Icp-Aes (Icp-Oes)

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ICP-AES (ICP-OES)

◼ Inductively coupled plasmas are at least 2X as hot


as flames or furnaces.
◼ The Ar plasma is the result of the flow of Ar ions in a
very strong, localized radio field.
◼ 6000-10000 K are common.
◼ Hot enough to excite most elements so they emit
light.
◼ Hot enough to prevent the formation of most
interferences, break down oxides and eliminate
most molecular spectral interferences.
◼ The way to do atomic emission spectroscopy today.
Atomic Spectroscopy for Metal
Analysis
Instruments for Atomic Spectroscopy
Inductively Coupled Plasma Atomic Emission (ICP-OES)
Atomic Spectroscopy for Metal
Analysis
Instruments for Atomic Spectroscopy
Inductively Coupled Plasma Atomic Emission (ICP-OES)

◼ Sample is nebulized and entrained in the flow of plasma support gas (Ar)
How does ICP work?
✓Radio frequency electrical current and associated magnetic field
✓Ionization of Ar gas (sparked by a Tesla coil)
✓Acceleration of ions and electrons by magnetic field
✓Energy in transferred from the electrons to the gas by collision so the
gas is heats up.
✓Production of high concentartion of both EXCITED ATOMS and ions
Atomic Spectroscopy for Metal
Analysis
Instruments for Atomic Spectroscopy
Inductively Coupled Plasma Atomic Emission (ICP-OES)

◼ Plasma torch inner tube contains the sample aerosol and Ar support gas
◼ Radio frequency generator produces a magnetic field which sets up
an oscillating current in the ions and electrons of the support gas (Ar)
◼ Produces high temperatures (up to 10,000 K)
Plasmas gas or

Three gases Support gas or


auxiliary gas
How to measure temperature?
◼ The plasma is thermodynamic equilibrium
◼ Cannot characterize a single temperature
◼ Four temperatures can be used
◼ Excitation Temp (Texc): measure of population density of the
energy levels (Boltzman equilibrium)
◼ Ionization Temp (Tion): measure of population density of
different ionization states (Saha equilibrium)
◼ Electron Temp (Te): a measure of the kinetic energy of the
electrons (related to the velocity of free electrons)
◼ Gas Temp (Tg or T kinetic): a measure of the kinetic energy of
the atoms.

Tg < Texc < Tion < Te


N1/N0 = g1/go exp(∆E/kT)
Performance characteristics
◼ Elements determined
◼ ~ 60 elements
◼ Line selection
◼ Most elements have several lines that can be selected
◼ Linear range
◼ Better than AAS
◼ Interferences
◼ Chemical interferences (lowered)
◼ Spectral interferences (still a problem)
◼ Detection limits
◼ Comparable or better than other atomic spectral
techniques
Calibration Curve

Ba Deionized water
Cr
5000 mg/mL Na
Cd
Zn Tap water (500 ppm hardness)
Intensity ratio

Pb 200 mg/mL Ca, 200 mg/mL Mg


( all solutions 0.1 M HCl)

0.03 0.1 0.3 1.0 3.0 10


Concentration mg/mL
Effect of Standardization
Frequency on Precision of ICP Data
Frequency of Relative standard deviatoin %
recalibration Concentration multiple above detection limit
101 to 102 102 to 103 103 to 104 104 to 105
0.5 3-7 1-3 1-2 1.5-2
2 5-10 2-6 1.5-2.5 2-3
5 8-15 3-10 3-7 4-8

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