Spectros

Analytical Chemistry: CHE3724 Module
Dr RC Chokwe
Florida Science Campus
Eureka building
Chemistry Department
K-M-032
[email protected]
+27 11-670-9393
Topics to be covered
• Spectroscopy
• Chromatography
Atomic absorption spectroscopy
• It measures the absorption of light by atoms in

the flame
• This technique is used to detect metals and
metalloids in samples
• Is very reliable and easy to use
• Can analyse up to 62 elements
Components of an AAS instrument
• Light source
• Nebulizer
• Atomizer
• Monochromator
• Detector
Light source in AAS
How the HCL works Hollow cathode lamp

• It contains a tungsten anode and cathode.
• The cathode is a hollow cylindrical tube which
is lined by the element to be determined.
• These are sealed in the glass tube filled with
an inert gas like neon or argon at a low
pressure.
• At the end of the cylinder is a window, made
up of quartz or pyrex, transparent to the
emitted radiation.
• Each element in question will thus emit
monochromatic radiation characteristic of the
emission spectrum of that particular element
involved. So, each element has its own unique
lamp which must be used for the analysis.
Nebulizer
• Sucks up the sample at a controlled rate.
• Creates a fine aerosol to introduce into the

flame.
• The aerosol, the fuel and oxidant are mixed

thoroughly for the introduction into the flame.
Atomizer
• The elements which needs to be analysed

needs to be in the atomic state.
• It breaks down the molecules into atoms by

exposing the analyte to high temperatures in a
flame or graphite furnace
Flame atomizer
• The flame is created by mixing oxidant gas and fuel

gas.
• Air-acetylene with a temperature of 2300°C and

nitrous oxide-acetylene with a temperature of
2700°C flames are the commonly used flames.
• Liquid samples are used with flame atomizer

Graphene atomizer
• Uses a graphite coated furnace to vaporize the

sample.
• Samples are coated on a graphite coated tube which

is then heated, then vaporize and atomize the
sample.
• The graphite tube are heated using a high current

power supply.
Monochromator
• A monochromator is used to select the specific

wavelength of light which is absorbed by the
sample and to exclude other wavelengths.
• The selection of the specific wavelength

allows the determination of the element.
Detector
• The detector is usually a photomultiplier tube.
• The photomultiplier tube functions to convert

the light signal into an electrical signal that is
proportional to the light intensity.
Atomic Absorption Spectroscopy (AAS)
Principle of AAS
• Molecules are converted into free atoms which
remain in the ground state.
• These atoms are capable of absorbing radiation of

their own specific wavelength.
• When radiation of their specific wavelength is passed

through the flame, part of the radiation will be
absorbed.
• These radiation will excite the atoms from the ground

state to a higher energy level.
• The difference between the emitted light and the

transmitted light will give the amount that was
absorbed.
• The absorbed light is directly proportional to the

concentration of the element in the sample.
B for Biology: Spectrophotometry - Atomic Absorption Spectrophotometry (namrataheda.blogspot.com)
Elements that can be analysed by AAS
atomic absorption spectroscopy (slideshare.net)

Atomic Emission Spectroscopy (AES)
• Is a spectroscopic method that uses the intensity of light

emitted from a flame at a particular wavelength to determine
the quantity of an element in a sample.
• The wavelength of the atomic spectral line gives the identity

of the element while the intensity of the emitted light is
proportional to the number of atoms of the element.
• The instruments are design to measure up to 10 elements

simultaneously, usually elements in group I and II of the
periodic table.
Components of an AES instrument
• Nebulizer
• Atomizer/ flame
• Monochromator
• Detector
Sources of energy in AES
• Flame or an Induced coupled plasm (ICP).
• The flame with temperature in the range 1700 –

3150 °C is useful for elements with low excitation
energies eg Na, K and Ca.
• ICP with temperature range 6000 - 7000°C is useful

for elements with high excitation energies.
Principle of AES
• The solution containing the metal to be
analyzed is placed into the flame, whereby
the solvent is evaporated, leaving behind only
the solid.
• The solid is then dissociated by vaporization.
• The volatilization of the molecules in the
solid produces free atoms which then, due to
heat, excites to a higher energy level.
• When they return to the ground state they
emit light at their characteristic wavelength
• The intensity of the radiation emitted is
directly proportional to the number of atoms
in the flame, which are directly proportional
to the concentration of the element in the
sample
B for Biology: Spectrophotometry - Atomic Absorption Spectrophotometry

(namrataheda.blogspot.com)
ICP-OES
• Type of emission spectroscopy that uses the inductively coupled plasma to
produce excited atoms and ions that emit EMR at wavelengths
characteristic of a particular elements
• Plasma: conducting gaseous mixture containing a significant concentration
of ions and electrons
• ICP-OES and ICP-MS usually uses argon gas
ICP-OES Instrument
https://biotecharticles.com/Biotechnology-products-Article/Speciation-Analysis-of-Silver-Ions-using-ICP-OES-4233.html
ICP Torch
• The sample is nebulized then it enters the flow of
plasma gas, which is typically argon.
• The plasma torch consists of three concentric quartz
tubes.
• The inner tube contains the sample aerosol, the
middle one carries the plasma gas and the outer
tube contains tangential argon flow, to keep the
tubes cool.
• Radiofrequency (RF) generator produces and
oscillates the current in an induction coil that wraps
around the tubes.
• The induction coil creates an oscillating magnetic
field, which in turn sets up as oscillating current in
the ions and electrons of the plasma gas.
• The resulting collisions with the abundant
unionized gas give rise to resistive heating,
providing temperatures as high as 10 000 K at the
base of the plasma.
• Between 6000 and 8000 K at a height of 15-20 mm
above the coil, where emission is usually
measured.
https://asdlib.org/imageandvideoexchangeforum/inductively-coupled-
plasma-torch/
Configuration of the plasma
UV-VIS Spectroscopy
• How a Simple UV-visible Spectrophotometer

Works - YouTube
UV-Vis spectrophometer
Single beam
Schematic Diagram Of A Single Beam Uv Vis Spectrophotometer - Home Design Ideas (thathipsterlife.com)
Double beam
Schematic representation of the dual-beam UV-VIS spectrometer. | Download Scientific Diagram

(researchgate.net)
ICP / AAS Comparison (slideshare.net)
Detection limits on Atomic spectrometric
Report outline
• Clearly write your full name and student number

on each report
• Abstract (200 WORDS MAX)
• Introduction
• Experimentation/ method
• Results
• Discussion
• Conclusion/s
• References
Schedule for the Week

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Analytical Chemistry: CHE3724 Module

• It measures the absorption of light by atoms in

How the HCL works Hollow cathode lamp

• Sucks up the sample at a controlled rate.

• Creates a fine aerosol to introduce into the

• The aerosol, the fuel and oxidant are mixed

• The elements which needs to be analysed

• It breaks down the molecules into atoms by

• The flame is created by mixing oxidant gas and fuel

• Air-acetylene with a temperature of 2300°C and

• Liquid samples are used with flame atomizer

• Uses a graphite coated furnace to vaporize the

• Samples are coated on a graphite coated tube which

• The graphite tube are heated using a high current

• A monochromator is used to select the specific

• The selection of the specific wavelength

• The detector is usually a photomultiplier tube.

• The photomultiplier tube functions to convert

• These atoms are capable of absorbing radiation of

• When radiation of their specific wavelength is passed

• These radiation will excite the atoms from the ground

• The difference between the emitted light and the

• The absorbed light is directly proportional to the

atomic absorption spectroscopy (slideshare.net)

• Is a spectroscopic method that uses the intensity of light

• The wavelength of the atomic spectral line gives the identity

• The instruments are design to measure up to 10 elements

• Flame or an Induced coupled plasm (ICP).

• The flame with temperature in the range 1700 –

• ICP with temperature range 6000 - 7000°C is useful

B for Biology: Spectrophotometry - Atomic Absorption Spectrophotometry

• How a Simple UV-visible Spectrophotometer

Schematic representation of the dual-beam UV-VIS spectrometer. | Download Scientific Diagram

• Clearly write your full name and student number

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