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PROCESS ANALYTICAL RESPONSE TO THE DEMANDS OF HIGH THROUGHPUT EXPERIMENTATION

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Title: PROCESS ANALYTICAL RESPONSE TO THE DEMANDS OF HIGH THROUGHPUT EXPERIMENTATION


1
PROCESS ANALYTICAL RESPONSE TO THE DEMANDS OF
HIGH THROUGHPUT EXPERIMENTATION
  • MEL KOCH
  • CPAC
  • UNIVERSITY OF WASHINGTON

2
NEW DIRECTIONSIN INDUSTRY
? GLOBALIZATION OF BUSINESSES
? CONSOLIDATION OF INDUSTRIES ? CONSTRICTED
RESOURCES
3
THE DRIVERS
? PRODUCTIVITY ? QUALITY ? ENVIRONMENTAL
4
THE DRIVERS ALLREQUIRE RESEARCH
YET RESOURCES ARE
S H R I N K I N G
5
EFFECTIVE PARTNERINGIS NEEDED
6
PARTNERING
? WITHIN AN ORGANIZATION ? ACROSS INDUSTRY ?
INDUSTRY - UNIVERSITY (GOVERNMENT) ?
INDUSTRY - GOVERNMENT - UNIVERSITY
7
CENTER FOR PROCESS ANALYTICAL CHEMISTRY
UNIVERSITY OF WASHINGTON,
SEATTLE
8
Real-time Data Acquisition . . .
  • . . . provides researchers with a video of a
    chemical process.
  • Deliverables
  • Composition
  • Unknown Identification
  • Reaction Pathways Kinetics
  • Chemical Topography
  • Emission Monitoring
  • Process Hardware Integrity
  • Reactive Chemical Issues
  • On-line Feasibility Studies

H2 Monomer C2H6
Gas-Phase Reactor On-line MS
9
Short-term On-line Analytical Measurements ...
Catalysis RD On-line MS, GC, FTIR
  • . . . maximize the investment of capital,
    hardware, staff by. . .
  • Shortening development time,
  • Increasing productivity, and
  • Maximizes asset utilization unattended data
    collected 24 hours a day. Allows process
    parameters to be tweaked in real time to link
    cause and effect.
  • Making better decisions.
  • Evaluate methods and instrumentation for
    permanent applications before committing capital.

MS
GC
High-Flow Reactor
FTIR
10
Allows On-line Concepts to be Developed
  • Over 190 materials evaluated in 5 reactors 1st
    year.
  • Each run at
  • 12 different combinations of T P.
  • Steady-state conditions for 3-6 hours.
  • 3 days to complete typical evaluation.
  • Potential for 605 catalysts/year.
  • 12X improvement in sample throughput.

Tube Reactors in Fluidized Bed
On-line GC/MS Direct MS
11
CPAC is a Consortium of Industrial Sponsors,
National Laboratories and Government Agencies
? Established in 1984, the Objective of the
Center is to Address Challenges in Real-Time and
Continuous Process Monitoring and Control
? Provides a Forum for Multidisciplinary
Participation in Process Analytical Technology
Definition, Creation, and Utilization
12
BENEFITS OF CONSORTIA MEMBERSHIP
New Technology
Peer Communication
Students
Deliverables
13
PEER COMMUNICATION
? BENCHMARKING ? CLEARING HOUSE ? FOCUS GROUPS
14
Sponsor Focus Groups
? Oil Petrochemicals ? Chemicals Materials ?
Food Consumer Products ? Bio Tech /
Pharmaceuticals ? National Labs Agencies ?
Instrument Companies
15
CPAC Industrial Sponsors
16
CPAC Government Sponsors
  • Environmental Protection Agency
  • Los Alamos National Laboratory
  • National Institute of Standards Technology
  • Pacific Northwest National Labs
  • Sandia National Laboratory
  • Westinghouse Savannah River Co.

17
Core Research Areas
? Chemometrics ? Sensors ? Spectroscopy /
Imaging ? Chromatography ? Flow Injection
Analysis ? Process Control
18
Multidisciplinary
? Chemistry ? Chemical Engineering ? Electrical
Engineering ? Bioengineering ? Applied Physics ?
Forestry ? Mechanical Engineering ? Food Science
Engineering ? Health Sciences
19
OTHER UNIVERSITY PARTNERING
University of Minnesota University of
Arkansas University of Alberta Clarkson
University University of Delaware Texas Tech
University University of Michigan Arizona State
University University of California
Davis University of Colorado
20
INDUSTRY NEEDS
  • ? MIXING EFFICIENCY
  • ? CLEANING VALIDATION
  • ? PARTICLE SIZING
  • ? CHEMICAL COMPOSITION (molecular, spatial)
  • ? COATING CONSISTENCY
  • ? VAPOR CHARACTERIZATION
  • ? VISCOSITY / RHEOMETRICS
  • MOISTURE CONCENTRATION
  • BIOASSAY

21
CPAC STRATEGIC PLATFORMS
  • ? SURFACE AND INTERFACIAL CHARACTERIZATION AND
    CONTROL
  • MULTICOMPONENT MATERIALS CHARACTERIZATION AND
    CONTROL
  • VERSATILE MICROANALYTICAL SYSTEMS
  • ? PROCESS MONITORING, MODELING AND CONTROL

PROBLEMS
SYSTEMS
22
  •  
  • Sensors
  • Grating Light Reflection Spectroscopy
  •  
  • High Precision Reflectometer
  •  
  • Fast Versatile Microfabricated Moisture Sensors
  •  
  • Vapochromic Detection and Identification of
    Volatile Organic Compounds
  • Advanced Surface Plasmon Resonance Sensors
  •  
  • In-Situ Evaluation of Physical Sensor Health
    and Output Signal Validity
  • Dynamic Surface Tension Detector

23
Relevance ofOptical Low Coherence Reflectometry
(OLCR)
  • Q What do the following things have in common?
  • airplanes
  • pharmaceutical tablets
  • plastic food wrappers
  • beverage bottles

A
  • All of them have surface layers (i.e., films or
    coatings) that give
  • products desired properties.
  • Surface layers need to be deposited and tested
    rapidly in industrial
  • processes.
  • Industry needs fast, sensitive, reliable,
    non-contact measurement
  • methods for these processes.

24
Multiple Layer Polymer Materials
Scattering materials
Drug delivery patch
Distance in micrometers
Distance in micrometers
25
Photo of new OLCR
Power supplies
Fiber optic interferometer
Delay line for setting end face reflection
location
26
Spectroscopy/Imaging Evaluating Raman
Spectroscopy to Improve Process Monitoring and
Materials Characterization Development and
Application of On-Line Particle Analyzers
Non-destructive Measurement of Moisture
Distribution with Fringing Electric Field Sensors
Application of MRI for Analysis
of Mixing   Development of a Micro NMR
System   Ultrasonic Sensor for Viscosity and
Microstructural Measurements
27
Raman Microscope w/ Waveguide Flow Cell
spectrograph/detector
Raman microscope
laser
beam splitter
CCD
filter
microscope objective
Purge
HPLC pump
Waste
waveguide
injection valve
column
28
HPLC/Raman Analysis of Aromatic Compounds
29
Raman Immersion Ball Probe Design
Probe barrel when used with collimated
laser length is not an issue.
Probe Tip O-ring sealed and threaded to barrel
Ball sapphire ball lens (focal point is on face
of lens)
Ball Fastener threads into tip and pressure
seals ball into a fluoroelastomer seal and the
probe tip
30
Monitoring Protein in a Separation Process _at_
Cargill-Memphis
  • Raman ball probe inserted directly
  • into flowing stream
  • Analysis performed 20 meters from
  • instrument
  • Analysis performed under moderate
  • process conditions (temp. and flow)

31
Future Applications of RamanBall Probe
Proposed use of a ball probe(s) in a V-blender
fiber to probe(s)
optical interface
  • use of fibers has the potential of
  • coupling multiple probes to one blender

32
CPAC INITIATIVES
  • NEW SAMPLING AND SENSOR INITIATIVE
  • CONNECTIVITY INTIATIVE
  • INSTRUMENTATION FOR MICRO REACTORS INITIATIVE
  • FERMENTATION MONITORING AND CONTROL INITIATIVE
  • CHEMOMETRICS ON-LINE INITIATIVE
  • RAW MATERIAL QUALITY RELATED TO FINAL PRODUCT
    PROPERTIES

33
NEW RESEARCH INITIATIVE
  • INSTRUMENTATION FOR MICROREACTORS

34
THE DRIVER IS THE NEED FOR HIGH THROUGHPUT
EXPERIMENTAION
  • DISCOVERY
  • SCREENING
  • PROCESS DEVELOPMENT
  • PROCESS CONTROL

35
DISCOVERY TO COMMERCIALIZATION
DESIGN OF EXPERIMENTS
REACTOR
DATA EVALUATION
ANALYZE
36
CPAC CHEMOMETRIC RESEARCH PROJECTS
  • Chemometrics for Smart Sensors
  •  
  • Novel Classification Tools Combining Data
    Mining and Statistical Inferencing Techniques
  • New Approaches to Transfer and Maintenance of
    Multivariate Calibrations
  •  
  • Genetic Algorithms that Emulate Human Pattern
    Recognition through Machine Learning for Data
    Mining and Knowledge Discovery
  •  
  • Incorporating Raw Material Variation into
    Process Chemometric Models
  •  

37
REVOLUTIONARY ADVANCES THAT ARE AFFECTING
CHEMICAL MEASUREMENTS
  • MEASUREMENT INFORMATION PROCESSING
  • MINIATURIZATION
  • ENGINEERED MATERIALS
  • ELECTRO-OPTICS

38
Developed and Fabricated Miniature Preconcentrato
rs, Gas Chromatographic (GC) Columns and Surface
Acoustic Wave (SAW) Arrays
Preconcentrator/ Thermal Desorber
4 SAW Array
One Meter GC Column
39
Gas analysis components are integrated on novel
electrical/fluidic circuit board
Preconcentrator
40
A fully autonomous hand-held microanalyzer

Containing Multiple coated/packed GC columns
w/multiple coated SAW detectors
and Multiple LC columns with fluorescence
electrochemical detection
41

Double Focusing Mass Spectrometer University
of Minnesota Proof-of-Concept Mass range
1-200amu Resolving Power 150
Detector
Mass Analyzer
Ionizer

42
The ILD-50 Industrial Leak Detector
43
Air, He, Ar, and Carbon Dioxide CS-50
7e-9
6e-9
5e-9
4e-9
Intensity
3e-9
2e-9
1e-9
0
-1e-9
0
10
20
30
40
50
60
m/z
44
Development of a Micro NMR System
  • UCD NMR Facility
  • MicroInstruments and Systems Laboratory
  • Department of Electrical and Computer Engineering
  • Department of Biological and Agricultural
    Engineering
  • University of California, Davis

45
Initial Results
NMR spectrum of a 3 microliter water sample using
the RF microcoil shown on the right.
46
CPAC Micro-Reactor Platform Initiative-
Argonaut Technologies Quest parallel reactor
  • 10 simultaneous reactions
  • Select temperatures from
  • 40 oC to 130 oC
  • Multitude of mixing speeds
  • Amenable for spectroscopic monitoring

47
  • Microfluidics Enables Integrated Chemical and
    Cellular Analysis in a Single Disposable Fluidics
    Module

48
(No Transcript)
49
CPC SELECTO A commercially available modular
microreaction system
  • Broad applicability
  • Demanding chemistry
  • Flexible and easy to use
  • High operational safety

50
Reactor Module
51
Raman Ball Probe on Outlet of CPC System
Real-time Reaction Monitoring
52
MICRO REACTOR TOPICS
  • BATCH - PARALLEL
  • CONTINUOUS / MICRO FLUIDIC
  • ELECTROTHERMAL
  • ACOUSTICAL
  • CALIBRATION / STANDARDIZATON
  • MONITORING / CONTROL

53
CHALLENGES TO USING MICROREACTORS
  • INTERFACING MODULAR UNITS
  • SAMPLING AND SCREENING
  • ANALTYICAL CHARACTERIZATION
  • DATA HANDLING
  • PROCESS MODELING AND FEED BACK CONTROL

54
SOME RELEVANT CURRENT CPAC RESEARCH EFFORTS
  • MICRO-LC
  • SURFACE TENSION DETECTION
  • GCxGC
  • FRINGE FIELD SENSORS
  • VAPOCHROMIC SENSORS
  • RAMAN
  • GRATED LIGHT REFLECTIVE SPECTROSCOPY
  • REFLECTOMETRY
  • FLOW-THROUGH PARTICLE ANALYZER
  • SURFACE PLASMON RESONANCE
  • MINI-MASS SPECTROMETER
  • DATA HANDLING

55
ADVANCES IN SENSORS AND CONTROLSHIGHLIGHT THE
NEED FOR IMPROVED SAMPLING AND DATA HANDLING
TECHNOLOGIES
56
SAMPLING
  • ? Most systems today are unique
  • But they could be Modularized
  • Smart Systems are Needed
  • NeSSI has appeared

57
Response to CPAC RFPsSwagelok
  • Complies with SP76
  • Metallic C seal design now
  • Elastomer seals later
  • 3 channels
  • 1.5 blocks downmounts
  • Lego? like assembly
  • IGC II technology
  • highly engineered
  • Investigating flow X-proofing solutions

Courtesy of Swagelok
58
Response to CPAC RFPsAutoflow
  • Fully compliant with SP76
  • TFE loaded elastomer seals
  • 3 channels
  • 1.5 blocks
  • Division 1 cartridge heating
  • Div. 2 thermal flow meter, flow switches
  • Utilizing current electrical X-proofing concepts

Courtesy of Autoflow
59
Response to CPAC RFPs Rosemount-Swagelok
  • Field mounted chromatograph with a
    miniature/modular sample system

Courtesy of Rosemount Swagelok
60
NeSSI with Analyzer on board and Wireless
SensorManager(I/OController)
61
CPAC FermentationInitiative
  • Goal to improve process control of fermentation
    processes through the use of both commercial and
    newly developed analytical tools

62
FERMENTATION CONTROL INITIATIVE
  • Set up a test bed that is maintained and operated
    by visiting scientists
  • Form a steering team from the 20 interested
    member organizations
  • Communicate project planning and results via
    sponsors only section of web site

63
SOME RELEVANT CURRENT CPAC RESEARCH EFFORTS
MICRO-LC DYNAMIC SURFACE TENSION GCxGC LAB-ON-A-VA
LVE FRINGE FIELD SENSORS VAPOCHROMIC
SENSORS RAMAN GLRS REFLECTOMETRY SPR MINI-MS DATA
HANDLING
64
CPAC Sponsor Support
Kaiser Optical Systems Kraft Foods Los Alamos
Natl Lab Merck Pharma. Novozymes Pharmacia
Procter and Gamble Rosemount Analytical Sandia
Natl Lab Swagelok
Agilent Amgen Aventis Pharma. Baxter
Bristol-Myers Squibb Cargill Dow Chemical DuPont
Genentech Honeywell
65
CENTERS ENHANCEACADEMIC PROGRAMS
? MULTIDISCIPLINARY ? SHOWCASE EMERGING
TECHNOLOGIES ? PROVIDE PRACTICAL FOCUS ? COMPETE
WELL FOR SCARCE RESOURCES
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