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College of Science

The Nature of Analytical


Chemistry, and Introduction to
Chemical Analysis
1. Role and Importance of Analytical Chemistry
in Various Aspects of Life
2. Classification and Types of Analyses
3. Steps in a Typical Quantitative Analysis and
Sampling Protocols

Technological University of the Philippines


Addie Albano

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What is Analytical Chemistry?

Generally, analytical chemistry is the science of obtaining, processing, and


communicating information about the composition and structure of matter.
In other words, it is the art and science of determining what matter is and
how much of it exists. (American Chemical Society)

Chemical characterization of a sample material

What are
you made
of??
Analyze me
and see for
yourself!

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Analytical Chemistry
Where is analytical chemistry used?

✓ Assuring the safety and quality of food, pharmaceuticals,


and water
✓ Assuring compliance with environmental and other
regulations
✓ Supporting the legal process
✓ Helping physicians diagnose diseases
✓ Providing measurements and documentation essential to
trade and commerce

Applications:
1. Process control in industry – Analysis of trace elements
2. Environmental monitoring – Analysis of heavy metals in air, water, soil
3. Food and Agriculture – Analysis pesticide residue
4. Medical diagnostic – Analysis of blood or urine
5. Pharmaceutical – Analysis of moisture in crude drug
6. Forensic – Analysis of gunpowder residue

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Analytical Chemistry

What’s in this vaccine?


What’s in this water?

What’s in this food?

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The Analytical Process

Separation Identification Quantitation Detection


How can the analyte be separated What is the identity of How much of substance Does the sample
from the sample matrix for better the substance in the A is in the sample? contain substance A?
quantitation and identification? sample?

1. Sample is obtained 2. Separation 3. Analysis: Identification,


(Sample preparation) Quantitation, Detection
Process of converting the sample
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into a form suitable for analysis
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Components of a Sample

Analyte: the constituent of interest in a sample;


one that is being sought in an analysis

Matrix: comprises all other constituents in a


sample except for the analyte

Sample: Facial cream


Analyte: Stearic Acid
Matrix: Facial cream without stearic acid

Facial cream sample

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Classification of Analyses

Based on the purpose of Based on the extent Based on the sample


Based on the method
determination of analysis size available
1. Physical 1. Fundamental 1. Complete 1. Macro
2. Chemical 2. Characterization 2. Partial 2. Semi-micro
3. Instrumental 3. Qualitative 3. Ultimate 3. Micro
4. Quantitative 4. Ultramicro

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Classification of Analyses
1. Based on the method

• Physical – involves visual comparison of the unknown against a standard. Organoleptic: sensory
properties of a product like taste, color, odor, etc.

• Chemical – involves the application of a chemical reaction; also called absolute methods (Gravimetry,
Titrimetry).

• Instrumental – based on the use of instruments; also called relative methods (Spectroscopy,
Chromatography, Electroanalytical methods).

a. Titrimetry – quantitative method that is based on measuring the amount of a reagent of known
concentration that is required to react completely with the analyte.

b. Gravimetry – quantitative method that is based on determining the mass of a pure compound to
which the analyte is chemically related.

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Classification of Analyses
c. Spectroscopy – analytical technique that is based on the interaction of electromagnetic radiation with
matter

d. Chromatography – analytical technique in which the components of a mixture are separated based on
differences in the rates at which they are carried through a fixed or stationary phase by a gaseous or liquid
mobile phase.

e. Electroanalytical method – analytical technique that is based on the measurement of an electrical


property of the system which is related to the amount of analyte in the sample

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Classification of Analyses

Physical analysis of water Chemical analysis of water


Color? Odor? Taste? (if applicable) Titration

Instrumental analysis of water


Determining pH of water sample
using pH meter
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Classification of Analyses

UV-vis Spectroscopy
Voltammetry

Column chromatography

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Classification of Analyses
2. Based on the purpose of determination

• Fundamental analysis - for the improvement/better understanding of the theory that supports an
analytical method including its limitations.

• Characterization analysis - for the characterization of the physical and chemical properties of a sample.

• Qualitative analysis - for the determination of the identity of the constituent species in a sample.

• Quantitative analysis - for the determination of how much of a constituent species is present in a sample.

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Classification of Analyses
3. Based on the extent of analysis

• Complete/exact – the amount of each constituent is determined

• Partial/proximate – only a selected constituent is determined

• Ultimate – the amount of all the element present is determined

Amount of each chemical substituent in shampoo (Complete)

Amount of paraben in shampoo (Partial)

Amount of each element: C, N, S, O, etc in shampoo (Ultimate)

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Classification of Analyses
4. Based on the sample size available

• Macro analysis: >100 mg, >100 uL

• Semi-micro analysis: 10-100 mg. 50-100 uL

• Micro analysis: 1-10 mg, <50 uL

• Ultramicro analysis: <1 mg

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Classification of Analytes
Weight percentage in the sample

Major constituent >1%


Minor constituent 0.01-1%
Trace constituent 0.001-0.01%
Ultratrace constituent <0.001%

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Analytical approach to solving problems

Step 1 Step 2 Step 3 Step 4 Step 5


Identify and Define Design Experimental Conduct Experiment Analyze Experimental Propose Solution to
Problem Procedure and Gather Data Data Problem

Establish design
criteria.
Identify potential Reduce and
What is the
interferents. transform data. Is the answer
problem’s context? Calibrate instruments
Establish validation Complete statistical sufficient?
What type of and equipment.
ciriteria. analysis. Does answer support
information is Gather data.
Select analytical Verify results. a new problem?
needed?
method. Interpret results.
Establish sampling
strategy.

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Typical steps

Selecting a
method

Interpretation Sampling

Sample
Analysis
Preparation

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Important terms

Atomic Absorption Technique: a chemical or physical principle that can be used


Spectroscopy to analyze a sample.

Method: a means for analyzing a sample for a specific


Pb in soil Pb in water Pb in blood
analyte in a specific matrix.

USP-NF Procedure: a set of written directions detailing how to apply


a method to a particular sample

AOAC Protocol: a set of written guidelines for analyzing a sample


specified by an agency; commonly encountered when
analytical chemistry is used to support or define public policy.
FDA

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Sampling
Sampling is the process of obtaining a portion of a material that will
represent the subject under study. Bulk sample
(Tons)
1. Gross sample – consists of several portions of the material to be tested
2. Laboratory sample – small portion of the sample that is actually
analyzed Gross sample (Kg)
3. Aliquot – measured portion of the volume of a liquid sample taken for
the analysis

Laboratory sample
(<1 grams)

Analytical sample

Aliquot

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Types of Sample
1. Selective sample - a sample which is deliberately chosen by using a sampling plan that screens out materials
with certain characteristics and/or selects only material with other relevant characteristics (directed/focused
sampling); often used in cases where contamination is suspected.

2. Composite sample – consists of two or more portions of material (collected at the same time) selected so as to
represent the material being investigated; appropriate when carrying out food surveys.

3. Representative sample – a sample that is typical of the parent material for the characteristic under inspection.
• Homogeneous – one phase, example: vegetable oil
• Heterogeneous – more than one phase, example: breakfast cereal
• Static system – composition of the parent material is permanent with respect to position in space and stable
in time; example: sample of oil in a drum
• Dynamic conditions – the parent material is changing with respect to time; removal of a portion at any instant
represents only a snapshot of that moment in time and in that particular location; example: estuarine water

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Types of Sample
4. Random sample – selected in a way that any portion of the material has an equal and known chance of being
chosen.
• Simple – any sample has an equal chance of selection
• Stratified – the lot is subdivided/stratified and a simple random sample selected from each stratum
• Systematic – the first sample is selected at random, then the subsequent samples are taken according to a
previously arranged interval

Important terms:
1. Analysis: a process that provides chemical or physical information about the constituents in the sample or the
sample itself.
2. Determination: an analysis of a sample to find the identity, concentration, or properties of the analyte.
3. Measurement: an experimental determination of an analyte’s chemical or physical properties.

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References
Christian et al. (2014). Analytical Chemistry, 7th ed. USA: John Wiley & Sons
Hargis, L. (1988). Analytical Chemistry. New Jersey: Prentice-Hall International Edition.
Harris, D. (2016) Quantitative Chemical Analysis, 9th edition.New York: W.H. Freeman and Company.
Harvey, D. (2016) Analytical Chemistry 2.0. Electronic version
Skoog et al. (2014). Fundamentals of Analytical Chemistry, 9th edition. Canada: Brooks/Cole Publishers Company

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