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Basic Principles of AAS

Atomic absorption spectroscopy (AAS) is an analytical technique that quantifies metal ion concentrations in solutions. It works by measuring the absorption of light by ground state metal atoms. The instrument is calibrated using standard solutions to create a calibration curve relating absorption to concentration. Potential interferences include chemical interactions that reduce the number of absorbing atoms and ionization that depletes ground state atoms. Careful calibration, choice of analytes, and use of releasing agents can minimize these effects to obtain accurate concentration measurements.

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478 views22 pages

Basic Principles of AAS

Atomic absorption spectroscopy (AAS) is an analytical technique that quantifies metal ion concentrations in solutions. It works by measuring the absorption of light by ground state metal atoms. The instrument is calibrated using standard solutions to create a calibration curve relating absorption to concentration. Potential interferences include chemical interactions that reduce the number of absorbing atoms and ionization that depletes ground state atoms. Careful calibration, choice of analytes, and use of releasing agents can minimize these effects to obtain accurate concentration measurements.

Uploaded by

Shaira Cogollodo
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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R & D Soils Laboratory

Baracatan, Toril Davao City

Basic Principles of
AAS
What is AAS?
Instrumentation
Calibration
Interferences
Preventive Maintenance

Things to Remember prepared by:


ramindo
Jan 29, 2010
What is AAS?

AAS – Atomic Absorption Spectroscopy


It is an advanced analytical technique used to quantify the
concentration of metal ions in a sample solution.
The instrument measures the amount of light energy absorbed
by ground state atoms at a certain wavelength. The instrument is
optimized and calibrated with a series of standard solutions. A plot
showing the relationship between the amount of light absorbed and
the concentration of the analyte present in the standards is then
used to calculate unknown concentration of the sample.
The AdDU - CARL uses the Perkin-Elmer AAnalyst 100.
The AdDU - CARL is capable of analyzing the metal ions; K,
Ca, Mg, Na, Zn, Mn, Fe and Cu from soil, leaf, fruit, water and
fertilizer samples. Analysis of Au and Ag for ore analysis and Pb
and Hg for water and waste water analysis is also available.
Atomic Absorption

Every element has a specific number of


electrons associated with its nucleus.
These electrons are arranged around the
Cross-cut view of the atom nucleus in stable orbital configurations.

The most stable orbital configuration of an


atom is known as the “ground state”. If
energy is applied to an atom, the energy
will be absorbed and an outer electron will
be promoted to a less stable configuration
known as “excited state”. Since this state
is unstable, the atom will immediately
return to the “ground state”, releasing light
energy.
Energy levels
Elements detectable by AAS
Instrumentation
There are five basic components of an atomic absorption instrument:
1.) The light source that emits the spectrum of the element of interest.
(Hollow Cathode Lamp – HCL)
2.) An “absorption cell” in which atoms of the sample are produced.
(flame)
3.) A monochromator for light dispersion (Eschelette grating)
4.) A detector, which measures the light intensity and amplifies the signal.
(Photo Multiplier Tube - PMT)
5.) A display that shows the reading after it has been processed by the
instrument electronics.
Perkin Elmer AAnalyst 100
Perkin Elmer AAnalyst 100
Accessories

Air compressor
(air)
To be set at 80 to 120 psi

Acetylene Tank
(fuel)
To be set at 13 to 14 psi
Perkin Elmer AAnalyst 100 (Schematics)
The Hollow Cathode Lamp (HCL)
Inserting the HCL into the Lamp Compartment
The Burner System
The Burner Assembly
Instrument Calibration
Calibration curve for Calcium
0.4
Quantitative measurements 0.35 0.333
in atomic absorption are based 0.3

Absorbance
on Beer’s Law, which states that 0.25
0.2
0.174
concentration is proportional to 0.15
0.1
absorbance (C = kA). 0.05
0.097

0 0
0 0.5 1 1.5 2 2.5
% Calcium

It is well known, however,


Calibration curve for Sodium
that for most elements, 2
particularly at high 1.8
1.6
1.808

concentrations, the relationship Absorbance


1.4
1.2 1.235
between concentration and 1
absorbance deviates from Beer’s 0.8
0.6
0.76

Law and is not linear. 0.4


0.2
0 0
0 200 400 600 800 1000
ppm Na
In the past, it was necessary to plot an
absorbance vs. concentration curve for several
standards to get an accurate reading of elemental
constant when samples were out of the linear
range.

When microprocessors were incorporated into


atomic absorption instruments, automatic curve
correction became a reality. Modern atomic
absorption instruments have the ability to calibrate
and compute concentrations using absorbance
data from linear and nonlinear curves.

All current Perkin-Elmer AA spectrometers


allow either linear or nonlinear calibration using
multiple calibration standards.
Interferences
CHEMICAL INTERFERENCE
If the sample being analyzed contains a thermally stable
compound with the analyte that is not totally decomposed by the
energy of the flame, a chemical interference exists. As a result,
the number of atoms in the flame capable of absorbing light is
reduced.
Interference of Phosphate on Calcium
A good example of a chemical 1.2
interference is the influence of Ca + PO4 + 1000 mg/L La
phosphate on calcium. 1
Using an air-acetylene flame, 0.8
1.0
0.91 0.90
calcium phosphate does not totally 0.87

mg/L Ca
dissociate. As the phosphate 0.6
0.77
concentration is increased, the
absorbance of calcium decreases. 0.4

To correct for this chemical 0.2


interference, a large concentration of
lanthanum can be added or the nitrous 0
oxide-acetylene flame can be used. 0 0.5 1
mg/L P as PO4
1.5 2
Chemical interferences can normally
be overcome or controlled in two
ways:
A.) the use of a higher
temperature flame or
A higher temperature flame will
provide additional energy to break
down a compound which is stable
in a lower temperature flame.

B.) the addition of a releasing agent to the sample (or


standard) solution.
A releasing agent, or competing cation, when added to the
sample will preferentially react with the interferent
releasing the analyte and thus removing the interference.
Ionization interferences
Ionization interference occurs when the flame
temperature has enough energy to cause the removal of an
electron from the atom, creating an ion. As these electronic
rearrangements deplete the number of ground state
atoms, atomic absorption is reduced.
Ionization Interference Effect on Barium
The increase in absorption at 0.5
0.45
the barium resonance line and the 0.4
0.35

Absorbance
decrease in absorption at the 0.3
455.3 ion line
0.25
barium ion line as a function of 0.2 553.5 nm resonance line
0.15
added potassium show the 0.1
0.05
enhancement of ground state 0

atoms as the ion form is 0 500 1000 1500 2000


mg/L Potassium added
2500 3000

suppressed.
By adding a high concentration
of potassium, the effects of
ionization can be eliminated.
Ionization interferences can be
controlled by the addition of an excess of
an easily ionized element to the blank,
standards, and samples. For this
purpose, the alkali metals (K, Na, Rb, Cs)
which have very low ionization potentials,
are normally used.
A cooler flame may also be used to
eliminate ionization interferences, but
chemical interferences may result.
Matrix interferences
Matrix interferences can cause either a suppression or
enhancement of the analyte signal. Matrix interferences occur
when the physical characteristics (viscosity, burning
characteristics, surface tension) of the sample and standard
differ considerably. This can happen when the sample
solution contains a high concentration of dissolved salts or
acid, when the sample and standard solutions are at radically
different temperatures.
To compensate for matrix interferences, try to match as
closely as possible the matrix components in the sample,
standard, and blank. Any added reagent to the sample
during preparation should also be added to the
standards and the blank.
When organic solvent are being used, the standard and
sample solutions must be prepared with the same
solvent. All solutions should be allowed to come to the
same temperature before the determination is begun.
When there is no other way to compensate for the matrix
interference, the method of additions can be used.
Thank You!

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