CHEM 2310

Fundamentals of Analytical
Chemistry

Lecture 1:
Introduction to Analytical Chemistry

Acknowledgement: Profs. Ian Williams, Jianzhen Yu 1

 Analytical Chemistry is Close By..

Where/What
is Analytical
Chemistry ?

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[Link]
 Analytical Chemistry is Close By..

• Food chemistry
• Food safety testing
• Environmental analysis
• Forensic chemistry
• Pharmaceutical analysis
• In biochemistry and
• all other areas of chemistry

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 Analytical Chemistry is Close By..

Food labelling

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 Analytical Chemistry is Close By..

Food labelling

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 Analytical Chemistry is Close By..

Cosmetics
Hg!?

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 Analytical Chemistry is Close By..

Food Safety

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 Analytical Chemistry is Close By..

Forensics

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Analytical Chemistry is Close By..

Heavy Metals Analysis

ICP-AAS,
ICP-OES,
ICP-MS

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Analytical Chemistry is Close By..

Heavy Metals Analysis

A = log (Po/P)

ICP-AAS, ICP-OES, ICP-MS

A   c b 10
Analytical Chemistry is Close By..

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Analytical Chemistry is Close By..

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Analytical Chemistry is Close By..

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Analytical Chemistry is Close By..
Analytical Chemistry is Close By..

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Analytical Chemistry is Close By..

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Analytical Chemistry is Close By..
Analytical Chemistry is Close By..
Analytical Chemistry is Close By..

Organic contaminants Analysis

Analytical Chemistry is Close By..

Organic contaminants Analysis

Analytical Chemistry is Close By..

Organic contaminants Analysis

Analytical Chemistry is Close By..

EIA

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Analytical Chemistry is Close By..

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Analytical Chemistry is Close By..

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 Analytical Chemistry is Close By..

Analytical
chemists!

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 Qualitative and quantitative analysis

• ANALYTICAL CHEMISTRY deals with the qualitative and

quantitative characterisation of a matter or a mixture.

• Qualitative analysis reveals the chemical identity of the species.

• Quantitative analysis establishes the amount of one or more of

the species.

• The analytical procedure may involve the

– separation
– identification, and
– determination of the relative amounts

of the components in a sample.

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Various stages in the overall analytical method

bulk sample pretreated result or chemical decision

material sample number information

sampling physics & test or calibration evaluation

procedure chemistry instrument

Analytical Chemist

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 Analytical methods
• The development of analytical methods has followed closely the
introduction of new measuring instruments.
GRAVIMETRIC METHODS
VOLUMETRIC / TITRIMETRIC METHODS
COLORIMETRIC / TURBIDOMETRIC METHODS
INSTRUMENTAL METHODS

Measurement of the amount of radiation that is

Spectral (optical) methods absorbed, emitted, scattered, refracted, diffracted, or
rotated by the sample.

Measurement of the electrical properties (electrical

Electroanalytical methods potential, charge, current or resistance) of the sample
solution.

Separation of sample components based on their

Separative methods
physical or chemical properties.

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 General steps in selecting methods for analysis
1. Define the problem
– What is the concentration range of the sample?
– What degree of accuracy is demanded?
– What other components are present in the sample?
– What are the physical and chemical properties of the sample?
– How many samples are to be analyzed?
2. Investigate the literature
– What methods are available?
– How do they work?
3. Choose a method
4. Test the procedures with standard samples
• Sampling
• Sample preparation
• Analysis
5. Modify the procedure, if necessary, and validate changes
6. Try other methods and compare results
7. Reporting and interpretation
8. Drawing conclusions
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If results are unsatisfactory or have new instrumentation – develop your own method !
 Factors in choosing analytical methods

 Accuracy and precision

 Sensitivity Neither precise
nor accurate
 Detection limit
 Concentration range
 Selectivity
Precise, but not
 Speed accurate

 Convenience
 Skill required for operation
Accurate and
 Cost precise

 Availability of instrument
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 Common applications

foods, pharmaceutical
Quality control
agents, industrial products

air pollution, water quality,

Environmental control
health hazards
diagnosis of diseases, body
Biomedical analysis
fluid tests

Forensic detection poisons, stains, drugs

reaction products, reaction

Chemical research
rate and mechanism

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 How to analyze a chocolate bar?

Analytes: Theobromine and Caffeine

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(Similar procedure for all other chemical species / Sample matrices)
 Analysis of Caffeine in a Chocolate Bar

Stimulant caffeine and its biochemical precursor theobromine (doesn’t contain Br)
to be analyzed. First the literature is searched for existing method.

Analytes: Theobromine and Caffeine

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(Similar procedure for all other chemical species / Sample matrics)
Preparation of Representative Samples

Which “sample” to pick for analysis?

Lot is the total material from which samples taken

Bulk sample taken from this and analyzed

(or archived) – should be representative

Smaller homogeneous lab sample then taken

with same composition as the bulk

Small test portions called aliquots then used for

individual analyses

Several analyses taken to give estimate

of reproducibility of results

Sample preparation may involve steps to remove

interfering species, or to concentrate the analyte

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 What is in the chocolate?
Step 1. Sample Preparation: Homogeneous Solid

Just inject the “sample” and wait for results!?

Chocolate is ground to fine powder Difficult

unless you freeze it first ! Then it becomes
brittle and more readily ground

use a ceramic mortar and pestle

Need for ‘powder’ is to dissolve away fat from

the chocolate, which would otherwise interfere
with the chromatographic analysis

Lumps of chocolate have low surface area and

extraction of fat not efficient

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Step 2. Sample Preparation: Removal of Interfering Species (Fat)

Loss of analytes??

The ground chocolate is shaken several times with petroleum ether as

hydrocarbon solvent that removes the fat (about 30% of the total mass)
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 Step 3. Extraction of Analytes into Aqueous Solution

Next the caffeine and theobromine are extracted into hot water. Several filtering steps
avoid fine suspension of solids that would contaminate the chromatography column
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Step 4. Chromatographic Separation of Analytes

Aqueous soln of analytes

injected into column packed
with SiO2 particles to which are
attached long hydrocarbon
molecules, i.e., coated with
hydrophobic surface – ‘greasy’

Molecules interact with column

particles to differential extent.
Some are retained longer than
the others–basis of
chromatographic separation

Theobromine (NH) elutes more

rapidly than caffeine (NMe)
(Q. Why ??)

Detection of the eluted

molecules by uv absorption at
254nm.

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Step 5. Detection of Analytes – Chromatographic Results

The peaks of two standard

samples of equal concentration
Theobromine and Caffeine

Q Why is peak height so different ?

Same??

Experimental result on left – can know peaks are due to caffeine

and theobromine by running authentic samples (above).

Response (based on uv absorption) varies so the peak heights

must be calibrated versus known concs. for each analyte
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Step 6. Construction of Calibration Curves for Analytes

Construction of such
Calibration curves is time
consuming but necessary
for obtaining reliable results

Also need to check

Linearity of response over the
concentration range of interest

i.e. check that the signal is

proportional to the conc.
of analyte – in some methods
signal becomes ‘saturated’

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 Step 7. Analysis of Results

Once the calibrations are conducted then peak heights can be converted to known quantities of
analyte in ppm. The mass of the analytes in the original in the amount of analyte per 100g of
sample can be computed.

The answers may be given as absolute numbers with appropriate # of significant figures.

Through multiple analyses estimate of the uncertainty/reproducibility of measurements can be

made and given as a standard deviation

Q. How many ppm do the above numbers represent ?

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