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1. Gamal A. Hamid

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To everyone who has helped us with support,
new books, hard/soft ware And over the internet
Special thanks for Thermo
http://www.thermofisher.com

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• Introduction ICP
• Fundamental parts of ICP
• Introduction ICP/MS
• Fundamental parts of ICP/MS
• Analysis
• Comparison
• Applications

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Selecting a technique requires the consideration of a variety of important criteria, including:
• Detection limits
• Analytical working range
• Sample throughput
• Data quality
• Cost
• Interferences
• Ease-of-use
• Availability of proven methodology

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• Electrons in the element are excited.
• They jump to higher energy levels
(excited state).
• As the electrons fall back down
(ground state).
• Emitted(photon), the wavelength of
which refers to the discrete lines of the
emission spectrum.

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Inductively Coupled Plasma – Atomic Emission
Spectroscopy (ICP-AES)
• It is a multi-element analysis technique that
will dissociate a sample into its constituent
atoms and ions and exciting them to a higher
energy level.
• Cause them to emit light at a characteristic
wavelength , which will be analyzing.

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• The sample is nebulized and entrained in the flow of plasma support gas, which is typically Ar.
• The plasma torch consists of concentric quartz tubes.
• The inner tube contains the sample aerosol and Ar support gas and the outer tube contains flowing
gas to keep the tubes cool.
• A Radiofrequency (RF) generator produces an oscillating current in an induction coil that wraps
around the tubes.
• The induction coil creates an oscillating magnetic field, which produces an oscillating magnetic
field, The magnetic field in turn sets up an oscillating current in the ions and electrons of the
support gas (argon).
• As the ions and electrons collide with other atoms in the support gas and temp increase.

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• Gas in which a significant number
of atoms are ionized (significant
being >1%) Will interact with a
magnetic field Inductive coupling
between varying field and the
plasma .

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The iCAP 6000 spectrometer consists of
several major components:
1. Sample introduction parts. Plasma torch.
2. Gas control.
3. Radio frequency power generator.
4. Optical system; Polychromator.
5. CID detector with thermoelectric cooling.

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a. Pump.
b. Nebulizer.
c. Spray chamber.
d. Centre tube.
e. Torch.

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• 4-channel 12-roller pump, with its unique
drain sensor.
• The pump speed shall be computer
controlled to provide programmable
sample flows both during and between
sample measurements .
• Included for the pump to be automatically
switched into a standby mode upon
instrument shutdown.

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1. The sample solution after being sprayed
by the nebulizer.
2. Entrained in argon as a fine mist.
3. Passes through the center channel of the
torch and into the plasma.
Control of the nebulizer pressure, or flow, is
either through the control software or via a
manual adjustment.

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• Most samples are liquids that are pumped
through a nebulizer to produce a fine
spray.
• The large droplets are removed by a spray
chamber and the small droplets then pass
through to the plasma.

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Types of Centre tube
• 1.5mm quartz for aqueous solutions (single red ring).
• 1.0mm quartz for organic solutions (double red ring).
• 2.0mm quartz for high dissolved solids solutions (single
blue ring, standard on Duo configurations).
• 2.0mm Ceramic for HF solutions.

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• The quartz torch surrounded by the copper induction coil.
• The copper coil is made from copper tubing and is kept
cool by circulating water.
• RF energy is supplied to the coil which inductively heats
the argon gas to approximately 10,000oC.
• At this temperature the gas turns into a plasma of
positively charged atoms and electrons.
• The plasma is kept off the sides of the quartz torch by a
separate flow of argon supplied tangentially to the inside
torch.

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iCAP 7200
• The nebulizer gas flow is manually controlled from 0 to 0.4 MPa.
• The auxiliary gas is controlled with precision restrictors with flows of 0, 0.5, 1.0
and 1.5 L/min. The coolant flow is fixed at 12 L/min.
iCAP 7400
• The nebulizer gas is computer controlled through an MFC with options from 0 -
1.5 L/min with increments of 0.1 L/min.
• The auxiliary gas is computer controlled through an MFC with options from 0 -
2 L/min in 0.1 L/min increments.
• The coolant flow is computer controlled through an MFC from 0 - 20 L/min.

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• Swing frequency impedance control.
• Frequency changes to match plasma load.
• Fast response, no complex matching networks.
• >78% Efficiency Ability to run even difficult organics
e.g. methanol.
• Nominal Frequency: 27.12 M Hz.
• Full range of power control.
• 750-1600w Radial, 750-1350w Duo Optimum
performance for all sample types.

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Wavelength Range
• The instrument shall be able to operate over
the range of 166.250 to 847.000 nm
• All elements must be represented by at least
3 sensitive and 3 secondary lines to satisfy
the requirements of a wide range of sample
types.
• An optical resolution of better than 0.007nm
at 200nm, 0.014nm at 400nm and 0.021nm
at 600nm.

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• New CID86 chip (Charge Injection Device).
• Allows free choice of wavelengths from 166
to 847 nm.
• More stable, lower noise.
• With the ability to measure transient signals.
• Thermoelectric cooling by a triple stage
peltier.
• Reduce dark current and background noise
resulting in enhanced detection limits.

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• It is a multi-element analysis technique
where The ICP source converts the atoms
of the elements in the sample to ions. The
ions positive are then separated and
detected by the mass spectrometer.

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1. Generating an aerosol of the sample
2. Ionizing sample in the ICP source
3. Extracting ions in the sampling interface
4. Separating ions by mass
5. Detecting ions, calculating the concentrations
• Using ICP-MS, all kinds of materials can be measured.
• Solutions are vaporized using a nebulizer, while solids can be sampled
using laser ablation. Gasses can be sampled directly.

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• Three plasma gas flows pass through the torch
• High voltage spark acts as initial ion generator.
• RF power supplied to the load coil generates oscillating
magnetic field.
• Initial ions move with the field, and collide with other Ar
atoms.
• Collisions produce more ions which then also move with the
field, Collisions also generate heat.
• Result is a self-sustaining plasma with a temperature of >
6000ºC

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• All isotopes of one element have identical chemical
properties, which only involve the electrons surrounding the
nucleus.
• It is difficult to separate isotopes from each other by
chemical processes.
• The physical properties of the isotopes, such as their
masses, boiling points, and freezing points, are different.
• Isotopes can be most easily separated from each other using
physical processes.

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• The mass-to-charge ratio (m/Q) is a physical quantity that is
most widely used in the electrodynamics of charged particles.
• The importance of the mass-to-charge ratio, according to
classical electrodynamics, is that two particles with the same
mass-to-charge ratio move in the same path in a vacuum
when subjected to the same electric and magnetic fields.
• The m/z notation is used for the independent variable in
a mass spectrum.

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The iCAP/MS instrument can be divided into
four main components,
I. Sample introduction
II. Interface (ion generation)
III. Ion Optics (ion focusing)
IV. Mass Analyzer

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The sample introduction system of the iCAP
MS comprises the:-
• Peristaltic pump,
• The nebulizer,
• The peltier-cooled spray chamber
• The torch with the injector.

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• The interface is the region where ions generated in the
plasma are transferred from atmospheric pressure to the
vacuum region and introduced to the mass spectrometer as
an ion beam.
• The interface comprises
1. The sample cone,
2. The skimmer cone,
3. The extraction lens.
• The interface region is water-cooled because of the intense
heat of the plasma.

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• Positive ions sampled from the plasma
focused and steered toward the mass
spectrometer using electrostatic plates
(lenses) held at specific voltages.
• The ion optics region comprises:-
1. The RAPID lens,
2. The QCell,
3. The DA assembly.
• Ion optics and mass spectrometer both
under high vacuum (< 10-6 mbar)

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• Ions then pass into the mass
spectrometer where they are separated
according to their mass to charge ratio
• Ion optics and mass spectrometer both
under high vacuum (< 10-6 mbar).
1. Quadrupole
2. detector

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• Short digestion times. Minutes, not hours
• No loss of volatile elements. Complete recovery of
Hg, As, Cd etc.
• No acid fumes. Improved laboratory working
conditions.
• No sample contamination from the environment.
• No cross contamination.
• Low blanks, as minimal quantities of acids are used.
Microwave digestion is the best solution for samples preparation.

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• ICP, Multi-element primary standards,
• And/or a combination of single-element
and multi-element primary standards.
• It is a widely accepted practice to use
NIST SRMs (standard reference materials)
to validate various kinds of laboratory
operations

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All acids, water and other used chemicals should be free of the required elements.

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• ICP and ICP/MS Are a comparative
techniques in which the counts by
solutions of known concentrations used
to generate a calibration curve is
compared to the counts of unknown
samples to generate results.

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ICP/MSICP

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• Liquid samples are desolvated, vaporized,
atomized, and excited in an argon plasma.
• When the excited atoms relax back to the
ground state, they emit characteristic
wavelengths of light.
• A solid state detector collects all the
emitted wavelengths of light
simultaneously.
• For each wavelength, the amount of
emitted light is directly proportional to the
concentration of the element in the sample.
• Liquid samples are desolvated, vaporized,
atomized, and ionized in an argon plasma.
• Each element has a different mass; once
ionized, each element forms its own
characteristic mass spectrum.
• An ion counting detector counts the
number of ions at each mass-to-charge
ratio, which is directly proportional to the
concentration of each element in the
sample.
ICP ICP/MS

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• Wavelength selection • Isotopes selection
ICP ICP/MS

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• Same components • Same + Cooling
ICP ICP/MS

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• Optical system, axial and radial views • Ions optics
ICP ICP/MS

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• CIDs composed of doped
silicon wafers, containing a
two dimensional array of
light sensitive elements
called pixels.
• light strike the surface of
detector photons liberate
electrons in the detector
substrate which are then
trapped in the pixel sites;
• The signal is then digitized.
• Ions pass into the mass
spectrometer where they
are separated according to
their mass to charge ratio
• Detector change the
number of ions striking
the detector “counts per
second (cps)” into an
electrical signal that can
be measured
ICP ICP/MS

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• Spectral
• Physical
• Chemical
• Spectral
• Physical
• Matrix
ICP ICP/MS
The interferences for ICP and
ICP/MS discussed in details in the
ICP presentation and ICP/MS
presentation

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• The large linear dynamic range for ICP of about
105.
• For example, copper can be measured at the
324.75 nm wavelength from its detection limit of
about 0.002 ppm to over 200 ppm.
• In ICP, extrapolation of two point calibrations can
be accurately used to achieve orders of
magnitude above the top standard.

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105
• ICP-AES has a considerably wider
dynamic range, up to 105 , making it a
more suitable technique for highly
concentrated samples,
108
• ICP-MS typically operates at much lower
concentration levels so that linear ranges
up to 108 can be achieved for some
analytes.
ICP/MSICP

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• ICP-OES is mainly used for samples with
high total dissolved solids (TDS) or
suspended solids and is, therefore, more
robust for analyzing ground water,
wastewater, soil, and solid waste.
• ICP-OES has much higher tolerance for
TDS (up to 30%).
• Although both ICP-OES and ICP-MS can
be used for high matrix samples, sample
dilution is often necessary for use on ICP-
MS.
• ICP-MS has much lower tolerance for
TDS (about 0.2%)
ICP/MSICP

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• ICP-AES systems are easy to set up and
have to be adjusted relatively infrequently.
• If there are major spectral interferences,
method development can be complicated.
• In general, though, method development
is moderately easy, although the library of
methods is less than for the AAS and
GFAAS techniques.
• ICPs are capable of a high degree of
automation, and can run unattended.
• ICP-MS systems are getting easier to set
up for routine analysis.
• Some parts of the system (e.g., the
interface cones) may need regular
attention to preserve performance.
• Method development can be more
involved than with the other techniques
and requires a higher level of expertise.
• ICP-MS systems can be fully automated,
and can run unattended.
ICP/MSICP

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• EPA 200.5
• EPA 200.7
• EPA 6010
• ISO 11885:2007
• ISO/TC 190/SC3/WG1 N0252
• NPR 6425:1995
• NEN 6426:1995
• EN 12506: 2003
• EPA 200.8
• EPA 321.8 (IC-ICP-MS)
• EPA 6020
• ISO/DIS 17294-1:2004
• ISO 17294-2:2016
• NEN 6427:1999
ICP/MSICP

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• Environmental Analyses
• Petrochemical Analyses
• Metallurgical analyses
• Geological analyses
• Foodstuffs analyses
• Pharmaceutical analyses
• And more.

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• Waters – potable, natural, effluent,
wastewaters, sea and coastal waters
• Soils – soils, sediments, foliage, biota,
contaminated land, landfill sites
• Sludge's – solid and digested waste
• Air – chimney exhaust filters, air filters of
contaminated sites, dusts

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• Specifically oils & greases,
• Additives, pigments, intermediates
• Petrochemical applications at refineries,
wear metal analysis for industrial fleets,
heavy industry by-products
• Paints and inks

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• Steels and Alloys
• Precious metals – PGMs
• Bulk Materials – bronzes and brasses
• Traces – contaminants.

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• Rock samples, sediments, slags, ceramics,
cements
• Survey work, quality control, raw material
screening
• Robust
• Matrix tolerant
• Stability
• Detection limits (traces)

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• Bulk materials, raw and finished products
in food production
• Trace analysis of micronutrients
• Toxins - contamination of land and sea
• Animal feed
• Crop analysis

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Comfortably meet the most demanding global pharmaceutical
regulations and legislation, including;
• International Council on Harmonization (ICH) guideline Q3D
• U.S. Pharmacopoeia (USP) chapters, 232, 233 and 2232
Comply with the most rigorous data audit and security
measures.
• Qtegra ISDS software is fully compliant with Food and Drug
Administration (FDA) 21 CFR Part 11 and is equipped with
full IQ/OQ procedures for simple implementation in
GMP/GLP regulated environments

66. gamal_a_hamid@hotmail.com