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Hyphenated Technique of Capillary Electrophoresis and Inductively Coupled Plasma Mass spectrometry Jesús Anzano University of Zaragoza– Department of Analytical Chemistry Zaragoza
[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],Outline
Elemental Speciation ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Capillary Electrophoresis (CE) ,[object Object],[object Object],[object Object],[object Object],[object Object]
Inductively Coupled Plasma Mass spectrometry (ICP-MS) ,[object Object],[object Object],[object Object],[object Object]
CE-ICP-MS Instrument Setup Quadrupole Mass Analyzer Detector Computer ICP Interface UV Detector Buffer / Sample Make-up Solution Capillary CE HV Power  Supply
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
The Modified Concentric Nebulizer Nebulizer Gas In CE Capillary Stainless Steel  Tube   To Spray Chamber CE Capillary Stainless Steel  Tube Nebulizer Inner  Tube
The   Concentric Nebulizer and Interface ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
The Direct Injection Interface Nebulizer Gas Platinum Electrode CE Capillary Nebulizer Body ICP Torch Sampler Cone
The Direct Injection Interface ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
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
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
Pulsed Field CE-ICP-MS ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],The effect of Joule heating on band broadening
Pulsed Field CE-ICP-MS ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Laminar Flow Effect in CE-ICP-MS Cross-Sectional Flow Profile Due to Electroosmotic Flow Cross-Sectional Flow Profile Due to Laminar Flow
Elemental Speciation Analysis Application ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],The most widely used wood preservative is chromated copper arsenate (CCA)
Preliminary Result The concentric nebulizer and interface
The Configuration of Nebulizer Tip Design 1 Design 2 Design 3 Design 4 CE liquid flow Make-up buffer Torr seal
Modified Nebulizer Gas Flow Rate Effect
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

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Ce icp-ms

  • 1. Hyphenated Technique of Capillary Electrophoresis and Inductively Coupled Plasma Mass spectrometry Jesús Anzano University of Zaragoza– Department of Analytical Chemistry Zaragoza
  • 2.
  • 3.
  • 4.
  • 5.
  • 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.
  • 10. The Direct Injection Interface Nebulizer Gas Platinum Electrode CE Capillary Nebulizer Body ICP Torch Sampler Cone
  • 11.
  • 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.
  • 15.
  • 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.
  • 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