It is a multi-element analysis technique where The ICP source converts the atoms of the elements in the sample to ions. These ions are then separated and detected by the mass spectrometer
2. 2
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3. 3
Contents
• Introduction
• Hardware
o Sample introduction
o Interface
o Ions optics
o Mass analyzer
• Peripherals
• Interferences
• Performance
• Analysis
• Applications
4.
5. 5
Plasma “ICP”
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 .
• Plasma is to change the sample aerosol into
positively charged ions.
6. 6
Mass
Analytical technique that separate positive
charge chemical species according to their
mass/charge ratio “m/z”, and introduce one
by one in order to be detected.
7. 7
ICP/MS
It is a multi-element analysis technique where The ICP source
converts the atoms of the elements in the sample to ions. These ions
are then separated and detected by the mass spectrometer.
8. 8
Analysis basic steps
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.
9. 9
Elements analyzing using ICP/MS
It can measure almost the whole periodic table in just about everything
11. 11
Analysis speed
• Consider the analysis time for each
technique, and the number of
samples you will need to test in a
day.
• Which technique will fit into your
production timelines?
• Does the same technique that
supports your timeline also support
the detection limits you require?
12. 12
ICP/MS Advantages
• High sensitivity and stability.
• Wide dynamic range.
• Extremely low detection limits.
• High productivity.
• High Throughput.
• Ease of Use.
• Isotopic analysis.
13.
14. 14
Plasma
• 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
16. 16
Hot and cold Plasma
• Cold plasma has been shown to be effective
in reducing argon based interferences, it is
even more prone to matrix suppression
than hot plasma and other polyatomic
interferences, previously not found under
hot plasma conditions, may be
preferentially formed.
• The use of cold plasma does provide an
additional benefit of a reduced background
equivalent concentration (BEC) for elements
with low first ionization potentials.
17. 17
Camera
• HD camera for remote
monitoring of plasma status.
• Useful for Plasma Optimization,
(e.g. O2 flow for organic
solvents).
• For monitor the cold or hot
plasma.
• Diagnose problems (see effect if
high TDS e.g. seawater).
18. 18
RF Generator
• All new solid state RF generator for ultimate
plasma robustness.
• 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 MHz
• Full range of power control Optimum
performance for all sample types.
19. 19
Argon gas
• Operation of the gas system shall be under full
computer control with mass flow controllers on all
three plasma gases.
• Coolant flow shall operate over 0-20 L/Min in steps
of 1 L/Min,
• Auxiliary flow shall operate over 0-2 L/Min in steps
of 0.1 L/Min, and.
• Nebulizer gas shall operate over 0-1.5 L/Min in
steps of 0.01 L/Min.
• An optional mass flow controller shall be available
for the addition of supplementary gases to the
plasma.
20. 20
Argon consumption (gas)
• A G size mixed argon gas cylinder
contains 8.7 cubic meters of gas (8700
Liters).
• The cylinder dimensions are 163cm high x
27cm diameter.
• Average rate of 20 L / min.
• The cylinder will be enough for more than
7 hours.
• More than 200 samples will analyzed
using one cylinder.
• Note: ( 1 L liquid = 781 L gas ) Argon
21.
22. 22
Isotope
• Atom is the basic structure from which all
matter is composed.
• Atomic number is the number of protons
• Atomic Mass is the ( protons + neutrons )
• Isotopes, Atoms for the same element with the same
number of protons and different numbers of neutrons.
23. 23
Isotopes separation
• 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.
24. 24
Isotope Abundance
Nickel Mass of atom “U” Abundance
1 58 Ni 57.935348 68.0769
2 60 Ni 59.930791 26.2231
3 61 Ni 60.931060 1.1399
4 62 Ni 61.928349 3.6345
5 64 Ni 63.927970 0.9256
Existence percentage of one isotope to all isotopes of the element
25. 25
Isobars & Isotones
• Isotopes : The atoms which have the same
number of protons but different numbers
of neutrons.
• Isobars : The atoms which have the same
mass number but different atomic
numbers.
• Isotones: the atoms which have different
atomic number and different atomic
masses but the same number of neutrons
26. 26
Dwell time,
• Dwell time (Sec.) the time spent for acquiring data at each of the channels which
make up a peak in the mass spectrum default 0.01 seconds.
• Major analytes (ppm level) require shorter dwell times.
• Minor analytes (ppt, ppb level) require longer dwell times.
• The length of time will ultimately affect the frequency with which data is acquired
at each mass.
• This will have a bearing on the final precision of the isotope ratio because of the
influence of various sources of noise on the analytical signal.
27. 27
Channels,
• Channels Displays the number of
channels used for each peak.
• The default number is when
entering an even number, the
system will automatically enter the
higher odd number.
28. 28
Spacing,
• Spacing (in mass units) (u) Displays the
distance in atomic mass units [u] between
the channels.
• Recommended Settings: Defining the
distance between the channels is closely
related to the number of channels
selected.
• For example, spacing of 0.1 with 9 channels
covers a mass width of ― 0.4 u either side
of the central channel of the peak (total
peak width of 0.8 u).
29. 29
Resolution (Resolving Power)
• Resolution is the ability of a mass
spectrometer to distinguish
between ions of different mass-to-
charge ratios.
Resolution = M/ΔM
• where M corresponds to m/z and
ΔM represents the full width at half
maximum (FWHM).
30. 30
Resolution
• Resolution “Resolution setting of the
quadrupole” .Displays the resolution
(Normal or High) for the selected isotope.
• By default, the resolution setting is
Normal.
Recommended Settings: Typically most
analytes are acquired using normal
resolution (NR).
• Select high resolution (HR) for analytes
that are at high concentration in the
samples (HR results in small intensity).
31. 31
Scan speed
• This refers to the rate at which the analyzer scans
over a particular mass range.
• Scan speed - In practice, the speed of the mass scan
is not limited by the quadrupole scan rate, but is
determined by the response time of the detector
and the "settle time" required by the quadrupole
after each mass jump.
• This settle time, which is typically of the order of a
few milliseconds, allows the quadrupole voltages to
stabilize at their new settings, prior to data
collection at the new set mass. A well-designed
32. 32
Mass spectra
• A mass spectrum will usually be
presented as a vertical bar graph, in
which each bar represents an ion
having a specific mass-to-charge
ratio (m/z) and the length of the bar
indicates the relative abundance of
the ion.
• The most intense ion is assigned an
abundance of 100, and it is referred
to as the base peak.
33. 33
Mass-to-charge ratio m/z
• 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.
34.
35. 35
Instrument
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
36. 36
I. Sample introduction system
The sample introduction system of the iCAP
MS comprises the:-
1. Peristaltic pump,
2. The nebulizer,
3. The peltier-cooled spray chamber
4. The torch with the injector.
37. 37
Introduction system
• Four channel, mini-roller peristaltic
pump for low sample pulsation.
• Peltier cooled spray chamber.
• Cyclonic spray chamber lose
mounted to torch.
• Easy access to mass flow controlled
gases.
• Removable sample tray.
38. 38
1. Peristaltic pump
• A peristaltic pump passes the liquid sample to the
nebulizer.
• Compact, low pulsation, 12 roller, 4 channel mini-
pump with inert rollers for improved reliability.
• Channel 1 for sample
• Channel 2 for drain
• Channel 3 for borohyride “ mercury kit”
• Channel 4 for acid “ mercury kit”
39. 39
2. The nebulizer
• The sample aerosol is generated by the
nebulizer.
• Sample introduced into the plasma as a fine
aerosol (mean droplet size < 10 µm - required
to enable efficient processing in the plasma).
• High performance, concentric nebulizers with
~0.4 mL/min sample consumption.
• Optional nebulizers in a range of flow rate
sizes and tolerance to total dissolved solids.
40. 40
3. The spray chamber
• The spray chamber filters out larger aerosol
droplets.
• Depending on the model ordered, the spray
chamber is made of either quartz or PFA.
• Low-volume, baffled cyclonic spray chamber
• Compatible with all 6 mm OD nebulizers.
• The spray chamber is cooled using a Peltier
cooled chiller to improve instrument
performance.
41. 41
4. Torch
• All connectivity (argon gas supplies and plasma
ignition) designed into the holder, reducing torch
complexity and improving usability.
• Pre-aligned torch mount.
• The torch consists of two concentric quartz tubes,
• The gas stream through the outer tube of the
torch shapes the plasma and shields the torch
body against the high temperatures of the plasma
(cool gas).
• The auxiliary gas flows through the inner tube.
42. 42
injector
• The injector is available with various internal
diameters (ID) and in various material for
different types of analysis 2.5 mm and 2.0
mm for organic samples.
• Injectors with smaller inner diameters are, for
example, employed with organic-based
solutions.
• Due to the semi-demountable design of the
torch, the injectors can easily be replaced.
43. 43
II. Interface (ion generation)
• 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.
44. 44
1. The sample cone
• The sample cone and the skimmer cone are
located at the right side of the interface to reduce
the flow of reactants comes from ICP torch.
• Sampler cone (1 mm i.d. orifice).
• The sample cone introduces ions from the plasma
into the first vacuum stage (interface vacuum)
and the skimmer cone admits the ions in the
mass spectrometer.
45. 45
2. The skimmer cone
• The skimmer cone is made of nickel
and the sample cone is made of
Ni/Cu.
• Sampler cone (0.7 mm i.d. orifice).
• Pt-tipped cones are optionally
available, for analysis of organics or
reactive acids like HF (hydrofluoric
acid).
46. 46
3. The extraction lens
• The extraction lens is located at the
left side of the interface.
• The extraction lens focuses and
accelerates the ions from the back
of the skimmer cone into the
intermediate vacuum region of the
analyzer.
47. 47
III. Ion Optics (ion focusing)
• 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)
48. 48
1. The Rapid lens
• Ions extracted from the iCAP Q interface are
accelerated to the RAPID (Right Angle Positive Ion
Deflection) lens which deflects analyte ions by 90 °
before they enter the QCell.
• The RAPID lens ensures that neutral particles from
the plasma pass directly out of the lens without
interacting with an active lens surface for improved
reliability and reduced maintenance.
• Elimination of neutral species and photons for
Highest Signal to Noise ratio of any Quadrupole
ICP-MS
49. 49
2. The Q Cell,
• Leaving the deflection device, the ions are
focused onto the entry of the collision cell
(QCell).
• It consists of a quadrupole with flat rods (f
pole) in a semi-contained region, which keeps
the ions close to the beam axis by a RF guide
field.
• The QCell can be pressurized (few 10-2mbar)
with helium or gas mixtures to remove
undesirable molecule ions by chemical
reactions (CCT mode) or by kinetic energy
discrimination (KED mode).
50. 50
Modes
• CCT (Collision Cell Technology)
• KED (Kinetic Energy Discrimination) collision cell mode.
• STD - standard mode. “no gases”
• CCTS, KEDS, STDS Used for Sensitivity Mode for samples without high matrix load.
• KED/KEDS and CCT/CCTS are the m odes of operation that can be employed for an
iCAP ICP-MS instrument fitted with a collision/reaction cell (QCell).
• (QCell) It consists of a quadrupole with flat rods (flat pole) in a semi-contained
region, which keeps the ions close to the beam axis by a RF guide field.
51. 51
CCT (Collision Cell Technology)
In this mode the CCT cell is pressurized with He gas
1. Polyatomic interfering species have larger cross
section areas than analyte ions of similar mass and
hence since they enter the cell with similar energies
they undergo more collisions, reaching the cell exit
with much lower kinetic energy than the
corresponding analyte ions (CCT).
2. Induce an appropriate energy barrier, will block the
polyatomic ions from passing into the analyzer,
whilst the analyte ions continue (KED).
52. 52
Kinetic Energy Discrimination (KED)
• He KED filters out unwanted
polyatomic interferences, based on
difference in cross-sectional size of the
analyte and polyatomic
• He KED filters out unwanted
polyatomic interferences
• High transmission enables analysis of
even low mass analytes in He KED
mode
55. 55
Mass cut-off
• QCell flatapole dynamically applies
Low Mass Cut Off (LCMO) relative to
target analyte
• Low mass cut off filters out
unwanted precursor ions; ions are
then unable to recombine later in
the QCell and backgrounds are
reduced further than KED alone
• All unwanted precursors that
contribute to interferences are
eliminated
56. 56
3. The DA assembly
• From the QCell, the ion beam is focused onto a small
differential aperture (DA plate), which separates the
intermediate vacuum stage from the high vacuum analyzer
region.
• Directly behind the DA plate, the beam is deflected again by the
DA lens to remove residual (collision) gas particles from the ion
beam.
57. 57
IV. Mass Analyzer
• 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
58. 58
1. Quadrupole
• quadrupole mass analyzer filters out ions of a specific
mass to charge ratio, depending on the RF voltage and
DC voltage applied to the quadrupole rods.
• Separates ions based on their m/z (mass to charge)
ratios.
• Only one mass (m/z) is allowed to reach the detector
at any given time.
• Quadrupole consists of 4 parallel rods
o One pair supplied with a positive DC voltage
and an RF voltage
o Second pair supplied with a negative DC
voltage and an RF voltage 180º out of phase
with the other pair
59. 59
Quadrupole Mass Analyzer
• Solid Molybdenum Quadrupole rods
• Low abundance sensitivity (< 0.5ppm at m-1
(m= 238U)
• Class leading mass stability (± 0.025 u / 8 h)
• High Scan speed: >90000 u/s (Li-U-Li in <5ms,
100μs at each mass) Mass range: 4 - 290 u.
• User definable resolution for improved
dynamic range and improved abundance
sensitivity
• Mass calibration assessed and automatically
updated when necessary through One Click
Setup.
60. 60
Principle
• Without AC the ions would stick to the negative loaded
rod and get lost.
• With the applied AC the ions get repelled from the rods
as soon the positive AC value is bigger than the negative
DC value.
• The inertia of Mx is smaller and the ion reacts fast to the
polarity change. The ion will pass through.
• The bigger mass M0 doesn‘t follow the polarity change
and will hit the rod at some point.
• The ion start to move in a spiral motion.
61. 61
Quadrupole mass spectra
• Some elements have only one isotope (e.g. Na, As and Bi); others have many more
(e.g. Cd (8) and Sn (10)).
• To cover the full mass range, the electronics rapidly change the conditions of the
quadrupole to allow different mass-to-charge ratio ions to pass through.
62. 62
2. Detector
• Detector is to change the number of ions striking
the detector “counts per second (cps)” into an
electrical signal that can be measured.
• The dynodes of the detector are covert with an
‘active film’ which increases the electron yield per
dynode (active film multiplier).
• Ions strike the first dynode surface causing an
emission of electrons. These electrons are then
attracted to the next dynode held at a higher
potential and therefore more secondary
electrons are generated.
• The dual mode secondary electron multiplier
(SEM).
63. 63
• The detector dynode chain can be divided into
an analog section (dynode 1 – 14) and a pulse
count section (dynode 15 – 29, respectively 1 –
29).
• The analog section provides low gain (e.g. 104)
for relatively large input signals.
• The pulse counting section operates at high
gain (e.g. 108) for very low-level signals.
• Detector switches automatically from PC to
analog when a large incoming ion count rate is
detected, it is called a simultaneous detector.
Signals
64. 64
Turbo molecular Pump
• The split-flow turbomolecular pump backed by
the forepump pumps the intermediate stage
and the high vacuum analyzer stage.
• The turbomolecular pump is located inside the
instrument.
• Active Pirani Gauge (APG) and an Active
Inverted Magnetron Gauge (AIM).
• The APG monitors the pressure in the interface
region. The AIM monitors the high vacuum in
the analyzer region.
65. 65
Vacuum System
• The ICP source operates at atmospheric pressure
while the mass analyzer and detector requires a
high vacuum for optimum performance.
• The iCAP Q instrument has a three-stage pumping
system realized by a rotary pump and split-flow
turbomolecular pump.
1. The interface vacuum region between the
sample cone and the skimmer cone.
2. The intermediate stage
3. The high vacuum analyzer stage.
68. 68
Interlocks
1. Instrument Covers Safety Switch
2. Argon Pressure
3. Source Enclosure Door
4. Torch Position
5. Sample Depth Position/Source Enclosure Door
6. Source Enclosure Exhaust
7. Leak Detection Swim Switch
8. RF Generator Water Flow
9. Sample Interface Temperature
10. Analyzer Pressure
11. Interface Pressure
The ignition of plasma will not start until the all of safety interlocks become green:
69. 69
Cooling system chiller
• Some components of the iCAP Q
mass spectrometer, for example
the interface and the RF
generated, must be water-cooled
for operation.
• The cooling water must be pure
and not contain additives.
• An in-line filter is supplied with
the instrument to guarantee
consistent water quality.
70. 70
Gas requirements
Plasma and Cooling Gas
• Argon Purity 99.996% or better
• Max. water content 5 ppm
• Supply rate max. 24 L/min
• Pressure min. 0.55 MPa (5.5 bar)/max. 0.6 MPa (6 bar)
CCT Gas
• Helium (for QCell) Purity 99.999% or better
• Max. water content 2 ppm
• Supply rate max. 10 mL/min per channel
• Pressure min. 0.05 MPa (0.5 bar)/max. 0.15 MPa (1.5 bar)
71. 71
Exhaust
• Argon is slightly heavier than air and tends to settle in
the bottom of the torch compartment.
• An argon environment is ideal for supporting high
voltage discharge.
• The vent is designed to “pull” the argon up and out of
the torch compartment.
• Exhaust velocity (plasma) 6 to 8 m/s
• Exhaust flow (plasma) 67 to 90 m³/h
• Exhaust velocity (heat) 4 to 6 m/s
• Exhaust flow (heat) 45 to 67m³/h
72. 72
Forepump
• The first vacuum region, the interface
vacuum region between the sample cone
and the skimmer cone, is pumped down by
a rotary vane pump, the so-called
forepump.
• The forepump is directly connected to the
interface.
• In addition to pumping down the interface
region, the forepump also provides backing
to the turbomolecular pump.
73. 73
Autosampler
• Full speed control (low to high), 96 well plate compatible
• Base platform for product accessory/new development
• 4x90/60/40/24/21 (360 samples max)
• Ideal for a wide range of analytical techniques including:
• AA
• ICP
• ICP/MS
• TOC
• UV-VIS
• fraction collection
• liquid handling, and much more...
74.
75. 75
Interference
• In an argon plasma, 80% of elements are
> 75% ionized
• Few ‘oxide’ molecular ions
Worst case Ce, forms around 2% [CeO]+
• Most elements yield mainly singly
charged ions
Worst case is Ba, at around 3% Ba++
77. 77
1. Spectral interference
• There is an endless list of spectral
interferences and this is part of the
Application to sort out the best way
to develop an analysis.
• Interferences are easily corrected
by selecting of another isotope of
the interfering element.
• Or use CCT or KED as mention
before.
78. 78
Sources of spectral interferences
1. Direct overlap between isobars, e.g. 114Sn overlap on 114Cd
2. Overlap from a polyatomic ion formed from the combination of species
derived from the plasma gas, sample solvent and/or sample matrix e.g.
40Ca16O overlap on 56Fe
3. Doubly-charged species resulting from ions created by the loss of two
electrons instead of just one. Because the quadrupole separates ions
based on m/z (mass over charge ratio), a doubly-charged ion (M2+) will
appear at mass M/2. An example of a doubly-charged interference would
be the 136Ba2+ overlap on 68Zn+
79. 79
Isobaric interferences
• Are caused by isotopes of different elements forming atomic ions with the same
nominal mass-to-charge ratio (m/z).
• 58Fe on 58Ni,64Ni on 64Zn,48Ca on 48Ti.
• They are best avoided by choosing alternative, noninterfered analyte isotopes, if
available.
• Given acknowledge of the natural abundances of the isotopes of all elements, isobaric
interferences are easily corrected by measuring the intensity of another isotope of the
interfering element and subtracting the appropriate correction factor from the
intensity of the interfered isotope.
80. 80
Polyatomic interferences
• Are due to the recombination of sample and matrix ions with Ar or other matrix
components (e.g. O, N, Cl, etc.) in the cooler regions of the plasma. Examples
include the following:
• 40Ar16O on 56Fe, 47Ti16O on 63Cu, 40Ar35Cl on 75As , 40Ar2 on 80Se.
• Most molecular ions formed by matrix components are predictable and may be
corrected for by applying correction factors determined by analyzing interference
solutions.
• Molecular interferences may also be avoided by using alternative, non-interfered
analyte isotopes. In some cases they can be reduced in severity or even eliminated
completely by using more appropriate sample introduction systems or optimizing
instrument operating conditions
81. 81
Doubly-charged ion interferences
• Are due to relatively rare doubly-charged matrix or sample ions with twice the
mass of the analyte and hence the same mass/charge ratio. The following is an
example: 90Zr++ on 45Sc.
• The formation of doubly-charged species can generally be minimized by
optimizing instrument operating conditions. Luckily, the first ionization potential
of Ar, although high enough to efficiently ionize most elements once, is not high
enough to produce doubly-charged ions of most elements, thus limiting their
numbers in Ar plasmas.
82. 82
2. Matrix effects
• Clogging of the orifices in either or both of the interface cones may be a problem
when samples with high total dissolved solid (TDS) contents are analyzed.
• The max. salt content less than 0.1 wt.%. The problem may be overcome by sample
dilution or may be use (e.g. an ultrasonic nebulizer with a desolvation unit).
• The presence of abundant, easily ionized matrix components such as Na in seawater
may lead to a suppression in the ionization efficiency of analytes.
• This effect may be reduced by sample dilution or by removal of the easily ionized
matrix component.
• Mass-charge effects between abundant heavy matrix ions (e.g. Pb, U) with high
kinetic energies and lighter analyte ions may also result in decreased analyte signal
intensities.
83. 83
3. Physical interference
• Physical interferences occur when
the physical properties of the
sample are vastly different than the
physical properties of the
calibration standards.
• Examples of physical properties
would include viscosity, density and
surface tension.
• Physical interferences within the
sample, injection and subsequently
inside the plasma.
84. 84
Solving physical interference
1. Dilution (degrades detection limits)
2. Matrix matching (must be known to be
effective)
3. Method of Standard Additions
4. Internal Standardization
Internal standards are dynamic drift corrections
used to correct for physical differences in samples
and standards by referencing all samples to the
same element performance
93. 93
Linear dynamic range
• The wide LDR means that the most sensitive elements will have a linear calibration up
to ~5 ppm and we show that for less sensitive elements or attenuated signals we can
calibrate up to 5000 ppm.
• This linearity will apply to any isotopes measured up in the count rate range of 0.1 cps
to over 109 cps (equivalent to over 10 orders of linear dynamic range) .
94.
95. 95
Sequence of analysis
1. The sample is introduced into the ICP plasma as an aerosol.
2. It is completely desolvated and the elements in the aerosol are converted
first into gaseous atoms and then ionized towards the end of the plasma.
3. (The ions formed by the ICP discharge are typically positive ions, M+ or M+2, therefore, elements
that prefer to form negative ions, such as Cl, I, F, etc. are very difficult to determine via ICP-MS).
4. Ions then brought into the mass spectrometer via the interface cones, which reduce the sample
amount, photons and the vacuum start in between.
5. The electrostatic lens, with positive charge, serves to collimate the ion beam and focus it into the
entrance aperture or slit of the mass spectrometer.
6. Once the ions enter the mass spectrometer, they are separated by their mass-to-charge ratio.
7. Filter is established that only allows ions of a single mass-to-charge ratio (m/e) pass through the
rods to the detector.
8. Most detectors use a high negative voltage on the front surface of the detector to attract the
positively charged ions to the detector .
96. 96
Standards preparation
There are several ways in making multi-element
working standard solutions:-
• By using standards from single-element
primary standards, 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.
97. 97
Sample preparation
Microwave digestion
• Microwave Digestion is a common technique used
to dissolve metals into an aqueous solution prior to
elemental analysis.
• The process involves irradiating a sample in strong
acids in a sealed vessel which raises the boiling
point of the acid, creating a super acid.
• This super acid, or combination of acids, increases
the speed of decomposition as well as the solubility
of metals in solution.
• Once they are in solution, it is possible to quantify
the samples for trace metal analysis.
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Water & chemicals
• All types of acids, water and other used chemicals should be free of the
required elements.
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Performance Test
• An automatic sequence can be started that switches on the plasma and will carry
out a routine check of the instrument’s performance by generating a performance
report.
• In case that the performance of the instrument does not match the requirements
from the performance report, an autotune sequence or mass calibration will be
automatically be triggered to fix the problems.
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Method parameters
• In the Method Parameters section,
you define all measurement settings
for your analytes.
• The availability of each parameter is
controlled by the type of Evaluation
defined for the Template .
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Elements “Analyte”
Default element properties defined in the
database are automatically selected for:-
• Dwell time,
• Channels,
• Spacing,
• Resolution,
• And possible interferences of the
selected isotope.
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Molecules
• Select the Molecules tab, if you want to
use analytes based on polyatomic ions
and background ions.
• Symbol displays the combinations of the
different isotopes of the participating
elements of the polyatomic ion (or the
background).
• Mass displays the mass of the
polyatomic ion.
• Abundance displays the value of the
calculated natural abundance of the
polyatomic ion.
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Interferences
• Always take care of
interferences, when creating the
list of analytes.
• A list of the isotopes if this
element is displayed with
symbol, mass, abundance and
known interferences as stored in
the element database.
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Acquisition Parameters
• Dwell time (in s) the time spent measuring this analyte on a single channel. By default,
this value is set to 0.01 seconds.
• Major analytes (ppm level) require shorter dwell times. Minor analytes (ppt, ppb level)
require longer dwell times.
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• Channels Displays the number of channels used for
each peak. The default number is when entering an
even number, the system will automatically enter the
higher odd number.
• Spacing (in mass units) (u) Displays the distance in
atomic mass units [u] between the channels.
• Resolution “Resolution setting of the quadrupole”
.Displays the resolution (Normal or High) for the
selected isotope. By default, the resolution setting is
Normal. The Number of sweeps to be performed
during one survey scan can be defined.