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Agilent 7500 Series ICP-MS An Introduction

Agilent 7500 Series ICP-MS An Introduction. Presented By: Ferdi Ferdian Kusnadhi. ICP - Inductively Coupled Plasma high temperature ion source decomposes, atomizes and ionizes the sample. MS - Mass Spectrometer featuring quadrupole mass analyzer mass range - 7 to 260 amu (Li to U...)

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Agilent 7500 Series ICP-MS An Introduction

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  1. Agilent 7500 Series ICP-MS An Introduction Presented By: Ferdi Ferdian Kusnadhi

  2. ICP - Inductively Coupled Plasma high temperature ion source decomposes, atomizes and ionizes the sample MS - Mass Spectrometer featuring quadrupole mass analyzer mass range - 7 to 260 amu (Li to U...) separates all elements in rapid sequential scan ions measured using dual mode detector ppt to ppm levels isotopic information available What is ICP-MS? An inorganic (elemental) analysis technique ICP-MS has the detection limits of GFAA and the sample throughput of ICP-OES

  3. Agilent 7500ce ICP-MS System withCollision Reaction Cell (CRC) Multi-element interference removal by on-axis octopole reaction cell Fast simultaneous dual mode detector (9 orders dynamic range) Reaction Gas Inlet High temperature 27MHz plasma generator Plasma Octopole Off-axis Lens High frequency hyperbolic quadrupole Low flow sample introduction system

  4. Agilent 7500 Series ICP-MS • Agilent 7500ce (G3272A) • Enviro, foods, biological... • Robust Octopole Reaction System (ORS) • Superb capability in the most complex matrix • Flexibility • Agilent 7500a (G3271A)– Standard ICP-MS • General purpose that does not require collision • Standard ShieldTorch System for cool plasma • Upgradeable to ORS • Agilent 7500cs (G3273A) • Semiconductor, R&D. • Ultra low BECs at high plasma power • Cool plasma also available

  5. Different ways of acquiring information from a sample Qualitative scan Semiquantitative Analysis Fully quantitative data

  6. Primary Agilent ICP-MS Team in Asia Pacific Dedicated Applications Support Dedicated Sales Support Asia Pacific Resource Dr Christopher Tye Asia Pacific Business Development Manager Based in Singapore Dr Deng-yun Chen Senior ICP-MS Applications Specialist Greater China Based in China Fan Chen ICP-MS Product Specialist SMT Kung-yu Chen Peak ICP-MS/semiconductor Sales Greater China Based in Taiwan David Wilkinson ICP-MSProduct Support Engineer Asia Pacific Based in Australia Yu-hong Chen ICP-MS Applications Specialist Greater China Based in China Fred Fryer Senior ICP-MS Applications Specialist South East Asia Based in Australia Jerry Leu ICP-MS Product Specialist Greater China Based in Taiwan

  7. Factory Trained Agilent ICP-MS Service Engineers(AP Region Only, excluded JPN) S Korea - 5 China - 8 Taiwan - 4 Hong Kong - 1 Vietnam - 1 Malaysia - 2 India - 1 Thailand - 1 Australia - 5 Singapore - 2 Country with Agilent ICP-MS installed New Zealand - 1 No Agilent ICP-MS installed

  8. Application Notes of interest to the Semiconductor Market • 5989-4348EN Determination of Impurities in Semiconductor Grade Hydrochloric Acid Using the Agilent 7500cs ICP-MS AN 12/2005 • 5988-8901EN Determination of Trace Metal Impurities in Semiconductor Grade Phosphoric Acid by High Sensitivity Reaction Cell ICP-MS AN 11/2004 • 5988-9190EN Analysis of Impurities in Semiconductor Grade Sulfuric Acid using the Agilent 7500cs ICP-MS AN 11/2004 • 5988-9529EN Characterization of Trace Impurities in Silicon Wafers by High Sensitivity Reaction Cell ICP-MS AN 11/2004 • 5988-9892EN Analysis of Impurities in Semiconductor Grade TMAH using the Agilent 7500cs ICP-MS AN 11/2004 • 5989-0629EN Direct Analysis of Photoresist and Related Solvents using the Agilent 7500cs ICP-MS AN 11/2004 • 5989-0321EN Analysis of Electroceramics Using Laser Ablation ICP-MS AN 10/2004

  9. Agilent ICP-MS in Asia PacificBig Growth - Big Rewards! • In FY06 we sold 84 units (in calendar year 2006 = 108!) • Our market share in ‘06 is 45%! • Why do we win? • Our technical advantages (especially the 7500ce) and the fact we have the best people supporting the field means we win most deals!

  10. M  M+ M  M- M+ M+ M+ M+ M+ M+ M+ M+ M+ M+ M+ M+ What is …. A Mass Spectrometer DETECTOR MASS FILTER ION SOURCE Produces ions that are separated according to mass and detected Chemical Ionization (CI) Electron Impact Ionization (EI) Time to Frequency (TOFs only) Time Of Flight (TOF) Electrospray Ionization (ESI) Ion Trap Electron Multiplier Quadrupole Atmospheric Pressure Photo Ionization (APPI) Atmospheric Pressure Chemical Ionization (APCI) Matrix Assisted Laser Desorption Ionization (MALDI)

  11. What Else Can Be Measured Using MS? • Many of you have been successful in selling organic MS • Used to get molecular or structural information from a sample • What about inorganic MS? • For characterising elements • Only dealing with the Periodic Table • Only 256 natural isotopes • Generally only quantitative data required • The difference between inorganic MS and organic MS lies primarily within one component of a mass spectrometer….. THE SOURCE

  12. Excellent detection limits low ppb - ppt for all elements Wide elemental coverage - from Li - U over 70 elements measurable High throughput all elements determined simultaneously 20 element run/3 replicates/washout in 3 minutes Wide dynamic range linear over 9 orders Powerful semiquantitative analysis no standards needed Isotopic analysis isotope ratios isotope dilution Routine technique many users run systems overnight Small size saves lab space mobile installations Advantages of ICP-MS

  13. Hg As Se Na 1180 ppm Sodium 7500ce – Widest Analytical Range of ANY ICP-MS- these 4 calibration plots were generated simultaneously in a single run Calibration rangesHg (0.01 – 2ppb) – Std ModeAs (0.1 – 200 ppb) – He ModeSe (0.1 – 200 ppb) – H2 ModeNa (0.05 – 1180 ppm) – He ModeOverall calibration range 10ppt (Hg) to 1180 ppm (Na) in a single method- without attenuating ion transmission to increase working rangeNaTypically, ICP-MS cannot measure above 200ppm Na without changing quad resolution or ion lens settingsHgHg detection limit by 7500ce is about 3ppt – 7500ce can QUANTIFY at 10ppt!7500ce can measure both Na and Hg in the same run!

  14. Elemental Coverage of ICP-MS Almost every element can be measured by ICP-MS (including actinides), mostly at extremely low limits of detection

  15. The Majority of Elements Have ppt and Below Detection Limits • Over 70 elements can be analysed at trace levels • In the same measurement cycle • Over a wide dynamic range

  16. Overview of Inorganic Analysis Techniques Atomic Absorption Spectrometry Light having a wavelength characteristic of the analyte is passed through the sample. The amount of light absorbed is proportional to concentration. ICP-Optical Emission Spectrometry Energy from the plasma promotes an electron to a higher energy level (excitation). Electron falls back and emits light at a characteristic wavelength. Light emission is proportional to concentration ICP-Mass Spectrometry Energy from the plasma ejects electron from shell (ionization). Result is a positively charged analyte ion. Ions are separated by the mass spectrometer and measured. Ions measured are directly proportional to analyte concentration. SequentialSimultaneous Criteria1 GFAAS ICP-OES ICP-OES ICP-MS Detection Limits ppt ppb ppb ppq-ppt Linear Range (orders) 2-3 4-6 4-6 8-9* Interferences Moderate Many Many Few Speed Slow Slow Fast Fast Elemental Coverage Poor Excellent Good Excellent Multi-element No Yes Yes Yes Simultaneous No No Yes Yes Sample Size uL mL mL uL or mL Capital Cost $$ $ $$ $$$ Operating Cost $$$ $$ $$ $$$ * Agilent 7500 Series only - (other ICP-MS - 8 orders) ICP-MS combines the sensitivity of GFAAS with the speed & flexibility of OES while offering a wider dynamic range and fewer interferences! 1 ICP-MS: The new standard for inorganic analysis American Laboratory News, Nov.1998

  17. Overview of Inorganic Analysis Techniques SequentialSimultaneous Criteria1 FAAS GFAAS ICP-OES ICP-OES ICP-MS Detection Limits +10ppb +50 ppt 1 ppb <1 ppb sub-ppt Linear Range (orders) 3-4 2-3 4-6 4-6 9* Interferences Chemical Many Many Some Some Some Spectral Some Many Some Some Some Matrix Many Many Some Some Few Speed Moderate Slow Slow Fast Fast Elemental Coverage Moderate Poor Good Good Excellent Typical no. 50 35 55 55 70 Multi-element No No Yes Yes Yes Simultaneous N/A N/A No Yes Yes Sample Size mL uL mL mL uL or mL Capital Cost $ $$ $ $$ $$$ Operating Cost $ $$$ $$ $$ $$$ * Agilent 7500 Series only - (other ICP-MS 8 orders) GFAAS operating cost high due to consumables (furnace tubes) and operator time (sample prep, many reruns due to small dynamic range)

  18. Who Uses Agilent ICP-MS WW ? • Over 2/3 of Agilent ICP-MS users Worldwide are either environmental or semiconductor, but other applications and lab types are extremely varied. Most users are in routine labs

  19. Comparison of Metals Techniques - Speed vs Detection Power Fast ICP-OES - most elements single figure ug/L DLs and good productivity ICP-MS - most elements single figure ng/L DLs and very productive Typical Speed of Analysis GFAAS is a key target market for ICP-MS! GFAAS – most elements sub-ug/L DLs; but poor throughput FAAS – most elements +10 ug/L DLs Slow ug/L (ppb) ng/L (ppt) mg/L (ppm) Typical Detection Limit

  20. <0.1 ppt 1 - 10 ppt >10 ppt Agilent 7500 - 3 Sigma Detection Limits Standard pneumatic nebuliser 3 sec/mass integration time * Class 1000 cleanroom with ShieldTorch 0.1 - 1ppt

  21. Extending the Capabilities of ICP-MS • ICP-MS instruments can be coupled to different sample introduction devices that extend the overall usefulness • Laser Ablation ICP-MS • Liquid (or Ion) Chromatography ICP-MS • Gas Chromatography ICP-MS • Capillary Electrophoresis ICP-MS

  22. Agilent 7500 ICP-MS Merchantek UP 213 Laser Ablation system Laser Ar Gas with ablated material Sample Laser Ablation ICP-MS • Pulsed Nd:YAG laser is used to ablate solid samples into the plasma • Useful for solids • No dissolution process required • Useful for bulk analysis and feature analysis • Oxide levels are much lower • Interferences less of a problem • Expensive !

  23. Connecting an LC to an ICP-MS

  24. Agilent GC-ICP-MS Interface GC-ICP-MS System used: ICP-MS: Agilent 7500 GC: Agilent 6890 Interface: Agilent G3158A Fully heated and insulated GC transfer line Modified torch with heated injector replaces standard demountable torch. “Silicosteel” transfer line and injector liner for inertness GC capillary can be inserted to tip of injector or terminated in GC oven GC effluent injected directly into base of plasma – essential for high boiling point compounds Species decomposed to atoms - atoms then ionized and passed into MS

  25. Key Benefits of ICP-MS • Wide Elemental Coverage • Almost every element can be measured • Very low detection limits – ng/L or sub ng/L • Equivalent to or lower than GFAAS (single-element technique) • Simple Mass spectra • Only small number of peaks for each element • Very wide dynamic range • Agilent systems provide 9 orders range – from <0.5ppt to >500ppm • High sample throughput • Multi-element analysis in 3 to 4 minutes • Relatively few interferences • Systems optimised to give minimal spectral interferences – low oxide (measured by CeO+/Ce+ ratio) and matrix interferences. Matrix-derived spectral interferences can be removed by collision/reaction cell

  26. Semiquantitative analysis • Simple process • spike sample with single internal standard • acquire data • software automatically corrects for • mass bias (mass response) • natural isotopic abundance • ionisation potential • print out data

  27. Example Semiquantitative Analysis IEAE Soil - 7 standard Values marked with an asterix * are not fully certified and for information only

  28. Environmental Drinking Water, Ambient Water, Sea Water Soils, Sludges, Solid Waste Plant material/agriculture Speciation of Hg, As, Pb, and Sn Clinical Blood, Urine, Serum Hair, Tissues Toxicology Nutrition/deficiency/vitamins Food Analysis Nutrition Toxic element and species monitoring QA/QC Pharmaceutical Routine heavy metal contamination Drug discovery Clinical trials HPI R&D QA/QC Semiconductor Process Chemicals Contaminants in Si Wafers Photoresists & Strippers Nuclear Fuel production Measurement of Radioisotopes Primary Cooling Water Typical Application Areas for ICP-MS • Geological • Soil, Rocks, Sediments • Hydrology • Isotope Ratio Studies • Laser Sampling • Archaeological • Artifact analysis, proof of origin • Tooth, bone, tusk, shell, coral analysis • Forensics • Gun Shot Residue • Materials Characterization • Point of Origin • Poisoning

  29. Metals Analysis can be Performed by 4 Different Techniques... • FAAS (Flame Atomic Absorption Spectroscopy) • Good, cost effective tool for users that do not require low detection limits and typically only analyze 1 to 5 elements • Low cost, cheap, ppm measurements • GFAAS (Graphite Furnace Atomic Absorption Spectroscopy) • Well documented but expensive analysis for users that require detection limits at the 50ppt level for only 1 to 5 elements • high cost, low productivity sub ppb measurements on a limited number of elements • high operating cost - consumables (graphite tubes) and operator time • ICP-OES (Inductively Coupled Plasma Optical Emission Spectroscopy) • Good multielement technique for customers that require measurements at the ppb level only • Cost effective multi element analysis at ppb levels • Also known as ICP-AES (Inductively Coupled Plasma Atomic Emission Spectroscopy) • ICP-MS (Inductively Coupled Plasma Mass Spectrometry) • Excellent technique for customers that require to measure samples over a wide dynamic range and that require low detection limits - can replace both GFAA AND ICPOES • Cost effective, fast multielement analysis from low detection limits to high concentrations – good flexibility Market in decline Market in decline Market flat Market is growing

  30. Advantages good detection limits for some elements - e.g. Cr in whole blood well documented methods good tolerance to dissolved solids unattended operation Disadvantages very very slow sample throughput poor linear dynamic range (3 orders) short term precision not as good as alternatives very susceptible to chemical interferences strong reliance on background correction hardware slow method development poor element flexibility high running costs Graphite Furnace Atomic Absorption Spectroscopy (GFAAS)

  31. Advantages multielement, fast flexible element selection well documented methods very good tolerance to dissolved solids good linear dynamic range Disadvantages relatively poor detection limits many spectral interferences sample consumption high (1 to 5 mL/min) element flexibility limited in older systems speed of analysis compromised in newer systems ICP-OES - Simultaneous

  32. Advantages excellent detection limits for most elements most elements in Periodic Table available good sample throughput wide dynamic range (8 to 9 orders) much simpler spectra than optical techniques low sample volume consumption mass spec - so isotopic information available flexible quantitation methods "semiquantitative" external calibrations isotope ratios Disadvantages dissolved solids/matrix effects - need to dilute samples more than other techniques capital cost high requires knowledgeable operator ICP-MS Due to the wide elemental coverage of ICP-MS or certain applications e.g. enviro - GFAAS, ICP-OES and single element detectors have been replaced by a single 7500!

  33. Price/Performance – How does ICP-MS Compare With Other Inorganic Techniques ? 200 Inductively Coupled Plasma Mass Spectrometry (Quadrupole) Typically 1ppt to 100ppm 150 Typical price range US$k Inductively Coupled Plasma Optical Emission Spectroscopy Typically 1ppb to >1000ppm (Simultaneous) 100 Graphite Furnace Atomic Absorption Typically 10ppt to 100ppb 50 Flame Atomic Absorption Typically 50ppb to 500ppm 1ppt 10ppt 100ppt 1ppb 10ppb 100ppb 1ppm 10ppm 100ppm 1000ppm Typical measurement range

  34. Agilent 7500 Series ICPMS Features • 1. Unmatched Interference Removal with ORS in He ModeSpectral comparison showing removal of ALL polyatomic interferences in a complex sample matrix – only the Agilent ORS can do this, using He collision mode. No other ICP-MS can use He collision mode – requires the focusing power of an octopole (applies to 7500ce, 7500cs) • 2. Detector Dynamic Range • 9 orders detector range, gives 10x more concentration range available all any other competitors (applies to all 7500 Series) • 3. Widest Analytical Measurement Range • Measurement of <10ppt Hg and >1000ppm Na – no other ICP-MS can do EITHER of these applications; the 7500ce can do both IN THE SAME RUN (applies to 7500ce) • 4. Lowest Metal Oxides of any ICP-MS • CeO less than 0.1% - possible due to He collision mode removing CeO – no other ICP-MS can do this (applies to 7500ce, 7500cs)

  35. Summary • Our product line up is perfectly aligned with the needs of the market, and is perfectly positioned to beat our competition • Price/performance • Upgradeability • Ease of use • Best design and build quality • Range of peripherals • Speciation market is growing fast • we are the only ICP-MS vendor with expertise in LC-ICP-MS and GC-ICP-MS • all the key speciation labs and opinion leaders use Agilent ICP-MS • We have the best hardware and applications support – because we have the best people!

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