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Overcoming Hydrogen-Bonding in On-line Spectroscopy of Hydrofluoric Acid

Paul G. Vahey, Honeywell

Jorge E. Perez, CIC Photonics, Inc.

PDF Version

 

Measure ppm Impurities On-line in HF

 

  • Benefits
    • Reduce - Grab Sampling, Exposure
    • Improve - Turnaround, Precision, Process Control
  • Challenges
    • Materials Compatibility
    • Unusual properties of HF
    • Could not reproduce in laboratory
    • Lab Instrument in plant environment
  • Enablers
    • Quality people at Plant, Vendors, Engineering, Lab

Experimental Conditions

 

  • Sampling
    • Anhydrous HF
    • Heat Tracing at 105°F
    • Manifold with By-Pass and N2 Purge
      • Dynamic and Stop flow capabilities
    • Safety Shut-off at several points
  • Instrumentation
    • IRGAS 100 Demo unit
    • 20 cm direct pass detection cell
      • independent heating control
    • IRGAS software

Ideal FTIR Spectrum of HF Gas

Severe Hydrogen Bonding

IRGAS Demo Instrument with Manifold

Demo Instrument, Heat Traced and Insulated

 

    Strategies for Reducing Saturation Pressure

 

  • 1. Reduce Total Pressure of Sample
    • Condensation / Heat of Expansion
    • Decrease Sensitivity
  • 2. Dilute with Inert Gas
    • Same as above
    • Not Robust for Manufacturing Process
  • 3. Increase Temperature
    • Simple
    • Maintain Sensitivity
    • Material Compatibility

Apparent Molecular Weight of HF vs. P,

Available on http://www.HFacid.com

Hydrogen Bonding Reduced by Dilution

Zoom in on Dilution

Eliminate Hydrogen Bonds by Heating

Ideal FTIR Spectrum of HF Gas

Dilution vs Heating

Compare Lab and FTIR Results for SO

    LessonsLearned for Trace Analysis in HF Lessons Learned for Trace Analysis in HF

 

  • Safety Safety Safety
    • Shut-offs, check valves, PPE
    • Alarms for Low-flow & High pressure
    • Materials Compatibility
  • Sampling
    • Heat >> Dilution for Reducing H-bonding
    • Materials Compatibility
    • Manifold improved flexibility
  • Instrumentation
    • IRGAS system is robust
    • >20 cm pathlength detection cell

    Acknowledgements

 
  • Honeywell Hydrofluoric Acid Plant
    • Bill Pepe, Dana Smith, John McCarthy, Bruce Perque
    • Jason Landry, Cheryl Smith, Jonathan Hulgan
    • Operators, I&E Technicians (Scott Guillory)
  • Honeywell Analytical Scientists
    • John Welch, Rob Bray, Ralph Borowski
  • CIC Photonics
    • Jorge Perez
    • Dick Meyer, John Derrig

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