ICP Lecture Notes PDF

EMISSION
SPECROSCOPY
Inductively Coupled
Argon Plasma (ICP)
Excitation
Electrothermal
Flames
Sample
Solution Aerosols Atomisation
or Solid
Emission
2
Skoog, Holler and Nieman, Ch. 10, 5th Edition
 It is possible at extremely high

temperature (~7000K -14000K) to
produce strong atomic emissions of
all elements
 However, ionisation problem is
endemic at high temperature
3
What is a Plasma?
 Ionised gas (highly charged cations,
electrons, neutral atoms & molecules)
 good conductor of electricity
 affected by magnetic field
4
Instrumentation
Axial view of the plasma torch
Emission
region Radial view of the plasma torch
Magnetic f
field Induction coils powered by
Radio-frequency generator
Concentric
Quartz
tubes Sample flow Ar gas introduced tangentially
at flow rate of 5-20L/min
5
Heat source - the ICP
Burner
 A 27- or 41-MHz induction coil is wrapped
around the upper opening of the quartz
apparatus.
 This inductor generates a rapidly oscillating

magnetic field.
 A spark from the Tesla coil ionizes the Ar gas

and free electrons are accelerated by the RF
field.
 The resulting ions and their associated

electrons from the Tesla coil interact with
the fluctuating magnetic field.
6
 The electrons in the magnetic field are accelerated and at
high speeds, cations and electrons known as the eddy current
collide with more Ar atoms producing further ionization .
 Ionisation produces highly charged species such as Ar+, Ar*,

Ar, e- etc.
 Within a few ms, a steady state results with high electron

density.
 Thus, a plasma is created at the top of the torch with

temperatures at a significant rise (to 6,000 – 10,000 K).
7
Plasma Characteristics
8
 Analyte atoms resides 2 seconds before
they reach 15-30mm height of the
plasma (temperature is 5000 to 8000K)
 Complete atomisation compare to flame
 Fewer chemical interference is
experienced…..Explain why?
 No ionisation interference
9
Desirable Properties of ICP
1. High resolution (0.01nm or / > 100,000)
2. Rapid signal acquisition and recovery
3. Low stray light
4. Wide dynamic range (>106)
5. Accurate and precise wavelength identification and
selection
6. Precision intensity readings (<1% relative standard
deviation at 500 x the detection limit)
7. High stability with respect to environmental changes
8. Easy background corrections
9. Computerized operation (readout, storage data
manipulations etc.)
10
Plasma Spectrometers
 Most spectrometers encompass
the entire UV-Visible spectrum
(170m to 800nm)
 Equipped with vacuum
spectrometer which can extend
analysis to 150 to 160nm
(especially for P, Si, C etc.)
11
Instrumentation
 programmed to determine resonance line of one
element at a time
 grating monochromator to disperse the emission
lines and a photomultiplier detector
 much slower and therefore consume more sample
Simultaneous multichannel
 simultaneous measurements of emission lines of up
to 60 elements at single excitation
 expensive (US$80,000)
 good reproducibility
12
Advantages
 Atomisation occurs in chemically inert environment
which results in lower inter-element intereference,
which is also a direct consequence of their higher
temperatures.
 High and uniform temperature therefore greater
precision
 They permit the determination of low concentrations
of elements that tend to form refractory compounds
(i.e., compounds such as the oxides of B,
 Low noise & background
 Multielement analysis
 long linear dynamic range
 ppb LODS
13
Disadvantages
 Complex spectra (sometimes)
 need high resolution monochromator
 high initial costs
 high operating costs
14
Sample Preparations
No difference to AAS
 liquid samples can be
aspirated directly
through the nebulizer
 solids may be dissolved
in suitable acids or
organic solvents
15
DIRECT ANALYSIS OF SOLIDS
 Electrothermal
vaporisation,
laser and spark
ablation, glow
discharge
16
Contrast to Flame Emission
 The temperature cross section of the plasma
is relatively uniform and a s a consequence
self absorption and self reversal effects are
not encountered. Thus, linear calibration
curves over several orders of magnitude of
concentration are usually observed.
17
Calibration Curves
 Plot of current versus analyte

concentration
 Log-Log plot is necessary due
to wide concentration range
at which it is linear
 Departure from linearity may
be encountered at high
concentration
18
19
Non Linearity is due to:
 self absorption
 erroneous background correction
 non linear responses of the detector
systems
Internal Standard is often used

 plot of intensity ratio vs concentrations
20
Interferences
 Almost free of chemical and matrix interference
effects - Explain
 Background correction is necessary at low

concentration of analyte - What is the problem?
 Spectral overlap is very real - How can this problem

be overcome? e.g Lines for Fe and Co+, for example,
occur at 369.0730 and 369.0723 nm, respectively
21

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EMISSION

 It is possible at extremely high

 good conductor of electricity

 affected by magnetic field

 This inductor generates a rapidly oscillating

 A spark from the Tesla coil ionizes the Ar gas

 The resulting ions and their associated

 Ionisation produces highly charged species such as Ar+, Ar*,

 Within a few ms, a steady state results with high electron

 Thus, a plasma is created at the top of the torch with

 need high resolution monochromator

 high initial costs

 high operating costs

 Plot of current versus analyte

Internal Standard is often used

 Background correction is necessary at low

 Spectral overlap is very real - How can this problem

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