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Application of Sampling Systems To Microreactors

Application of Sampling Systems To Microreactors. Brian J. Marquardt Dave Veltkamp CPAC. Benefits of Sampling Systems to Reaction Analysis. Conditioning and manipulation of sample introduced to analyzer Better control of sample physical parameters Phase Temperature Velocity

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Application of Sampling Systems To Microreactors

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  1. Application of Sampling Systems To Microreactors Brian J. Marquardt Dave Veltkamp CPAC

  2. Benefits of Sampling Systems to Reaction Analysis • Conditioning and manipulation of sample introduced to analyzer • Better control of sample physical parameters • Phase • Temperature • Velocity • Ability to implement sensors at points where measurement parameters are optimal • Fast switching of streams for measurement, calibration or validation

  3. Online Monitoring of a Continuous Microreactor

  4. Benefits of Raman Analysis • Little or no sample preparation is required • Water is a weak scatterer - no special accessories are needed for measuring aqueous solutions • Water and CO2 vapors are very weak scatterers - purging is unnecessary • Inexpensive glass sample holders, non-invasive probes and immersion probes are ideal in most cases • Fiber optics (up to 100's of meters in length) can be used for remote analyses • Since fundamental modes are measured, Raman bands can be easily related to chemical structure (very good for fingerprinting) • Raman spectra are "cleaner" than mid-IR spectra - Raman bands are narrower, and overtone and combination bands are generally weak • The standard spectral range reaches well below 400 cm-1, making the technique ideal for both organic and inorganic species • Raman spectroscopy can be used to measure bands of symmetric linkages which are weak in an infrared spectrum (e.g. -S-S-, -C-S-, -C=C-)

  5. Current Sensor Integration Online Raman Probe Continuous Microreactor Sample Flow Cell

  6. toluene 4500 Nitro compounds 4000 3500 3000 2-nitrotoluene Intensity 2500 2000 4-nitrotoluene 1500 1000 500 400 600 800 1000 1200 1400 1600 Raman Shift (cm-1) Nitration of Toluene Data

  7. 4 Factor 1 Scores, Reaction Kinetics x 10 1 22 23 19 26 20 28 31 17 27 18 29 30 21 14 products 16 15 0.5 0 reaction Score Values 24 11 12 -0.5 25 13 10 • air bubbles in sample line • two phase system 9 -1 4 5 6 8 3 2 7 1 reactants -1.5 0 5 10 15 20 25 30 35 Sample Number Formation of Nitrotoluene(s)

  8. Benefits of NESSI System for Microreaction Monitoring • Control sample stream temperature, pressure and flow to sensor • Ability to insert probe at optimal sensing point • Flexibility for performing calibration online without removing sensor • Generate real-time calibration and validation samples

  9. Raman Sensor Module

  10. NESSI Microreactor Sampling/Calibration System Reactor Feed 1 Product Stream Reactor Feed 2 waste prod Raman Probe

  11. Summary • NESSI allows for increased control of sample stream at analyzer interface • Typical pressure and flow are compatible with our microreactor • NESSI enables flexibility in calibration, validation, sampling and sensor location • NESSI may actually take the place of the reactor itself in the future

  12. Acknowledgments • Swagelok • Dave Simko • Rick Ales • John Warowski • Parker/Hannifin • Steve Doe • Larry Ricker – UW Chem. E. • Sylvie Theas – UW Chem. E.

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