ATOMIC
EMISSION
SPECTROSCOPY
Submitted By-:
Yudhveer Singh
&
Mandeep
CONTENT
• INTRODUCTION
• PRINCIPLE
• INSTRUMENTATION
• INTERFERENCES IN AES
• ADVANTAGES AND DISADVANTAGES
• CONCLUSION
Atomic Emission
Spectroscopy
• Used for qualitative identification of elements
present in the sample
• Also for quantitative analysis from ppm levels
to percent
• Multielement technique
• Can be used to determine metals,
metalloids, and some nonmetals
simultaneously
• Emission wavelength and energy are related
by ΔE = hc/λ
Principle of AES
• It uses quantitative measurement of the emission
from excited atoms to determine analyte
concentration.
• The analyte atoms are promoted to a higher
energy level by the sufficient energy that is
provided by the high temperature of the
atomization sources .
• The excited atoms decay back to lower levels by
emitting light
• In atomic Emission the sample is atomized and
the analyte atoms are excited to higher energy
levels.
Schematic Diagram of an
Atomic Emission
spectrometer
INSTRUMENTATION
• Excitation Source
• Nebulizer
• Spectrometer
• Monochromator
• Detector & readout device
Excitation Source
• Flame
• Plasma
• Arc and Spark
Flame
• Mechanism:
It consist of total consumption burner in
which sample is drawn through a capillary
tube which injected directly into flame and
flame is high temperature source that is
used to desolvate and vaporize a sample
and generate free atom for spectroscopic
study.
Plasma
• The inductively coupled plasma torch
consist of 3 concentric silica quartz tube.
• Argon stream that carries the sample in
the form of an aerosol, passes through the
central tube.
• Plasma is initiated by a spark from a tesla
coil. Argon gas ionized and emission is
measured.
Spark
• Mechanism:
It consist of the primary circuit a voltage of
110-220V is maintained. The high voltage
is obtained from setup transformer which
convert the line power to 15000-40000V
which then charge the capacitor. When
energy stored in the capacitor,
synchronous trigger the spark between the
electrodes.
Monochromator
• It is a device use to transmit narrow band
of wavelength which is chosen from
wavelength of wider range available.
• Types of monochromator:
(a) Prism Monochromator
(a) Grating Monochromator
INTERFERENCES
• Spectral interferences-:
• caused by background emission from continuous or recombination
phenomena,
• stray light from the line emission of high concentration elements,
• overlap of a spectral line from another element,
• or unresolved overlap of molecular band spectra.
• Corrections-:
• Background emission and stray light compensated for by subtracting
background emission determined by measurements adjacent to the
analyte wavelength peak.
• Correction factors can be applied if interference is well characterized
• Inter-element corrections will vary for the same emission line among
instruments because of differences in resolution, as determined by
the grating, the entrance and exit slit widths, and by the order of
dispersion
Physical interferences
• Cause-:
• effects associated with the sample nebulization and transport
processes.
• Changes in viscosity and surface tension can cause
significant inaccuracies,
• especially in samples containing high dissolved solids
• or high acid concentrations.
• Salt buildup at the tip of the nebulizer, affecting aerosol flow
rate and nebulization.
• Reduction-:
• by diluting the sample
• or by using a peristaltic pump,
• by using an internal standard
• or by using a high solids nebulizer.
Interferences
• Chemical interferences-:
• include molecular compound formation,
ionization effects, and solute vaporization
effects.
• Normally, these effects are not significant with
the ICP technique.
• Chemical interferences are highly dependent
on matrix type and the specific analyte
element.
Advantages of AES
• Highly specific
• Sensitive (low concentration 0.0001%)
• Metalloids (arsenic, silicon, selenium) have been
identified by this technique
• Samples in solid or liquid state and rarely gas
samples can be used
• Techniques requires minimum sample preparation
• No preliminary treatment of sample is required
• Spectra can be taken simultaneously for more than 2
elements and no separation is required. (1 – 10 mg)
• Rapid results, if automated, times required is 30 – 60
seconds
Disadvantages of AES
• Equipment is costly and experience is required for
handling and interpretation of spectra.
• Recording is done on a photographic plate which
takes sometime to develop, print and interpret the
results.
• The spectrograph is essentially a comparator. For
quantitative analysis, standards of similar
composition are required.
• Radiation intensities are not always reproducible
• Method limited to the analysis of elements
Applications of AES
• Qualitative analysis is done using AES in the same
manner in which it is done using FES. The
spectrum of the analyte is obtained and compared
with the atomic and ionic spectra of possible
elements in the analyte. Generally an element is
considered to be in the analyte if at least three
intense lines can be matched with those from the
spectrum of a known element.
• Quantitative analysis with a plasma can be done
using either an atomic or an ionic line. Ionic lines
are chosen for most analyses because they are
usually more intense at the temperatures of
plasmas than are the atomic lines.
Applications of AES
• In practice ~60 elements detectable
→ 10 ppb range most metals
• In determining the impurities of Ni, Mn, Cu, Al etc., in
iron and steel in metallurgical processes. The
percentage determined is 0.001% in iron to 30 in steel.
• Lubricating oils can be analysed for Ni, Fe, Mn etc.,
• Solid samples and animal tissues have been
analysed for several elements including K, Na, Ca,
Zn, Ni, etc.,
• To detect 40 elements in plants and soils, thus metal
deficiency in plants and soils can be diagnosed.
