Vision of Micro- Analytics on NeSSI

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1 Applied Physics Laboratory / Center for Process Analytical Chemistry University of Washington Seattle, WA Vision of Micro- Analytics on NeSSI Brian Marquardt Charles Branham, Lauren Hughs

2 Analytical Sampling for Online Applications

3 Why Use Process Sensors? Real-time analysis for.. Corrosion Monitoring Process development Process optimization Process control Production?

4 Process Challenges Analytical characterization Sampling and screening Data handling Sensor fusing Multi-sensor modeling Process modeling and feed back control Process optimization move toward feed forward control????

5 Spectroscopic Analysis of a Process Possible problems with performing online spectroscopic measurements Bubble formation in sample lines due to pressure drop sample degassing Phase change between reactor and analyzer due to temperature or pressure change Most PAT problems are due to sampling not measurement device Need better systems to sample processes

6 Benefits of Being NeSSI Your condition space is constrained Volumes, flow rates, pressures, and viscosities inherently bounded by architecture Your interfaces are defined Electrical power, communication, and sample are all available in a standard way Power budget could be main driver to miniaturize Your sample conditioning can be defined and controlled Specify up-stream and down-stream NeSSI components (and verify) All this means your analytical can be more directed and focused

7 Where Does NeSSI Fit in the Lab Instrument/Sensor Interfaces Design standards make development simpler Reduced toolset to be mastered Reduced sample variability to account for Calibration/validation built-in Consistent physical environment for measurement Stream switching and/or mixing allow generation of standards to match analytical requirements Reaction monitoring Microreactors and continuous flow reactors Batch reactors (with fast loop) Sample Preparation Gas handling (mixing, generation, delivery) Liquid handling (mixing, dilution, conditioning, etc.)

Actuator V Standard hockey-puckpc Standard Mechanical Interface Rail

8 NeSSI : Enabler for MicroAnalytical (the rail concept) Standard connectivity Standard Electrical (Digital) Interface Rail SAM* Anyone s Sensor P Anyone s Actuator V Standard hockey-puckpc Standard Mechanical Interface Rail *Sensor/Actuator Manager What technologies are available Suitability for modular sampling systems

9 C2V Fast Micro-GC as well as

10 Calidus GC from Falcon Analytical

11 At-Line GC s with NeSSI Compatibility ABB Natural GC Agilent 3000 Micro GC Siemens microsam

12 Applied Analytics Inc. Diode Array OMA-300 A Fiber-optics-diodearray process analyzer For on-line concentration monitoring

13 Small Diameter ATR-IR-Fiber Probes Fiber Photonics Inc. Diamond ATR-IR-Fiber Probe of 2.7mm diameter in NeSSI

14 microptix

models for CO, H 2 S, wet CL 2 4 20mA, RS422 or RS232 serial connectivity Stable results On site verification and calibration

15 H 2 Scan Adaptation to NeSSI TM Platform Hydrogen specific: 0.5% H2 to 100% H2 v/v Response time (T90) < 30 sec In line, real time measurements in process gas streams up to 100 O C Unique models for CO, H 2 S, wet CL mA, RS422 or RS232 serial connectivity Stable results On site verification and calibration Approved for hazardous locations Intrinsically safe design ATEX certificate granted; UL pending Cost effective to buy / install / maintain Field verification and calibration kit available

16 Astute Sampling System Sampling + Sensors & micro-analyzers GAS TREATMENT COLUMN Astute System with C 2 V Micro GC and H 2 Scan hydrogen analyzer Process

17 Exploded View Agilent NeSSI Dielectric Sensor Cable to Agilent Network Analyzer Dielectric Probe Inner Body Close up of Coaxial Probe Tip O-ring (inside) Swagelok 2-Port Valve Base Outer Body

18 NeSSI IR Gas Cell

FNL-120 UV-Visible ATR Cell In Development Raman Cells (Single- and

19 NeSSI Compatible Optical Cells Axiom Analytical, Inc. Currently Available FFV Series Transmission Cells (Near-IR, UV-Visible) FNL-120 UV-Visible ATR Cell In Development Raman Cells (Single- and Multi-pass) Possible Development Diffuse Reflectance Cells Mid-IR ATR Cells Courtesy of Mike Doyle Axiom Analytical, Inc.

20 Chevron NeSSI/Analytical Unit Specifications ASI Microfast GC Parker NeSSI gas handling/sampling system Carrier gas Mobility

21 NeSSI based Analytical Developments at CPAC

22 NeSSI Gas/ Vapor System ASI microfast GC Aspectrics EPIR w/ glass cell Permeation Tower N 2 Waste NeSSI Gas/Vapor System NeSSI Flow Cell

23 NeSSI Calib. Gas Generation System Features of NeSSI System : Fully digital 4 Stage dilution, able to produce and maintain gas concentrations in ppb range Fully automated system, set and forget capability Integrated C2V NeSSI compat. GC Calib, platform for gas sensor dev.

24 Gas Calib. System LabView Control Program Perform automated DoE calibration runs input and log sensor, reference, temperature and pressure feeds System designed for full digital (plug and play) performance as h/w matures

variety of analytes wireless communication battery powered Oxygen Moisture Ammonia Hydrogen Common Solvents Alcohols

25 Design of Small Fiber Optic Sensors vapochromic chemistry optical response to analyte 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 Oxygen Moisture Ammonia Hydrogen Common Solvents Alcohols Esters Amines Chlorinated Organics Organic Hydrocarbons (BTEX) Carbon Dioxide (in development) Hydrogen Sulfide (in development)

Fiber optic ferrule with plastic housing Close up of

26 Modular NeSSI Oxygen Gas Sensor 1/16 in bifurcated fiber optic fiber 1/16 to 1/8 in Swagelok union Sensor Body Fiber optic ferrule with plastic housing Close up of Outer Body Tip Vapochromic Tip Exploded View Agilent NeSSI Mount

27 Vapochromic Humidity Sensor Predicted Y Elements: 6 Slope: Offset: Correlation: RMSEC: SEC: Bias: e-06 - Measurment time 100 ms - 3 reps per concentration per70.mas per80.mas per50.mas 20 0 per10.mas per20.mas per30.mas 2 PC calibration model humidity range: 10 80% Ohmic feedback control humidity generator used for reference stds. Measured Y humid meas, (Y-var, (humid PC): meas,2)

28 Vapochromic Benzene Sensor Full spectrum response of the 0%, 10%, and 50% bubbler flow samples used to make the PLS model showing both the change in intensity and shift in peak maximum with changing benzene concentration.

29 Sensor response to O 2 Predicted O 2 % replicates at each concentration Concentration range: 0-100% Oxygen R 2 = 0.990, 3 PC RMSEC = Intensity (counts) 0% 100 % Calculated O 2 % 60 Wavelength (nm)

30 Liquid Chromatography for NeSSI Scott Gilbert, CPAC Visiting Scholar Crystal Vision Microsystems LLC Atofluidic Technologies, LLC Split flow approach to sampling Liters per minute microliters per minute sample in diluent in nanoliters per minute μ-fluidic LC Chip for On-line Sample Pretreatment Pulsed electrochemical detection (on-chip) micromixer column mobile phase in

31 Analytics and Sampling the Fastest Route to QBD? Brian Marquardt Wes Thompson Applied Physics Laboratory University of Washington U.S. Food and Drug Administration MEPI

32 CPAC/FDA/Corning AF Reactor Goal: to improve reaction development and optimization through the use of continuous glass flow reactors, 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) Partners: FDA, Corning, CPAC, Kaiser, Parker QbD Project began November 2008 Process Reactions June 2009

33 AF Reactor and Raman Analyzer 4 channel, 785 nm Kaiser Optical Systems Rxn2 probes placed at different reactor zones

34 Chloroformate Chemistry Organic Acid Chloride Organic Carbonate + dimer O O OH pyridine Cl + O HO toluène O O OH + N.HCl 2-ethylhexyl chloroformate butane-1,2-diol 2-ethylhexyl 2-hydroxybutyl carbonate OH O Cl + O O O O O O O O O O 2-ethylhexyl chloroformate 2-ethylhexyl 2-hydroxybutyl carbonate dimmer dimer Carbonate and dimer formation

Raman Analysis of AF Reactor 1 2 3 4 monitor

35 Raman Analysis of AF Reactor monitor reaction with 4 channel 785 nm Raman system NeSSI sampling systems (1-4) equipped with Raman ballprobes Online GC also used as post quench online analyzer (4)

36 NeSSI Ballprobe - Raman/NIR/UV Matrix Solutions:

37 Advanced Flow Reactor Images Raman Probes

38 NeSSI Sampling and Raman Probe Images

39 3D Plot of Raman Rxn Data GC Results (%) Test R-OH 2EHCF R-Cl Carbonate Dimer Ch. 1 Toluene Chloroformate Toluene

40 Reaction Profiles for 2 DoE Steps GC Results (%) Test R-OH 2EHCF R-Cl Carbonate Dimer Carbonate ---- Chloroformate Test 3 Test 0

Current Status Data collected and organized 14 days in Toulouse France Analysis and Modeling Evaluation of various modeling protocols PCA, MCR, ALS Calibrate to GC results

41 Current Status Data collected and organized 14 days in Toulouse France Analysis and Modeling Evaluation of various modeling protocols PCA, MCR, ALS Calibrate to GC results (PLS) Evaluate different chemistry for Phase 2 More chemical change in reaction space Implement more sensors Acquire reactor at CPAC Implement Models for Process Feedback Control

42 Thanks U.S. Food and Drug Administration Moheb Nasr Christine Moore David Morley Erik Henrikson Corning Glass Philipe Caze Celine Guermeur Jérémy Jorda Parker Mike Cost Kaiser Optical Systems Ian Lewis Hervé Lucas Bruno Lenain CPAC University of Washington Applied Physics Lab U.S. Food and Drug Administration La Maison Européenne des Procédés Innovants (MEPI ) Annelyse Conté MEPI

Coupling a Continuous Flow Reactor System to a Platform for Improved Process Development and Optimization - An Approach to Defining FDA's QbD

Coupling a Continuous Flow Reactor System to a Platform for Improved Process Development and Optimization - An Approach to Defining FDA's QbD Brian Marquardt, Wesley Thompson, Michael Roberto, Charles