Notes
Slide Show
Outline
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Glow Discharge MS, an affordable technique for the lab
  • Meike Hamester and Lothar Rottmann
  • Thermo Electron (Bremen)
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Bremen - Germany
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Thermo Electron (Bremen)
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Thermo Bremen Manufacturing
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Glow Discharge Mass Spectrometry – History
  • Gas discharge ion sources are used since the early days of mass spectrometry by pioneers like
    • Joseph John Thomson
    • Francis Aston
    • Arthur J. Dempster
    • Problem with gas discharge ion sources: interfacing HV to mass spectrometer
  • GD-MS in mid 80‘s as technique for direct trace analysis of solid samples
    • First commercial instrument launched 1985
    • Successful instrument VG9000



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Finnigan Element GD
  • It´s time to reinvent GD-MS…


  • …based on proven
    HR-ICP-MS
    Finnigan Element2


  • …for routine analysis
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Worldwide 350 ELEMENT HR ICP-MS
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Principle components of a SF ICP-MS
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Components of the Finnigan Element GD
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The self-sustaining DC glow discharge plasma
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GD Ion source
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Finnigan Element GD – Sample Holder
  • Flat samples


  • Sample size
    • Max. Ø 70 mm, 40 mm Height
    • Min. Ø 22 mm

  • Unloading and reloading of the sample in less than 1 minute
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Changing samples (1)
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Changing samples (2)
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Finnigan Element GD – Ion Source
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Controlled Sample Cooling
  • Peltier cooled cathode
    • Stable temperature at the sputtered sample area
    • Cooling of sample with low melting point
    • Heating of sample for outgasing e.g. pressed powders

  • Sample holder for small samples with additional cooling from rear side
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Sample surface quality
  • In a ‘normal’ GRIMM type design the sample seals the ion source vacuum i.e. the sample has to be ‘perfectly’ flat



  • Finnigan Element GD: Vacuum seal at the sample holder i.e. independent from sample flatness
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Interface to Mass Analyzer
  • Extract ions from the plasma into the mass analyzer


  • Interface at ground potential


  • Cone
    • Separation of ion source region
      (~ 1 mbar) from first analyzer chamber
      (~ 10-3 mbar)
    • Extraction of ions into mass analyzer

  • Easy access for removal or cleaning of the cone


  • Valve behind cone to maintain analyzer vacuum during sample change
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Magnetic sector
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Why high resolution ? More interference compared to ICP ! High Selectivity
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Nickel Alloys: Sn119 (HR) zoom
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Slit system - Resolution
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Slit System - Easy slit exchange
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Detection System
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Finnigan ELEMENT GD Analog/Counting
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Automatic switch to Faraday Detector
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Ion Trajectories SEM - Faraday
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Dynamic Range Finnigan ELEMENT GD
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Finnigan Element GD Detection System
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Detection System – Triple Mode (NIST 1761)
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Finnigan ELEMENT XR Cross Calibration
  • Mass independent cross calibration
    • e.g. Argon
  • Fast
    • 3 s for ACF and FCF determination
  • Reliable
    • automatic
    • user independent

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Filter Lens GD: Improved Abundance Sensitivity
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Element GD - Software
  • Optimized for the needs of  routine work
    • Effortless tuning of instrument parameters
    • Intuitive and easy creation of methods and analysis sequences
    • Real time display of spectra, time resolved data and results
    • Automatic data export to LIMS systems
    • Sequence import from LIMS (XML, ASCII)


  • Easy network data transfer as well as remote control possibilities


  • Microsoft® Windows® XP Operating System


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Sensitivity (Medium Resolution R ≥ 4000)
  • 63Cu Copper sample
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Signal Stability (Cu, 350 mL·min-1 , 850 V, 55 mA)
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Stability IBR (Cu, 350 mL·min-1 , 850 V, 55 mA)
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Accuracy (BCR Copper standard CRM 075)
  • *M. Kasik, C.Venzago, R. Dorka,
  • J. Anal. At. Spectrom. 2003 (18) 603-611
  • Average of 8 labs SD
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Reproducibility (5 Pieces of AgCu sheet)
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Speed: (Cu 5 N semi-quantitative survey analysis)
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Detection Power (Th in Copper)
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Sputter Crater – Depth profiling
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Finnigan Element GD
  • GD-MS designed for routine operation


  • High sensitivity
    > 1010 cps  (1.6-9 A) total ion current @R=4000 Cu matrix (at LR about 10x higher signal intensity)
  • Low Detection Limits (e.g. Th ~ 5 ppt in Cu)
  • Excellent Reproducibility
  • Easy to use
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Plasma Winter Conference 2005 Budapest
  • Thermo (Bremen) has launched 2 new products in Budapest:
    • ELEMENT GD
    • ELEMENT XR
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"0.2 cps to 1x1012 cps"
  • 0.2 cps to 1x1012 cps
    • complete analysis from
      ultra-trace to matrix
  • Minimum integration time:
    • counting: 0.1 ms
    • analog: 1 ms
    • Faraday: 1 ms
  • No decay time with Faraday detection system
    • Due to integration circuit
  • Automatic switching between detection modes
    • no preset
    • - < 1 ms to Faraday detection
  • Automatic cross calibration