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Published byOlivia Stafford Modified over 9 years ago
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CPAC Webinar Feb. 2009 Process Spectroscopy and Optical Sensing
Brian Marquardt Ph.D. Director – Applied Optical Sensing Lab Applied Physics Lab University of Washington Seattle, Washington 98105
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Process Raman Applications
Pharmaceuticals Food quality and safety Polymers/coatings Fermentation/biotech Cellular/tissue Oil/fuels/petrochemicals Oceanography/environment Challenges Reproducible sampling Fluorescence
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Quantitative Raman = Effective Sampling
no moving parts sapphire spherical lens constant focal length and sample volume probe is ALWAYS aligned when in contact with sample effective sampling of liquids, slurries, powders, pastes and solids high sampling precision allows it to be used effectively to monitor dynamic mixing systems (powder/slurry/particle) improved measurement precision leads to robust multivariate calibration of process Raman data CPAC developed, patented and licensed Raman ballprobe
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Analysis of a Batch Fermentation Process
Real-time Fermentation Monitoring Yeast Fermentation Process Image from Purves et al., Life: The Science of Biology, 4th Edition
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Raw Raman Data for Fermentation Batch Reaction (8 day run)
Fluorescence
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Raman Data After Fluorescence Correction Algorithm Applied
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3D Plot of fluorescence corrected Raman fermentation data
Brian Marquardt - confidential
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Raman Analysis and Optical Trapping of Single Cells
Raman Microscope and Instrument Raman Microscope and Microchip
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Micro-reactors and Raman lead to improved understanding and control
500 1000 1500 2000 2,4-dinitrotoluene 2,6-dinitrotoluene 2-nitrotoluene 3-nitrotoluene 4-nitrotoluene nitric acid sulfuric acid toluene Raman Shift (cm-1)
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Real-time Understanding and Control
without residence time module flow rate: 0.89 ml/min (residence time ~ 5 min) PCA Analysis on data after mixing: 1st PCA scores Increase in reaction yield after each temperature step
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CPAC/FDA/Corning MicroReactor
Goal: to improve reaction development and optimization through the use of continuous glass microreactors, NeSSI and analytics Funded by the FDA to demonstrate the benefits of improved reactor design, effective sampling and online analytics to increase process understanding (QbD) QbD Project began November 2008
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What is NeSSI? Industry-driven effort to define and promote a new standardized alternative to sample conditioning systems for analyzers and sensors Standard fluidic interface for modular surface- mount components Standard wiring and communications interfaces Standard platform for micro analytics
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What does NeSSI Provide
Simple “Lego-like” assembly Easy to re-configure No special tools or skills required Standardized flow components “Mix-and-match” compatibility between vendors Growing list of components Standardized electrical and comm. (Gen II) “Plug-and-play” integration of multiple devices Simplified interface for programmatic I/O and control Advanced analytics (Gen III) Micro-analyzers Integrated analysis or “smart” systems
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NeSSI Gas Generation System
Automated Circor NeSSI Gas/Vapor System N2 O2 Mixed Gases Mass Flow Controllers Fully automated gas generation system for sensor calibration: 4 Stage dilution, able to produce and maintain gas concentrations of 100% to 0.1%(1000 ppm) from standard bottle gas Fully calibrated, automated system with set and forget capability
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Small Optical Sensors vapochromic chemistry
Oxygen Moisture Ammonia Hydrogen Common Solvents Alcohols Esters Amines Chlorinated Organics Organic Hydrocarbons (BTEX) Carbon Dioxide (in development) Hydrogen Sulfide vapochromic chemistry optical response to analytes simple design reversible response low power inexpensive fast response times high quantum efficiency long term sensor stability sensitive to a variety of analytes wireless communication battery powered
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Vapochromic Humidity Sensor
- Measurment time – 100 ms - 3 reps per concentration
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Sensor response to O2 Gas
120 20 replicates at each concentration Concentration range: % Oxygen 100 R2 = 0.990, 3 PC RMSEC = 80 Predicted O2 % 60 Intensity (counts) Wavelength (nm) 100 % 0% This oxygen concentrations were calculated from the mass flow controllers 40 20 10 20 30 40 50 60 70 80 90 100 Calculated O2 %
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Low Concentration Dissolved O2 Calibration
5 replicates at each concentration Concentration range: 1 μmol/L μmol/L 39 31 R2=0.997, 2 PCs, RMSEC= 24 Predicted [O2] (μmol/L) 16 39 μmol/L 1 μmol /L Intensity (counts) Wavelength (nm) 9 5 2 1 1 μmol/L = 32.5 ppb Measured [O2] (μmol/L)
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LIBS: Remote Elemental Analysis
Remote elemental analysis with no sample preparation Fiber-optic delivery or long range delivery of laser by telescope for remote analysis Laser-induced plasma ablates and super heats samples to provide elemental spectral data
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Potential Applications
Analysis of metal complexes in food, cellulosic biomass, pharmaceuticals and fermentation apps. Determination of ionic and inorganic species in a variety of chemical/production processes Glasses, ceramics, zeolites, alloys, corrosion analysis Quantitative analysis of catalyst composition for screening and development Couple with vibrational techniques to develop a hyphenated technique (Raman/LIBS) to define both organic and inorganic analytes in a process system
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Acknowledgements CPAC Washington Tech. Center
National Science Foundation National Institute of Health, Charlie Branham and Wes Thompson Many current and past CPAC sponsors
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