Wardiere Inc.

TECHNICAL
Analysis

INSTRUCTOR ANLEE A. REFUERZO

TITLE: TECHNICAL ANALYSIS
CODE: ES7L
CREDIT UNITS: 3 units
HOURS PER WEEK: 3 hours per week
DESCRIPTION: The course covers the the
general principles of chemical analysis. It
also includes the study of standard
methods of Chemical Analysis
COURSE REQUIREMENTS
& GRADING SYSTEM

• Major Exams (Midterm and Finals) 45%

• Homework & Quizzes 15%
• Chapter Test 35%
• Attendance & Cooperation 5%
 LECTURE 1
INTRODUCTION

ROLE AND IMPORTANCE OF ANALYTICAL CHEMISTRY

IN VARIOUS ASPECTS OF LIFE

CLASSIFICATION AND TYPES OF ANALYSES

BASICS OF ANALYTICAL DESIGN AND

SELECTING A METHOD

SAMPLING PROTOCOLS
LECTURE 1: ROLE AND IMPORTANCE OF
ANALYTICAL CHEMISTRY IN VARIOUS
ASPECTS OF LIFE
What is Analytical Chemistry?

• Analytical chemistry is the science of obtaining,

processing, and communicating information
about the composition and structure of matter.
• 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
LECTURE 1: ROLE AND IMPORTANCE OF ANALYTICAL
CHEMISTRY IN VARIOUS ASPECTS OF LIFE
Where is analytical chemistry used?

Food ,Water and Drugs

Level of Contaminants and

impurity

Verification of Products

Medical diagnosis

Legal Purposes
 LECTURE 1: ROLE AND IMPORTANCE OF ANALYTICAL
CHEMISTRY IN VARIOUS ASPECTS OF LIFE
Application

PROCESS CONTROL INDUSTRY MEDICAL DIAGNOSTIC

Analysis of trace elements Analysis of blood or urine

ENVIRONMENTAL MONITORING PHARMACEUTICAL

Analysis of moisture in crude drug
Analysis of heavy metals in air, water,
soil

FOOD AND AGRICULTURE FORENSIC

Analysis pesticide residue Analysis of gunpowder residue

 LECTURE 1: ROLE AND IMPORTANCE OF ANALYTICAL
CHEMISTRY IN VARIOUS ASPECTS OF LIFE
The Analytical Process

1. Sample is 2. Separation (Sample preparation) 3. Analysis: Identification,

obtained Process of converting the sample Quantitation, Detection
into a form suitable for analysis
 LECTURE 1: CLASSIFICATION OF ANALYSES

Classification of Analyses
 Lecture 1: Classification of Analyses
1. Based on the method

Physical Chemical Instrumental

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)
 LECTURE 1: CLASSIFICATION OF ANALYSES
Instrumental Methods

TITRIMETRY
quantitative method that is based on
measuring the amount of a reagent of
known concentration that is required CHROMATOGRAPHY
to react completely with the analyte. analytical technique in which the components
of a mixture are separated based on
GRAVIMETRY differences in the rates at which they are
carried through a fixed or stationary phase by
quantitative method that is based on
a gaseous or liquid
determining the mass of a pure
mobile phase.
compound to which the analyte is
chemically related.

SPECTROSCOPY ELECTROANALYTICAL
analytical technique that is based on the
analytical technique that is based on
measurement of an electrical property of the
the interaction of electromagnetic
system which is related to the amount of
radiation with
analyte in the sample
matter
 LECTURE 1: CLASSIFICATION OF
ANALYSES
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
 LECTURE 1: CLASSIFICATION OF ANALYSES

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
LECTURE 1: BASICS OF ANALYTICAL DESIGN AND SELECTING A
METHOD

A typical quantitative analysis includes the sequence of steps

shown in the flow diagram.
LECTURE 1: BASICS OF ANALYTICAL DESIGN
AND SELECTING A METHOD

Important
terms
LECTURE 1: BASICS OF ANALYTICAL DESIGN
AND SELECTING A METHOD
Choosing a Method
• The selected method usually represents a compromise between
the accuracy required and the time and money available for the
analysis.

• Search the chemical literature to find appropriate procedures

or,
• if necessary, devise new procedures to make the required
measurements
LECTURE 1: BASICS OF ANALYTICAL DESIGN
AND SELECTING A METHOD
Acquire a Method
• An analysis must be performed on a sample that has the same
composition as the bulk of material from which it was taken

• A representative sample is used in

statistical analysis and is a subset of a
population that reflects the
characteristics of the entire population.

• Sampling is the process of collecting a small mass of a material

whose composition accurately represents the bulk of the material
being sampled.
LECTURE 1: BASICS OF ANALYTICAL DESIGN
AND SELECTING A METHOD
Processing the Sample
• Sample processing is a process done to a sample to prepare it for
testing

Processing the sample often divided into two steps:

• Sample Preparation
• Analysis

• Sample preparation is the process of converting a

representative sample into a form suitable for chemical
analysis.

Factors to be considered in Preparing samples:

• Sample with low concentration

• Homogeneity of sample
• Moisture of the sample
• Liquid Samples
LECTURE 1: BASICS OF ANALYTICAL DESIGN
AND SELECTING A METHOD
Processing the Sample

Sample with low Concentration

• Samples with a low concentration of analyte may

need to be concentrated prior to analysis.
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Homogeneity of Sample

• solid laboratory sample is ground to decrease

particle size, mixed to ensure homogeneity .
LECTURE 1: BASICS OF ANALYTICAL DESIGN
AND SELECTING A METHOD
Processing the Sample
Moisture of the sample

• any loss or gain of water changes the chemical

composition of solids, it is a good idea to dry
samples just before starting an analysis.
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Liquid Sample

• Liquid samples may undergo filtration or stirring

LECTURE 1: BASICS OF ANALYTICAL DESIGN
AND SELECTING A METHOD
Processing the Sample
Analysis

• If necessary, use different analytical methods on similar samples

to make sure that all methods give the same result and that the
choice of analytical method is not biasing the result

Defining Replicate Samples

• Most chemical analyses are performed on replicate
samples
Aliquot is a type of sub-sample that is taken or
extracted from an original sample.

Replication improves the quality of the results

and provides a measure of their reliability.
LECTURE 1: BASICS OF ANALYTICAL DESIGN
AND SELECTING A METHOD
Processing the Sample

Analysis

Preparing Solutions: Physical and Chemical Changes

• Strength of Solvent
• Heating with aqueous solutions
• Igniting the sample

The matrix, or sample matrix, is the collection of all of the

components in the sample containing an analyte. .

Techniques or reactions that work for only one analyte are said
to be specific.

Techniques or reactions that apply to only a few analytes are selective

LECTURE 1: BASICS OF ANALYTICAL DESIGN
AND SELECTING A METHOD
Eliminating Interferences
• Eliminate substances from the sample that may interfere with
measurement .
• Few chemical or physical proper ties of importance in chemical
analysis are unique to a single chemical species.

An interference or interferent is a species that causes an error in

an analysis by enhancing or attenuating (making smaller) the
quantity being measured.

The addition of lanthanum will overcome phosphate

interference in magnesium, calcium, and barium
determinations.
LECTURE 1: BASICS OF ANALYTICAL DESIGN
AND SELECTING A METHOD
Measuring Results

• Analytes with equal concentrations give different detector

responses.
• Therefore, the response must be measured for known
concentrations of each analyte.

A graph of detector response as a function of analyte concentration

is called a calibration curve or a standard curve.

To construct such a curve, standard

solutions containing known concentrations
LECTURE 1: BASICS OF ANALYTICAL DESIGN
AND SELECTING A METHOD
Calculating Results
• These computations are based on the raw experimental data
collected in the measurement step, the characteristics of the
measurement instruments, and the stoichiometry of the
analytical reaction.

Samples of these calculations appear throughout this book

LECTURE 1: BASICS OF ANALYTICAL DESIGN AND
SELECTING A METHOD

Evaluating Results by Estimating Reliability

• Analytical results are complete only when their reliability has

been estimated.
• The experimenter must provide some measure of the
uncertainties associated with computed results

Measurement Uncertainty (MU) relates to the margin of

doubt that exists for the result of any measurement

Reliability is the extent to which an "experiment, test, or any

measuring procedure yields the same results on repeated
trials
LECTURE 3: SAMPLING PROTOCOL
Sampling

Sampling is the process of obtaining a portion of a material that

will represent the subject under study.
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
3. Aliquot – measured portion of the volume of a liquid sample
taken for the analysis
LECTURE 3: SAMPLING PROTOCOL
Types of Sample

1. Selective sample - a sample that 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 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, for example vegetable oil
• Heterogeneous – more than one phase, for example breakfast cereal
• Static system – composition of the parent material is permanent concerning 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
LECTURE 3: SAMPLING PROTOCOL
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