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2/24/2017

Lecturer / Subject Leader :


Ms Haniza Kahar
hanizakahar@unikl.edu.my
012 391 6447
Admin Block - Lecturer Room 6

Introduction to Analytical
What is Analytical Chemistry..?
Chemistry
A branch of Chemistry that deals with :
-
Separating, identifying & quantifying of relative
amount of components in a sample
Analyte components of samples that are to
: means find be determined.
the composition & identity of It is a scientific discipline used to study:
chemical compounds / elements
present in a sample.
Importance - Forensics, quality
control, medical tests & etc.

What is Analytical Chemistry..? Methods of Analysis

Detection:
An analysis involves several steps & operation
Does the sample contain substance X ?
procedures which depend on:
Identification:
What is the identity of the substance X in the the particular problem
sample? your expertise
Separation: the apparatus or equipment available
How the substance X could be separated from the
The analyst should be involved in every step.
sample matrix for better quantitation and identification?
Quantitation:
How much of substance X is in the sample?

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Methods of Analysis Methods of Analysis

Qualitative vs Quantitative
I love coffee I drink 4 cups of
very much coffee everyday.

Classification of Analytical Methods Classification of Analytical Methods


Classical Methods Instrumental Methods
Classical Methods
Instrumental Methods Called as wet chemical methods Measurement of physical
Analyte is separated from a sample properties of analyte -
by: precipitation, extraction or conductivity, electrode potential
distillation. light absorption or emission,
mass to charge ratio; began to
Qualitative analyses: used for quantitative analysis.
The analyte is then treated using
suitable reagent that yield product Chromatographic /
that could be recognised by colour, electrophoretic techniques
melting point, solubilities, odours, replaced distillation, extraction
pH etc. & precipitation & separation of
complex mixtures prior to
Example: Qualitative analysis of quantitative & qualitative
3+ 2+ 2+
common ions ( Al , Fe , Cu ) analysis.
in water sample.

Classification of Analytical Methods Classical vs Instrumental Methods


Classical Methods Instrumental Methods
Quantitative analysis: These new methods of separation
The advantages of instrumental
1) Gravimetric measurement : & determination of chemical methods over classical methods
Determine the mass of analyte or species are known collectively as
some compound produced from Instrumental Method of
the analyte. Analysis.
1. The ability to perform trace analysis capable of detecting
Example: Precipitation method for individual atoms or molecules in a sample.
determining calcium in
2. Generally, large numbers of samples may be analyzed very
natural waters.
quickly.
2) Volumetric methods : Measure 3. Many instrumental methods can be automated.
the volume of standard reagents 4. Most instrumental methods are multi-channel techniques.
required to react completely with
5. Less skill & training is usually required to perform
the analyte.
Example: Standardization of sodium instrumental analysis than classical analysis.
hydroxide solutions

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Instrumental Method of Analysis Instrumental Method of Analysis

SPECTROSCOPIC METHOD a) SPECTROSCOPIC METHOD


SEPARATION METHOD
The procedures that uses light
to determine chemical Use term chromatography.
concentration. The main purpose is to
Measure the amount of separate, to identify & to
radiation produced or absorbed quantify the target sample in
by molecular or atomic species matrix.
of interest. There are different kinds of FT IR Spectrometer
Molecular & atomic Atomic Absorption
chromatography methods, Spectroscopy (AAS)
spectroscopic methods are which differ in the mobile
among the most widely used phase and the stationary
instrument analytical methods. phase used. UV VIS
Spectrophotometer

Instrumental Method of Analysis Sample Preparation

b) SEPARATION METHOD The different type of samples will be prepared


differently according to the method to be used.
Solid samples dilute in solvent / water, wet
ashing / dry ashing, microwave digestion.
Liquid Filter, dilute

Gas Chromatography (GC) High Performance Liquid


Chromatography
(HPLC)

Analytical Procedures & Instrumentation Typical Analysis Steps

Steps in a Typical Analysis 1) Define the Problem


What is the problem what needs to be found?
Define the problem Qualitative and/or quantitative..??
Select a method What will the information be used for? Who will use
Obtain a representative sample it?
When will it be needed?
Prepare the sample for analysis How accurate and precise does it have to be?
Perform any necessary chemical separations What is the budget?
Perform the measurement The analyst (the problem solver) should consult with
the client to plan a useful and efficient analysis,
Calculate the results and report
including how to obtain a useful sample.

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Typical Analysis Steps Typical Analysis Steps

2) Select a Method 3) Obtain a Representative Sample


Sample type / homogeneity / size
Sample size Expertise/experience
Sampling statistics / errors
Size of sample Cost
Sample preparation needed Speed 4) Prepare the Sample for Analysis
Concentration and range Does it need to be
Solid / liquid / gas?
(sensitivity needed) automated?
Ash or digest?
Selectivity needed Are methods available
Dissolve in water or solvent?
(interferences) in the chemical Chemical separation or masking of interferences needed?
Accuracy/precision needed literature? Need to concentrate the analyte?
Tools/instruments that are Are standard methods Need to adjust the solution conditions (pH, temperature,
available available? add reagents)?

Typical Analysis Steps Typical Analysis Steps

5) Perform Any Necessary Chemical Separations 7) Calculate the Results and Report
Distillation or Filtration..?
Precipitation..? Statistical analysis (reliability)
Solvent extraction or Solid phase extraction..? Report results with limitations / accuracy
Chromatography (may be done as part of the measurement information
step) State any possible source of errors during the
analysis
6) Perform the Measurement Give recommendations / suggestions for
Calibration improvement
Validation / controls / blanks
Replicates

Applications of Analytical Chemistry Examples of Role of Analytical


Chemistry in Modern Science
Chemistry Physics The concentrations of oxygen & of carbon dioxide are
determined in millions of blood samples every day &
Medicine Social Science
used to diagnose & treat illnesses.

Engineering Agricultural Smog-control is done by the measurement of quantities


of hydrocarbons, nitrogen oxides & carbon monoxide in
automobile exhaust.
Biology Geology

Analytical chemistry helps diagnose parathyroid


Analytical
diseases in humans measurements of ionized calcium in
Material Chemistry Environmental blood serum.
Science Science

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Examples of Role of Analytical


Chemistry in Modern Science

Determination of nitrogen in foods establishes their


protein content and thus their nutritional value.

Analysis of steel during its production permits


adjustment in the concentrations of such elements as
carbon, nickel & chromium to achieve a desired
strength, hardness, corrosion resistance & ductility. Any Question??