the

percent composition of a compound.

• In addition, the molecular formula requires a

knowledge of the molar mass of the species.
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Example 6: Stoichiometric Calculations

What mass of AgNO3 (MW =169.9 g/mol) is

needed to convert 2.33 g of Na2CO3

(MW=106.0 g/mol) to Ag2CO3 ?

Given:

Na2CO3(aq) + 2AgNO3(aq) → Ag2CO3(s) + 2NaNO3(aq)

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 Answer

• Step 1: Mol of Na2CO3

• Step 2: The balanced equation reveals that

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• Step 3: Mass of AgNO3

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End of Topic

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 Exercise 1

Q1:
Calculate the mass of Ag2CO3 (MW = 275.7
g/mol) formed when 25.0 mL of 0.200 M AgNO3
(MW = 169.9 g/mol) are mixed with 50 mL of
0.0800 M Na2CO3 (MW = 106 g/mol)?

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Q2:
Exactly 0.2220 g of pure Na2CO3 (MW = 106
g/mol) was dissolved in 100.0 mL of 0.0731 M
HCl (MW = 36.46 g/mol).

a. What mass in grams of CO2 (MW = 44 g/mol)

were evolved?
b. What was the molarity of the excess reactant
(HCl or Na2CO3)?
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