G-4 :Atomic Absorption Spectroscopy

Participants:
Tehreem Naz Areej Mansoor
Areeba Sundas
Momna Sabahat
Amna Manzoor Amna Sadia
Fatima
Atomic Absorption
Spectroscopy
Contents
• History
• Introduction
• Principle
• Instrumentation
• Application
History
The first Atomic absorption spectrometer was built by CSIRO scientist Alan Walsh in
1954.
Atomic absorption spectroscopy
Introduction :
⮚ Atomic Absorption spectroscopy is a very common technique for
detecting metals and metalloids in samples.

It is very reliable and simple to use.

⮚ Atomic absorption spectroscopy are more sensitive and needs much
smaller samples .
⮚ It can analyze over 62 elements.
⮚ It also measures the concentration of metals in the sample.
Principle
• In atomic spectroscopy, the analyte must be present in the atomic vapour
state. In atomic absorption spectrophotometry the atomisation is performed
by aspirating the sample solution into a flame where the analyte element is
converted into gaseous phase atoms.
• Alternatively, the sample is fed into a graphite furnace where the atomisation
is achieved electrothermally at relatively lower temperature, below 3000 K. As
the temperature of atomisation is low; most of the atoms remain in the
ground state which can absorb characteristic radiation from the radiation
source made from the analyte element.
• The atomic vapours containing free atoms of an element in the ground state
are illuminated by a radiation source emitting the characteristic radiation of
the analyte. In halogen cathode lamp the cathode is made of the element that
needs to be determined and gives radiations characteristic of the element.
INSTRUMENTATION
A typical atomic absorption spectrophotometer consists of
the following components.
⮚ Radiation source
⮚ Atom reservoir
⮚ Monochromator
⮚ Detector
⮚ Readout device
INSTRUMENTATION
Components:

● Radiation Sources :
⮚ All commercially available atomic absorption
spectrophotometers use a radiation source that emits the
characteristic spectrum of the element to be determined. The
essential requirement of the radiation source is that it gives a
constant and intense output. Generally two types of sources are
in use: line sources and continuum. Sources.
1. Hollow cathode lamp are the most common radiation source.
Radiation Sources
 Radiation source
Other types of radiation sources used are:
2 .Deuterium Lamp:
● Deuterium discharge lamps are used
in LS AAS for background correction
purposes.
● The radiation emitted by these lamps
decreases Significantly with increasing
wavelength.
 Radiation Source
3. Electrodeless discharge lamp:
● Electrodeless discharge lamp EDL contains a
small quantity of analyte as a metal or a salt
in a quartz bulb together with an inert gas,
typically Argon gas at low Pressure .
● The emission from EDL is higher than that
from HCL and the line width is generally
narrower .But EDLs needs a separate power
supply and might need a longer time to
stabilize .
Atomisers:
⮚ The purpose of atomiser is to provide a representative portion of
the analyte in the optical path and convert it into free neutral
ground state atoms.
⮚ In atomic absorption spectrophotometry, the flames and
furnaces that that generate a temperature in the range of
1500 to 3000 ºC are the most common methods of atomisation.
⮚ Two common types of atomisers used for generating atomic
species in the vapour phase are flame atomisers and
electrothermal atomisers.
 Flame Atomiser :
⮚ In a typical flame atomisation process,
the analyte solutions are generally
nebulised with the help of a nebuliser
into a spray chamber.
⮚ The aerosol so produced along with a
mixture of a burning gas and an oxidant
is directed into a suitable burner.
⮚ Flame temperature depends on fuel-
oxidant ratio and the requisite
temperature for analysis can be obtained
by varying the fuel-oxidant ratio.
Disadvantages of flame atomiser :

● Only about 10 % of the nebulised sample reach the flame and it is

further diluted by fuel and oxidant gases so that test material has
very small concentration in the flame.
● A minimum sample volume of 0.5-1.0ml is needed to give a
reliable measurement .
● Viscous samples such as blood ,serum ,oils require dilution with
the solvent .
Burners:
● Two major types of nebuliser burners used in AAS are
premix nebuliser-burner system and total consumption
burner.
● liquid is sprayed into a mixing chamber where the
droplets are mixed with the combustion gas and are sent
to the burner.
● On the other hand, in the total consumption burner, the
nebuliser and burner are combined. This is also called
turbulent flow burner.
Burners:
Monochromator:
● Monochromators are the devices that can provide radiation of
desired wavelength Out of the range of the wavelength emitted by
source or emitted by analyte sample.
● In AAS, it selects a given emission line and isolate it from the other
lines due to molecular band emission and all non absorbed lines.
● Most commercial AAS Instruments use differaction grating as
monochromators.
Monochromator:
● Types of
monochromators:
1. prism
2. Differaction grating
Detectors:
The most commonly used detector in atomic
absorptionspectrophotometry is photomultiplier (PM)
tube whose output is fed to a readout system.
Read out Device
⮚ The readout systems include meters, chart
recorders and digital display meters.
⮚ Modern instruments provide a fast display of
the experimental conditions, absorbance data,
statistical values and calibration curves, etc.
Applications
• AAS concerns the absorption of characteristic analyte radiation by
the atomised analyte element in the ground state. The wavelength(s)
of the radiation absorbed and the extent of the absorption form the
basis of the qualitative and quantitative determinations respectively.
• In flame atomic absorption spectrophotometry, either an air-
acetylene or a nitrous oxide-acetylene flame is used to evaporate the
solvent and dissociate the sample into its component atoms.
• It not an absolute method of analysis; the routine quantitative
determinations using AAS are based on calibration method. In
addition, the internal standard method and standard addition
methods are also employed.
Application
• Compounds of the alkali metals, some of the heavy metals such as lead
or cadmium and transition metals like manganese or nickel are all
atomised with good efficiency by flame However, a number of
refractory elements like V, Zr, Mo and B do not perform well with a
flame source.
• Graphite furnace atomic absorption spectrophotometry (GFAAS) in
which the atomisation is achieved electrothermally, is a much more
sensitive method as compared to flame AAS. The higher atom density
and longer residence time in the graphite tube improve furnace AAS
detection limits by a factor of up to 1000 compared to flame AAS. The
detection limits may extend to the sub-ppb range.
Application
• GFAAS requires a very small sample size and does not
require any sample preparation; even solid samples can
be analysed without dissolution.
• The background absorption effects in GFAAS are managed
by diluting the sample or selecting another resonance
wavelength line. In matrix modifier method a reagent is
added to the sample that may modify the matrix
behaviour and thereby tackle the problem of background.