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Ce icp-ms

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  • 1. Hyphenated Technique of Capillary Electrophoresis and Inductively Coupled Plasma Mass spectrometry Jesús Anzano University of Zaragoza– Department of Analytical Chemistry Zaragoza
  • 2.
    • Introduction:
    • a. Elemental Speciation
    • b. Capillary Electrophoresis (CE)
    • c. Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
    • CE-ICP-MS Hyphenated System
    • a. CE-ICP-MS Instrument Setup
    • b. Interface and Modified Nebulizer Design
    • c. Direct Injection Interface design
    • d. Pulsed Field Capillary Electrophoresis
    • e. Laminar Flow Effect
    • Elemental Speciation Analysis application
    • a. Chemical forms of As and Cr in preservative wood
    • b. Leaching effect of As and Cr in surround soil
    • Preliminary Results
    Outline
  • 3. Elemental Speciation
    • Elemental Speciation is the identification and quantification of the chemical form of an element.
    • The toxicological, physiological and biological effects are species dependent.
    • Main area :
    • ---Environmental area
    • ---Food area
    • ---Health area
  • 4. Capillary Electrophoresis (CE)
    • Separate mixture of ionic species quickly
    • Good resolution and separation efficiency
    • Simple instrument set-up
    • Relative low cost
    • Require much less sample
  • 5. Inductively Coupled Plasma Mass spectrometry (ICP-MS)
    • Direct element information and quantification
    • Species identification via migration time
    • Low detection limit
    • High sensitivity and selectively
  • 6. CE-ICP-MS Instrument Setup Quadrupole Mass Analyzer Detector Computer ICP Interface UV Detector Buffer / Sample Make-up Solution Capillary CE HV Power Supply
  • 7. The CE-ICP-MS Interface Requirements: An electrical connection to the end of CE capillary High aerosol transport efficiency Low dead volume ICP Nebulizer Flow From CE Capillary CE Platinum Ground Electrode Make-up Sheath Flow O-ring
  • 8. The Modified Concentric Nebulizer Nebulizer Gas In CE Capillary Stainless Steel Tube To Spray Chamber CE Capillary Stainless Steel Tube Nebulizer Inner Tube
  • 9. The Concentric Nebulizer and Interface
    • Advantages:
    • - Universally applicable
    • - Easy to install and remove
    • - Inexpensive
    • Disadvantages:
    • - Sample solution from CE is diluted and causes losses in sensitivity.
    • - Increase sample solution flow rate may decrease CE resolution.
    • - Decrease make-up sheath flow rate may decrease ICP-MS aerosol transfer efficiency
  • 10. The Direct Injection Interface Nebulizer Gas Platinum Electrode CE Capillary Nebulizer Body ICP Torch Sampler Cone
  • 11. The Direct Injection Interface
    • Advantages:
    • - Improve precision.
    • - Reduce rinse-out time.
    • - Low absolute detection limit.
    • - Reduce peak broadening due to the low dead volume.
    • Disadvantages:
    • - ICP-MS plasma may be extinguished.
    • - High cost.
    • - Difficult to use.
  • 12. Pulsed Field CE-ICP-MS Instrument Setup V A Sample or Buffer UV Detector Current Voltage Probe Pulse Power Supply Capillary Interface Nebulizer To ICP Capillary with Silver Paint + G
  • 13. Pulsed Field CE-ICP-MS Comparison of power consideration for a continuous versus pulsed CE Continuous  s or ms, Pulsed DC 20kV, 40  A 0.8W Dc: 5kV, 10  A (0.05W) Pulse: 100kV, 0.2mA, 100  s, 200Hz (20W) Average: 0.45W t 1 t 2 Pulse DC
  • 14. Pulsed Field CE-ICP-MS
    • Theoretical plate number N=L 2 /  L 2 =(  ep +  eo )V/2D (1)
    • Resolution R s = N 1/2 (  v /  ) /4 (2)
    • Plate Height H heating =(  2 S 2  2 /  2 D)((K 1 E 5 r c 6 /  app )
    • + (K 2 E 6 r c 6 /LD)) (3)
    • Where V is the applied voltage, E is the electric field strength.
    • 1. Kennedy, R. T.; German, I.; Thompson, J. E.; Witowski, S. R. Chem. Rev . 1999 , 99, 3081-3131.
    The effect of Joule heating on band broadening
  • 15. Pulsed Field CE-ICP-MS
    • Advantages:
    • - Reduce the Joule heating which causes band broadening in conventional CE.
    • - Large diameter capillary can be used to attain high flow rate.
    • - The interface is simpler and high sensitivity without dilution of the analyte.
    • Disadvantages:
    • - High cost.
  • 16. Laminar Flow Effect in CE-ICP-MS Cross-Sectional Flow Profile Due to Electroosmotic Flow Cross-Sectional Flow Profile Due to Laminar Flow
  • 17. Elemental Speciation Analysis Application
    • Major consideration:
    • The toxicity of copper (Cu), chromium (Cr) and arsenic (As) is dependent on elemental species.
    • Preservative wood and soil sample Preparation.
    • The state of As and Cr on treated wood.
    • The effect of pH on leaching of As and Cr.
    • As and Cr leach from the treated wood into soil .
    The most widely used wood preservative is chromated copper arsenate (CCA)
  • 18. Preliminary Result The concentric nebulizer and interface
  • 19. The Configuration of Nebulizer Tip Design 1 Design 2 Design 3 Design 4 CE liquid flow Make-up buffer Torr seal
  • 20. Modified Nebulizer Gas Flow Rate Effect
  • 21. 0.0E+00 5.0E+05 1.0E+06 1.5E+06 2.0E+06 2.5E+06 3.0E+06 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 Make-up sheath flow rate (mL/min) 1ppm In signal (acps)/solution flow rate (mL/min) Make-up Sheath Flow Rate Effect