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ICP / MS Technique

The document provides an overview of ICP-MS (Inductively Coupled Plasma Mass Spectrometry), detailing hardware components, analysis techniques, and the operational mechanism including sample introduction, ion generation, and mass analysis. It highlights advantages such as high sensitivity, low detection limits, and the ability to analyze nearly all elements of the periodic table. Additionally, it explains the importance of plasma conditions, ion optics, and various operational modes for efficient analysis.

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Gamal A. Hamid
2 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
3 Contents • Introduction • Hardware o Sample introduction o Interface o Ions optics o Mass analyzer • Peripherals • Interferences • Performance • Analysis • Applications
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 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 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 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 Elements analyzing using ICP/MS It can measure almost the whole periodic table in just about everything
10 Detection limits
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 ICP/MS Advantages • High sensitivity and stability. • Wide dynamic range. • Extremely low detection limits. • High productivity. • High Throughput. • Ease of Use. • Isotopic analysis.
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
15 Processes in the plasma
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 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 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 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 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
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 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 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 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 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 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 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 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 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 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 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 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.
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 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 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 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 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 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 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 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 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 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 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 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 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 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 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 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 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 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
53 KED
54
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 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 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 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 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 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 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 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 • 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 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 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.
66 Vacuum system
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 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 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 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 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 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.​..
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++
76 Interference types • Interferences in ICP-MS are generally classified into three major groups: 1. Spectral, 2. Matrix, 3. Physical.
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 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 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 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 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 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 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 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
85 Interference removal
87 MDL performance
88 Stability
89 Recovery
90 Sensitivity
91 iCAP RQ sensitivity
92 Relative standard deviation %RSD
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) .
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 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 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.
98 Water & chemicals • All types of acids, water and other used chemicals should be free of the required elements.
99 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.
100 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 .
101 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.
102 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.
103 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.
104 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.
105 • 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.
107 Almost Any Element in any matrix
108
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ICP / MS Technique

  • 1.
  • 2.
    2 To everyone whohas helped us with support, new books, hard/soft ware And over the internet Special thanks for Thermo http://www.thermofisher.com
  • 3.
    3 Contents • Introduction • Hardware oSample introduction o Interface o Ions optics o Mass analyzer • Peripherals • Interferences • Performance • Analysis • Applications
  • 5.
    5 Plasma “ICP” Gas inwhich 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 thatseparate 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 amulti-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 usingICP/MS It can measure almost the whole periodic table in just about everything
  • 10.
  • 11.
    11 Analysis speed • Considerthe 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 • Highsensitivity and stability. • Wide dynamic range. • Extremely low detection limits. • High productivity. • High Throughput. • Ease of Use. • Isotopic analysis.
  • 14.
    14 Plasma • Three plasmagas 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
  • 15.
  • 16.
    16 Hot and coldPlasma • 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 camerafor 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 • Allnew 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 • Operationof 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
  • 22.
    22 Isotope • Atom isthe 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 • Allisotopes 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 Massof 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, • Dwelltime (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 Displaysthe 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 (inmass 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 “Resolutionsetting 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 • Thisrefers 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 • Amass 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.
  • 35.
    35 Instrument The iCAP/MS instrumentcan 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 introductionsystem 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 • Fourchannel, 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 spraychamber • 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 • Allconnectivity (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 injectoris 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 (iongeneration) • 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 samplecone • 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 skimmercone • 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 extractionlens • 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 Rapidlens • 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 QCell, • 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 (CollisionCell 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 CellTechnology) 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
  • 53.
  • 54.
  • 55.
    55 Mass cut-off • QCellflatapole 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 DAassembly • 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 • quadrupolemass 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 ACthe 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 • Detectoris 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 detectordynode 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 • TheICP 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.
  • 66.
  • 68.
    68 Interlocks 1. Instrument CoversSafety 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 andCooling 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 isslightly 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 firstvacuum 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 speedcontrol (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.​..
  • 75.
    75 Interference • In anargon 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++
  • 76.
    76 Interference types • Interferencesin ICP-MS are generally classified into three major groups: 1. Spectral, 2. Matrix, 3. Physical.
  • 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 spectralinterferences 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 • Arecaused 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 • Aredue 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
  • 85.
  • 87.
  • 88.
  • 89.
  • 90.
  • 91.
  • 92.
  • 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) .
  • 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 areseveral 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.
  • 98.
    98 Water & chemicals •All types of acids, water and other used chemicals should be free of the required elements.
  • 99.
    99 Performance Test • Anautomatic 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.
  • 100.
    100 Method parameters • Inthe 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 .
  • 101.
    101 Elements “Analyte” Default elementproperties defined in the database are automatically selected for:- • Dwell time, • Channels, • Spacing, • Resolution, • And possible interferences of the selected isotope.
  • 102.
    102 Molecules • Select theMolecules 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.
  • 103.
    103 Interferences • Always takecare 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.
  • 104.
    104 Acquisition Parameters • Dwelltime (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.
  • 105.
    105 • Channels Displaysthe 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.
  • 107.
  • 108.
  • 109.