Introduction
It is very reliable and simple to use
It can analyze over 62 elements
It also measures the concentration of metals in sample
HISTORY
The technique was introduced in 1955 by Alan Walsh in Australia ( 1916
1998 ).
The first commercial atomic absorption spectrometer was introduced in 1959.
PRINCIPLE
The technique uses basically the principle that free atoms
( gas )
generated in an atomizer can absorb radiation at specific frequency.
Atomic absorption spectroscopy quantifies the absorption of ground state
atoms in the gaseous state.
The atoms absorb ultraviolet or visible light and make transitions to high
electronic energy levels. The analyte concentration is determined from the
amount of absorption.
Concentration measurements are usually determined from a working curve
after calibrating the instrument with standards of known concentration.
Atomic absorption is very common technique for detecting metals and
metalloids in environmental samples.
INSTRUMENTATION
LIGHT SOURCE
Hollow Cathode Lamp are the most common radiation source in AAS.
It contains a tungsten anode and a hollow cylindrical cathode made of the
element to be determined.
These are sealed in a glass tube filled with an inert gas (neon or argon ) .
Each element has its own unique lamp which must be used for that analysis .
Hollow Cathode Lamp
Hollow Cathode Lamp for Aluminum (Al)
Flame Atomization
Nebulizer suck up liquid samples at controlled rate.
Create a fine aerosol spray for introduction into flame.
Mix the aerosol and fuel and oxidant thoroughly for introduction into flame.
An aerosol is a colloid of fine solid particles or liquid droplets, in air or another
gas.
Flame Atomization
Disadvantages of Flame Atomization
Only 5-15% of the nebulized sample reaches the flame.
A minimum sample volume of 0.5-1.0 ml is needed to give a reliable reading.
Samples which are viscous require dilution with a solvent.
Electro Thermal Atomization
Uses a graphite coated furnace to vaporize the sample.
ln GFAAS sample, samples are deposited in a small graphite coated tube
which can then be heated to vaporize and atomize the analyte.
The graphite tubes are heated using a high current power supply.
Graphite Furnace Technique
Advantages of Graphite Furnace Technique
Small sample size
Very little or no sample preparation is needed
Sensitivity is enhanced
Direct analysis of solid samples
Disadvantages of Graphite Furnace Technique
Analyte may be lost at the ashing stage
The sample may not be completely atomized
The precision is poor than flame method
Analytical range is relatively low
MONOCHROMATOR
This is a very important part in an AA spectrometer. It is used to separate out
all of the thousands of lines.
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 light allows the determination of the selected
element in the presence of others.
DIFFRACTION GRATING
DETECTOR
The light selected by the monochromator is directed onto a detector that is
typically a photomultiplier tube , whose function is to convert the light signal
into an electrical signal proportional to the light intensity.
The processing of electrical signal is fulfilled by a signal amplifier . The signal
could be displayed for readout , or further fed into a data station for printout
by the requested format.
PHOTOMULTIPLIER
Calibration Curve
A calibration curve is used to determine the unknown concentration of an
element in a solution.
The instrument is calibrated using several solutions of known concentrations.
The absorbance of each known solution is measured and then a calibration
curve of concentration vs absorbance is plotted.
The sample solution is fed into the instrument, and the absorbance of the
element in this solution is measured.
The unknown concentration of the element is then calculated from the
calibration curve
Applications
1) Presence of metals as an impurity or in alloys could be done easily
2) Level of metals could be detected in tissue samples like Aluminum in blood
and Copper in brain tissues
3) Due to wear and tear there are different sorts of metals which are given in
the lubrication oils which could be determined for the analysis of conditions of
machines
4) Determination of elements in the agricultural and food products
ATOMIC ABSORPTION SPECTROSCOPY
Preston
islamabad
Introduction
It is very reliable and simple to use
It can analyze over 62 elements
It also measures the concentration of metals in sample
HISTORY
The technique was introduced in 1955 by Alan Walsh in Australia ( 1916
1998 ).
The first commercial atomic absorption spectrometer was introduced in 1959.
PRINCIPLE
The technique uses basically the principle that free atoms
( gas )
generated in an atomizer can absorb radiation at specific frequency.
Atomic absorption spectroscopy quantifies the absorption of ground state
atoms in the gaseous state.
The atoms absorb ultraviolet or visible light and make transitions to high
electronic energy levels. The analyte concentration is determined from the
amount of absorption.
Concentration measurements are usually determined from a working curve
after calibrating the instrument with standards of known concentration.
Atomic absorption is very common technique for detecting metals and
metalloids in environmental samples.
INSTRUMENTATION
LIGHT SOURCE
Hollow Cathode Lamp are the most common radiation source in AAS.
It contains a tungsten anode and a hollow cylindrical cathode made of the
element to be determined.
These are sealed in a glass tube filled with an inert gas (neon or argon ) .
Each element has its own unique lamp which must be used for that analysis .
Hollow Cathode Lamp
Hollow Cathode Lamp for Aluminum (Al)
Flame Atomization
Nebulizer suck up liquid samples at controlled rate.
Create a fine aerosol spray for introduction into flame.
Mix the aerosol and fuel and oxidant thoroughly for introduction into flame.
An aerosol is a colloid of fine solid particles or liquid droplets, in air or another
gas.
Flame Atomization
Disadvantages of Flame Atomization
Only 5-15% of the nebulized sample reaches the flame.
A minimum sample volume of 0.5-1.0 ml is needed to give a reliable reading.
Samples which are viscous require dilution with a solvent.
Electro Thermal Atomization
Uses a graphite coated furnace to vaporize the sample.
ln GFAAS sample, samples are deposited in a small graphite coated tube
which can then be heated to vaporize and atomize the analyte.
The graphite tubes are heated using a high current power supply.
Graphite Furnace Technique
Advantages of Graphite Furnace Technique
Small sample size
Very little or no sample preparation is needed
Sensitivity is enhanced
Direct analysis of solid samples
Disadvantages of Graphite Furnace Technique
Analyte may be lost at the ashing stage
The sample may not be completely atomized
The precision is poor than flame method
Analytical range is relatively low
MONOCHROMATOR
This is a very important part in an AA spectrometer. It is used to separate out
all of the thousands of lines.
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 light allows the determination of the selected
element in the presence of others.
DIFFRACTION GRATING
DETECTOR
The light selected by the monochromator is directed onto a detector that is
typically a photomultiplier tube , whose function is to convert the light signal
into an electrical signal proportional to the light intensity.
The processing of electrical signal is fulfilled by a signal amplifier . The signal
could be displayed for readout , or further fed into a data station for printout
by the requested format.
PHOTOMULTIPLIER
Calibration Curve
A calibration curve is used to determine the unknown concentration of an
element in a solution.
The instrument is calibrated using several solutions of known concentrations.
The absorbance of each known solution is measured and then a calibration
curve of concentration vs absorbance is plotted.
The sample solution is fed into the instrument, and the absorbance of the
element in this solution is measured.
The unknown concentration of the element is then calculated from the
calibration curve
Applications
1) Presence of metals as an impurity or in alloys could be done easily
2) Level of metals could be detected in tissue samples like Aluminum in blood
and Copper in brain tissues
3) Due to wear and tear there are different sorts of metals which are given in
the lubrication oils which could be determined for the analysis of conditions of
machines
4) Determination of elements in the agricultural and food products
THANK YOU
A transmission-geometry powder diffractometer, Debye-Scherrer camera is now
available in the BL15 experimental hutch (Table 1 & Figs. 1, 2). As a detector, the
camera has an imaging plate (IP) on the 2arm. A powder sample is sealed in a
glass capillary with a diameter of 0.1-0.5 mm and rotated at a speed of ~60 rpm
during measurements. The station is equipped with an off-line IP reader (Fig. 3). The
two-dimensional diffraction image (Fig. 4) can be transformed into one-dimensional
powder diffraction data using image-analysis software. NIST standard reference
materials (SRMs), silicon powder (640c) and lanthanum hexaboride powder (660a),
are also available for use as line position standards.
able 1. Properties of diffractometer
Camera length
286.5 mm
Measurement range (2)
5~75, 0.01 step*
Detector
Imaging plate (IP)
IP size
400 (H) 200 (W) mm2
Capillary diameter
0.1~0.5 mm
*Measurement range can be extended to higher angles (~120) by moving the 2 arm and exchanging the
IP.
The term Debye-Scherrer is named after the originators, Debye, Scherrer and Hull,
and is one of the oldest known powder diffraction geometries, though originally it was
used only with photographic film on a "powder diffraction camera". It uses a nearparallel incident beam of X-rays with sufficient cross-section to bathe the whole
powder-sample. One of its virtues is its simplicity as illustrated by the following
schematic of the Debye-Scherrer camera/diffractometer.
translate this geometry into the context of a synchrotron powder
diffractometer we get the arrangement depicted in the schematic
below. The sample is usually held in a glass capillary, which spins on
its axis to increase the number of crystallite orientations offered to
the incident X-ray beam, and of course the photographic film is
replaced by a detector which scans around the full 2 range by
rotating around the capillary; also shown is an example of a pattern
collected this way from Aerinite, a completely new mineral type
discovered in Morocco in 1997.
The main advantages of this method are that
it is relatively easy to use;
it produces a very good diffraction peak shape (the significance of peak shape
will become more apparent later during the course).
There are no real disadvantages to this method, though it is not practical to use it for
high pressure work. Also some purists do not like to have scattering in their pattern
from the glass nor have the inconvenience of loading their samples into a narrow
capillar
