WEEK 1 Introduction To Analytical Chemistry

Analytical Chemistry for Engineering
SSCK 1203
Aemi Syazwani binti Abdul Keyon, PhD
Email: aemi@kimia.fs.utm.my
Room No: C18-310, Department of Chemistry, FS, UTM JB
1
Week 1 1
COURSE OUTLINE
This course:
Introduction to quantitative chemical analysis, with emphasis on
Chemical analysis
1 2 instrumental methods
procedures
- introduction to analytical chemistry,

- sampling,
- sample preparation and sample preservation
the principles, instrumentation, and

application of chromatographic and
spectroscopic methods such as :
- gas chromatography (GC),
- high performance liquid chromatography (HPLC),
- ultraviolet-visible (UV-VIS) spectroscopy,
- atomic absorption (AAS) and
- atomic emission spectroscopy (AES)
Week 1 2
General steps in chemical analysis . Sampling, storage, sample presevation . Solution preparation
Week 1
Chapter 1
Introduction to
Analytical Chemistry
1 General steps in chemical analysis
2 General sampling, storage, sample preservation procedures
3 General procedures on solution preparation
Week 1 3
Chapter 1
Introduction to
3 General procedures on solution preparation
Week 1 4
What is analytical chemistry and

how it plays a role?
Obtain, process and communicate information about
the composition and structure of a matter (analyte) in a sample.
In other words, it is the ‘’art’’ and science of determining

what matter is and how much of it exists
Whereby it deals with the separation, identification &

determination of analytes (components) in a sample.
It involves the application of a range of techniques and methodologies
to obtain and assess qualitative, quantitative and structural
information on the matter.
Week 1 5
What is Analyte, Matrix and Sample?
Analyte Matrix Sample

• the matter/substance • the medium in which • representative of the
to be identified, the analyte is population or gross
detected, or analyzed sample
separated using • all other constituents
selected methods in a sample except
for the analyte
Week 1 6
Type of sample and matrix can be anything…

It depends on things (analytes) we are going to analyze
Sample: Oil sample from the Gulf of Mexico oil spill disaster
Analyte: Hydrocarbons, sulphur, trace metals
Soil/sand Or even feathers!

Water Smoke
Week 1 7
Type of sample can be anything… its depend

on things we are going to analyze.
Week 1 8
Gulf of Mexico oil spill, 2010
Week 1 9
Area of analytical chemistry

Environmental analysis: pollutants (air-borne
matters, oil, pesticides, wastewater), soil and water
analysis
Clinical analysis: blood, urine, feces, cellular fluids,

etc., for use in diagnosis.
Pharmaceutical analysis: establish the physical

properties, toxicity, metabolites, quality control, etc.
Forensic analysis: analysis related to criminology;

DNA finger printing, finger print detection; blood
analysis.
Industrial quality control: required by most

companies to control product quality.
Bioanalytical chemistry and analysis: detection

and/or analysis of biological components (i.e.,
proteins, DNA, RNA, carbohydrates).
Week 1 10
Analytical chemist/analyst?
A true analyst has several characteristics:

✓Has knowledge of the methods and instruments used for
analysis.
✓Understands the principles of analysis, so that he/she can
apply and if necessary modify analytical methods to solve a
particular problem.
✓Can develop new methods of analysis.
✓Can evaluate and interpret the result of a quantitative analysis.
An analytical chemist is a skilled and well-

trained chemist and also known as a problem
solver
Week 1 11
Type of analysis
Analogy Acceptable worldwide,
more valid and accurate
for reporting
Quantitative analysis
is an analysis to determine how much of analyte
(s) is/are present in a sample.
Qualitative analysis
is performed to identify what analyte present in a
sample.
www.mybizmaster.com
Week 1 12
Steps in quantitative analysis

Understand and define the problem
Literature search
Select analytical method
Sampling and sample preparation (eliminate interference)
Analysis (perform measurement, compare results with standard method)
Apply required statistical techniques and verify results
Reporting
Week 1 13

•Learn as much as possible about the overall problem that is being faced.
What is the Who will use

problem? What the
needs to be information?–
investigated? to provide
(Qualitative evidence for
and/or What analysts must know ? possible future
quantitative?) litigation, to
help improve
company profit
When will the How many samples
or to satisfy
result be needed? are to be analyzed?
customers
Week 1 14

•Learn as much as possible about the overall problem that is being faced.
• After the problem is defined this will dictate to:
How accurate and precise does it have to be?

(how sensitive the method must be?)
What is the budget ? How the sample is

obtained (sampling) ?
Does it require any preliminary treatment ?

(What separation must be required to
eliminate interferences?
Week 1 15
Chemical literature search

•Research analytical procedure are procedures newly developed from series of trials and can be used for
reference in research activity .
•Standard method: accepted, validated procedure used by various recognized agency/agencies with
proper calibrations and records, eg ISO 17025 accredited methods from ASTMs or USEPA or CODEX.
AOAC
ASTM
Week 1 16
•Online scientific and technical journal papers obtained through research activities→
Analytical Chemistry, Analytica Chimica Acta, Journal of Chromatography, Analytical
Bioanalytical Chemistry , Analyst, Journal of Separation Science, Electrophoresis etc..
Week 1 17
Method selection
Factors to consider include:
• On what chemistry principle the analyte can be analyzed and detected?

→ Does it interact with electromagnetic radiation? Can it be precipitated with metal
reagent? Is it an ion or hydrocarbon?
•Equipment – spectroscopy instruments, chromatography instruments, detectors
•Are methods valid/certified?
•Accuracy
•Detection limit (the lowest amount of analyte that can be detected, the lower the
detection limit, the better)
•Time and cost/number of analyses

•Complexity of sample – how selective the method to the target analyte
•Technical expertise
•Speed
•Can it be automated?
Week 1 18
The classification of analytical method

Gravimetric Methods
→quantitative isolation of an analyte by precipitation and the weighing of the
precipitate (mass)
Example:
Volumetric Methods
Measuring the volume of a solution to react with the analyte (containing
sufficient reagent) (i.e., titration or gas analysis)
Week 1 19
Separation Methods
Measuring the peak height/area of separated analytes in samples. Suitable for
determination of multiple analytes in a sample
HPLC
chromatogram
Spectroscopic Methods
Measuring the interaction between the analyte and electromagnetic radiation (or
the production of radiation by an analyte)
Electroanalytical Methods
Measuring electrical property (i.e., potential, current or amperes) which is
chemically related to the amount of analyte
Week 1 20
Sampling
Deciding how to obtain a sample for
A process to get a representative and analysis depend on:
homogeneous sample. i. The size of the bulk to be sampled.
Representative means that content of ii. The physical state of the fraction to be
analytical sample reflects content of bulk analyzed. (solid, liquid, gas)
sample.
iii. The chemistry of the material to be
Homogeneous means that the analytical assayed.
sample has the same content throughout.
(Nothing can be done that would destroy or
alter the identity or quantity of the analyte)
Steps involved in sampling bulk material:

Identify the population from which the sample is to be
obtained.
Collect a gross sample that is truly representative of the
population being sampled.
Reduce the gross sample to a laboratory sample that is
suitable for analysis.
Week 1 21
Inhomogeneity of the material, make sampling of solids

more difficult.
Sampling
The easiest way to sample a material is grab sample –
solid the sample taken at random and assumed to be
representative.
For reliable results→ take 1/50 to 1/100 of the total

bulk. The larger the particle size, the larger the gross
sample should be.
Examples:
•Stockpile of grains: take increment from
surface and interior via grab method or
motion method (conveyor belt)
•Compact solids (metals and alloys): obtained

by random drilling or by sawing across the
metal at random intervals and collecting the
`sawdust’ as the sample.
Week 1 22
1
•Obtaining a random sample from
a bulky material (ore, grain, coal)
can be achieved while the material
in motion (conveyor belt).
Periodically transfer portion into a
sample container.
•The gross sample must be reduced

in size to obtain a laboratory
sample.
3
• Coning and Quartering : The sample is crushed and mixed to form a conical
pile. This pile is flattened, cut into equal quarters, and two opposite quarters are
chosen at random.
•→ until the gross sample is small enough to be transported to the laboratory.
Week 1 23
Sampling liquid
• Liquid samples are homogeneous and are much easier to sample.
• The gross sample can be relatively small.
• If liquid samples are not homogeneous, and have only small quantity, they can be
shaken and sampled immediately.
• Sampling techniques will depend on the types of liquid.
Examples
1.Large volume of liquids (impossible to mix)
→Sampled after transfer (during discharge) or if in a
pipe, sampled after passing through a pump or at
different points in pipe system.
2.Large stationary liquids (sea, rivers, reservoir)
→Samples may be obtained at different depths using a
sample thief (a bottle that can be opened and filled at
any desired location in the solution). The separate
aliquots of liquids can be analyzed individually or can be
combined into one gross sample (composite sample)
and replicate analyses performed.
3.Biological fluids (blood, urine, saliva)
→The timing of sampling is very important. For
example, the composition of blood varies before and
after meal. The sample is collected after the patient has
fasted for a number of hours.
Week 1 24
Sampling gas
•Tend to be homogeneous
•Large volume of samples is required because of their low density.
•Examples:
1. Environmental air analysis: Use a `Hi-Vol’ sampler which contains filters to
collect particulates.
2. Gas/smoke from burning activities: use gas sampling bulb glass
3. Breath sample: blow into a sampling bag.
Week 1 25
Sample storage and preservation

•Objective:
To preserve the nature of analytes contained in the sample, as similar as possible
during sampling process.
•Sample container materials can introduce either positive or
negative errors in measurement, particularly ultra-trace levels, by
contributing contaminants through leaching or surface desorption,
or by depleting concentrations through adsorption. Additionally,
the sample containers should be compatible with the reagents
used for sample preservation
Mechanism of preservation:
•Refrigerated /freeze after collection until the time of analysis
→ to prevent decomposition of biological samples through the action of
bacteria.
•Acidified with 10% HNO3 immediately upon collection
→ to prevent precipitation of metals from water samples.
Week 1 26
amber vials/bottles with tight cap for

light sensitive samples
Polyethylene bottle for inorganic

metal containers for trace analyses
hydrocarbon samples
Week 1 27
Chapter 1
Introduction to
Introduction to concentration and general

3 procedures on solution preparation
Week 1 28
Concentration is the amount of solute in a known

amount of solution
Concentration = Amount of solute
Amount of solution
Week 1 29
Unit for concentrations
• Molarity (M) – mole of solute/liter of solution

• Molality (m) - moles of solute/kilogram of solvent.
• Normality (N) (not common) – can only be calculated when we deal with
reactions (eg. Acid base rxn) , because normality is a function of equivalents.
• Parts per million (ppm) – milligram of solute/liter of solution
• Parts per billion (ppb) – microgram of solute/liter of solution
• Percent concentration (%w/w, %w/v, %v/v)
Week 1 30
• Molarity (M) = number of moles of solute

liters of solution
concentration of a particular chemical species
• Molality (m) = number of moles of solute

kilograms of solution
Week 1 31
Example:
What is the molarity of a salt solution when
0.60 g NaCl was dissolved in 100 mL water?
(MW NaCl = 58.5 g/mol)
mol 1
Molarity (mol/L) = 0.60 g x x
58.5 g 0.100 L
= 0.10 mol/L (0r 0.10 M)
Week 1 32
Class activity
What is the molarity of a solution

prepared by dissolving 8.0 g of NaOH
in water so that the final volume is
250 mL?
Week 1 33
Concentration in terms of percent composition

The concentration of substance in commercial aqueous reagents, organic
solvents and commercial household products are usually expressed in
percent composition
• Weight percent = Weight of solute x 100%

(%w/w) Weight of solution
• Volume percent = Volume of solute x 100%

(%v/v) Volume of solution
• Weight-volume = Weight of solute x 100%

(%w/v) Volume of solution
Example: 37% is labeled on a HCl reagent bottle. This means that it contains 37 g
HCl per 100 g solution
Week 1 35
Week 1 36
Weight/Weight Percent (%w/w)

Weight of solute (g)
Weight percent =  100
Weight of solution (g)
Example:
What is the weight percent of a solution of
6 g salicylic acid in 100 g of solution?
Weight percent = (6 g/100 g)  100

= 6 %w/w
Week 1 37
Eye medication
Week 1 38
Weight/Volume Percent (%w/v)

Weight of solute (g)
Weight/Vol ume Percent =  100
Total volume of solution (mL)
Example:
What is the weight percent of a solution of

0.05 g epinastin in 100 mL of solution?
Weight/Volume percent = (0.05 g/100 mL)100

= 0.05 %w/v
Week 1 39
Week 1 40
Volume/Volume Percent (%v/v)

Volume of solute (mL)
Volume/Vol ume Percent =  100
Volume of solution (mL)
Example:
How many mL of HCl needs to be added into a 100

mL solution to prepare 33% v/v?
33% mL/mL = (X mL/100 mL)100

= 33 mL
Week 1 41
Some shark can detect odours

(mostly blood) at concentration of
one part per billion
Yahner,R. Wildlife Behaviour and Conservation, Springer: New York
Week 1 42
http://www.abcwua.org
Week 1 43
Million→ 1,000,000
Billion → 1,000,000,000
Trillion→ 1,000,000,000,000
Million→ 106
Billion → 109
Trillion→ 1012
1 part per Million→ 1 in 106

1 part per Billion → 1 in 109
1 part per Trillion→ 1 in 1012
Week 1 44
1 part per Million→ 1 in 106

1 unit volume in 106 unit volume
Blood in ocean
1 unit mass in 106 unit mass

Mineral in solid
1 unit mass in 106 unit volume

Salt in water
Week 1 45
Commonly used UNIT
Week 1 46
1 unit mass in 106 unit mass

Mineral in solid
Grams of solute (g)

ppm = 6
Grams of solid (g) x 10
Therefore the unit :

g/g or mg/kg
ppm = g/g = mg/kg
Week 1 47
Example:
A 2.6 g sample of plant tissue was
analyzed and found to contain 3.6 g
zinc. What is the concentration of zinc
in the plant in ppm?
Parts per million = (3.6 g / 2.6 g)

= 1.4 g/g or ppm
Week 1 48
1 unit mass in 106 unit volume

Salt in water For water:
1 g ~ 1 mL
1 kg ~ 1 L
Grams of solute (g)
ppm = 6
mL of water (mL) x 10
Therefore the unit :

g/mL or mg/L
ppm = g/mL = mg/L
Week 1 49
Week 1 50
Exercise:
1. A 0.25 mL serum sample was analyzed for
glucose content and found to contain
26.7 g. Calculate the concentration of
glucose in ppm.
Week 1 51
Both of these
→The w/w % unit may also be expressed as a fraction units are for
e.g. 37% (w/w) can be expressed as 37 parts per hundred SOLID SAMPLE
How about smaller fractions??
• Parts per thousand = g of solute
103 g solution
Or = mg/g
• Parts per million (ppm) = g solute

106 g solution
Or = µg/g
When the sample is in liquid form, we can use w/w % in

volume unit as well. How?
As the density of aqueous solution often very close to 1.00 g/L, we usually
correlates 1 g water with 1 mL water (approximation)
Therefore, 1 ppm = 1 µg/g can also be converted to 1 µg/mL = 1

mg/L
Week 1 53
For trace analysis in liquid sample

~Analysis of very very very little amount of analytes
• Parts per billion (ppb) = g solute

109 g solution
Therefore,1 ppb = 1 ng/g = 1 ng/mL = 1 µg/L
• Parts per trillion (ppt) = g solute

1012 g solution
Therefore,1 ppt = 1 pg/g = 1 pg/mL = 1 ng/L
Week 1 54
Converting percent composition to molar concentration

-converting ‘commercial term’ to ‘easier laboratory term’-
• Example:
A commercial aqueous ammonia (NH3 ) bottle is labeled as 28.0% w/w,
and has a density of 0.899 g/mL and MW of 17.03 g/mol. Let say you want
to convert the concentration into molarity for easier calculation in your lab
book, how can you do that?
density
= 28 g/100 g x 0.899 g/mL
= 0.2517 g/mL
= 0.2517 g/mL / 17.031 g/mol MW
= 0.01478 mol/mL x 1000 mL/1L
= 14.8 mol/L or 14.8 M
55
Week 1 55
Preparation of solution
Example: How to prepare 250 mL of 0.100 M NaOH from NaOH
solid? [MW: NaOH = 40 g/mol]
1. Calculate the weight (g) of NaOH pellet using MW to produce 0.1 M

solution
Calculations ???
2. Weigh ??? g of solid (generally  0.1 mg, ie up to 4 decimal places in
grams)
3. Dissolve in water, transfer (quantitatively with rinsing) to a 250 mL
volumetric flask, and dilute to the mark
Dissolve and
Calculate Weigh
transfer
Week 1 56
Dilution of solution
The mantra that you have to remember
M1V1 = M2V2
Where,
M1 is the concentration of the original solution
V1 is the volume of the original solution
M2 is the concentration of the diluted solution
V2 is the volume of the diluted solution
Week 1 57
Week 1 58
Example:
What is the volume needed to prepare
2.50 L of a 0.360 M H2SO4 starting
with concentrated acid that is 18.0 M?
M1V1 = M2V2
18.0 M  V1 = 0.360 M  2.50 L

V1 = 0.0500 L or 50 mL
Week 1 59

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Analytical Chemistry for Engineering

- introduction to analytical chemistry,

the principles, instrumentation, and

2 General sampling, storage, sample preservation procedures

3 General procedures on solution preparation

2 General sampling, storage, sample preservation procedures

3 General procedures on solution preparation

What is analytical chemistry and

In other words, it is the ‘’art’’ and science of determining

Whereby it deals with the separation, identification &

What is Analyte, Matrix and Sample?

Analyte Matrix Sample

Type of sample and matrix can be anything…

Analyte: Hydrocarbons, sulphur, trace metals

Soil/sand Or even feathers!

Type of sample can be anything… its depend

Gulf of Mexico oil spill, 2010

Area of analytical chemistry

Clinical analysis: blood, urine, feces, cellular fluids,

Pharmaceutical analysis: establish the physical

Forensic analysis: analysis related to criminology;

Industrial quality control: required by most

Bioanalytical chemistry and analysis: detection

A true analyst has several characteristics:

An analytical chemist is a skilled and well-

Steps in quantitative analysis

Select analytical method

Sampling and sample preparation (eliminate interference)

Analysis (perform measurement, compare results with standard method)

Apply required statistical techniques and verify results

Understand and define the problem

What is the Who will use

Understand and define the problem

• After the problem is defined this will dictate to:

How accurate and precise does it have to be?

What is the budget ? How the sample is

Does it require any preliminary treatment ?

Chemical literature search

• On what chemistry principle the analyte can be analyzed and detected?

•Equipment – spectroscopy instruments, chromatography instruments, detectors

•Are methods valid/certified?

•Time and cost/number of analyses

The classification of analytical method

Steps involved in sampling bulk material:

Inhomogeneity of the material, make sampling of solids

For reliable results→ take 1/50 to 1/100 of the total

•Compact solids (metals and alloys): obtained

•The gross sample must be reduced

•Large volume of samples is required because of their low density.

Sample storage and preservation

amber vials/bottles with tight cap for

Polyethylene bottle for inorganic

2 General sampling, storage, sample preservation procedures

Introduction to concentration and general

Concentration is the amount of solute in a known

• Molarity (M) – mole of solute/liter of solution

• Molarity (M) = number of moles of solute