PAT Session PAT Session
Paul OPaul O’’ Connell Connell BSc.EngBSc.Eng. MIEI. MIEIJ.M.Canty InternationalJ.M.Canty InternationalBuffalo NY / Dublin Ireland Buffalo NY / Dublin Ireland
IMAGE ANALYSIS SYSTEM
Lab and online ImagingLab and online Imaging
nn Lab Microscopy is a typical Lab Microscopy is a typical segment of online imagingsegment of online imaging
nn Static not Dynamic imagingStatic not Dynamic imagingnn Imaging is 2D (or 3 Imaging is 2D (or 3
Dimensional)Dimensional)nn Size range .7 micron through Size range .7 micron through
millimeter range and largermillimeter range and largernn Correlates to other Analytical Correlates to other Analytical
MethodsMethods
Standards for Dynamic Standards for Dynamic Image AnalysisImage Analysisnn ASTM E29.02 (draft particle sizingASTM E29.02 (draft particle sizingnn ASTM E55 PATASTM E55 PATnn ISO/DIS 13322ISO/DIS 13322--2 (DISC particle sizing)2 (DISC particle sizing)nn NIST ref materialNIST ref materialnn NIST ref grids (reticule)NIST ref grids (reticule)nn ASME BPE (manufacturing standard)ASME BPE (manufacturing standard)
Examples of other methodsExamples of other methodsParticle Particle
nn Sieve matches within 1 % to a particle Sieve matches within 1 % to a particle sieve set (sieves vary by 3% in sieve set (sieves vary by 3% in themselves) ASTM E29themselves) ASTM E29
nn Laser 1 Dimensional (equivalent Laser 1 Dimensional (equivalent sphere) and not recommended for sphere) and not recommended for large aspect ratio. Tend not to large aspect ratio. Tend not to correlate to each other or when correlate to each other or when suspension fluid changesuspension fluid change
Many laser manufacturers are adding vision measurement to product lineNo plan to add laser measurement capability
No color measurementDirect measure of Particle color
Only ‘characteristic diameter’ -- a one dimensional measurement provided
Able to thin measurement data using:•Minimum particle size•Maximum particle size•Particle aspect ratio
Only ‘characteristic diameter’ -- a one dimensional measurement provided
Direct measure of Major axis and Minor axis –a two dimensional measurement
No Perimeter measurement, only ‘characteristic diameter’ -- a one dimensional measurement provided
Direct measure of Particle Perimeter – a two dimensional measurement
No Area measurement, only ‘characteristic diameter’ -- a one dimensional measurement provided
Direct measure of Particle Area – a two dimensional measurement
No visual verification at any timeVisual verification both of set-up and measurement run, allows particle shape to be identified
Laser FeaturesImage Based Features
Typical Data from Image Processing SystemTypical Data from Image Processing System
Ultimate Goal: Lab = PATUltimate Goal: Lab = PAT
nn Make sure both methods are identical Make sure both methods are identical not similarnot similar
nn Ideal system will have:Ideal system will have:–– Same data Same data –– Same SensorSame Sensor–– Same Optics Same Optics
PAT Failures/LimitationsPAT Failures/LimitationsGeneral Difficulties of integrating Lab to OnlineGeneral Difficulties of integrating Lab to Online
nn Lab is light dutyLab is light duty……not not explosion proofexplosion proof
nn Sample PreparationSample Preparationnn Dilute sampleDilute samplenn Sample locationSample locationnn Sample size limitedSample size limitednn Sample is Sample is ““cutcut”” downdown
nn Adapting Lab unit Online Adapting Lab unit Online normally requires normally requires purgingpurging……this creates a cold this creates a cold end which builds upend which builds up
nn Not designed for Full Not designed for Full ConcentrationConcentration
nn Online not at Ideal sample Online not at Ideal sample pointpoint
nn Limited by sizeLimited by sizenn Limited by locationLimited by location
Pilot testPilot test……testtest……testtest
nn There is no substitution for good pilot There is no substitution for good pilot testing at temperature ,pressure and testing at temperature ,pressure and flow to duplicate production conditionsflow to duplicate production conditions
nn An Ideal Image Processing System An Ideal Image Processing System should integrate to all process should integrate to all process conditionsconditions
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM --ConceptsConcepts--
nn Visual Receiver: Human Eye or Imaging CameraVisual Receiver: Human Eye or Imaging Camerann Lighting (Key Component)Lighting (Key Component)nn Digitizing ImageDigitizing Imagenn Image FiltersImage Filtersnn 2D True Size and Shape Analysis2D True Size and Shape Analysisnn Output Signal / Data StorageOutput Signal / Data Storage
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM Particle Sizing and ShapeParticle Sizing and Shapenn Human EyeHuman Eye--Live viewLive viewnn Recorded Digitizing Recorded Digitizing
ImageImagenn 2D True Size and 2D True Size and
Shape AnalysisShape Analysisnn Variable outputs for Variable outputs for
control specific to control specific to applicationapplication
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM -- System OverviewSystem Overview
nn Light sourceLight sourcenn Viewing windowViewing windownn Acquiring Image (camera)Acquiring Image (camera)nn Image processor (computer)Image processor (computer)nn Image analysis (software)Image analysis (software)nn OutputsOutputs
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM Ideal Light Source and Ideal Light Source and SightglassSightglass
nn Key Component of Particle Size SystemKey Component of Particle Size Systemnn No External Heat introduced to the ProcessNo External Heat introduced to the Process
–– Fiber Optic TransmissionFiber Optic Transmission–– IR FILTEREDIR FILTERED–– NO NO ““BakeBake--onon””
nn ATEX / EXPATEX / EXPnn LED LED –– Good for some applicationsGood for some applicationsnn Strobe Strobe –– Difficult to Integrate onlineDifficult to Integrate online
nn Advantage of Fused Advantage of Fused SightglassSightglass–– High PressureHigh Pressure–– High TemperateHigh Temperate–– Proven ReliabilityProven Reliability–– NoNo Recess/ Cavity/ FoulingRecess/ Cavity/ Fouling–– Can Be Welded for Sanitary unitCan Be Welded for Sanitary unit
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM -- CrystallisationCrystallisation Reactor MicroscopeReactor Microscope
nn Colour or Black & WhiteColour or Black & Whitenn Fused Glass Fused Glass nn Back or Front LightingBack or Front Lightingnn Adjustable Flow gapAdjustable Flow gapnn EXP/FP or Weather ProofEXP/FP or Weather Proofnn Microscopic Zoom Lens System Microscopic Zoom Lens System
to view 1 micronto view 1 micronnn Ideally Single Nozzle ConnectionIdeally Single Nozzle Connection
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM Solids Particle SizingSolids Particle Sizing
nn AgglomerationsAgglomerationsnn ClassifiersClassifiersnn ScreeningScreeningnn CrushingCrushingnn Grinding / MillingGrinding / Milling
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM --ProcessorProcessor
nn Analog Camera inputAnalog Camera inputnn Ethernet Camera inputEthernet Camera inputnn Windows/Linux Windows/Linux ……nn Industrial ChassisIndustrial Chassisnn Multiple InputsMultiple Inputsnn Multiple OutputsMultiple Outputsnn 44--20mA / OPC/ Other20mA / OPC/ Other
IMAGE IMAGE ANALYSISANALYSIS SYSTEM SYSTEM Software Analysis of ImagesSoftware Analysis of Images
nn Camera presents image to computer up to 25 images/secCamera presents image to computer up to 25 images/secnn Shutter/Exposure time up to 1/100,000sec for fast moving particlShutter/Exposure time up to 1/100,000sec for fast moving particles.es.nn Typical image size from PAL (768 x 576) to Typical image size from PAL (768 x 576) to MegapixelMegapixel (1600 x 1200)(1600 x 1200)nn Software analyses each pixel of image for information using ColoSoftware analyses each pixel of image for information using Colour ur
standards (LAB, RGB, YUV, ETC)standards (LAB, RGB, YUV, ETC)nn Images and Particles processed using standard AlgorithmsImages and Particles processed using standard Algorithms
IMAGE IMAGE ANALYSISANALYSIS SYSTEM SYSTEM -- AnalysisAnalysis
nn Particle Presentation is Particle Presentation is the key Online and the key Online and LABLAB
nn Visual Verification in Visual Verification in the softwarethe software
nn Outputs:Outputs:–– Graphical Graphical –– OPC OPC –– 44--20mA 20mA
Typical Image: Typical Image: ColourColour CrystalsCrystals
Typical image: SeedingTypical image: Seeding
Typical Image: Intermediate CrystalsTypical Image: Intermediate Crystals
Typical Image: Needle CrystalsTypical Image: Needle CrystalsNote: Large Aspect ratioNote: Large Aspect ratio
Typical Image: Spherical ParticlesTypical Image: Spherical Particles
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM -- Image Processing CalibrationImage Processing Calibration
n Still Image of Calibration scalen System Calibrated by use of reticule grid standardn Line drawnn Length enteredn Micron/Pixel calculated automatically
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM -- Image Processing GrabImage Processing Grab
n Image of particle taken.n Sharp image of Small fast moving particlesn Frame rate: 25 frames per secondn Shutter speed: up to 1/100,000second
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM -- Calculating SizeCalculating Size
n Image Digitisedn Standard Threshold Algorithm usedn Practical Data Acquired
—Particle Area—Perimeter—Length—Width—Colour—Particle Count—Shape
n Data can be outputted to file and spreadsheets
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM -- Output Data/Process ControlOutput Data/Process Controlnn DisplaysDisplays
–– GraphsGraphs–– Bin AnalysisBin Analysis–– TablesTables
nn Output SignalsOutput Signals–– 44--20mA20mA–– DigitalDigital
nn ……ETHERNETETHERNET
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM -- Output Data: Excel GraphsOutput Data: Excel Graphsnn Sample of possible Graphs:Sample of possible Graphs:nn Volume calculated using LengthVolume calculated using Length--
Width dimensions and Cylinder Width dimensions and Cylinder model.model.
nn Various shape models possible Various shape models possible (Sphere, Cube etc)(Sphere, Cube etc)
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM -- Visual VerificationVisual Verification
nn Key AdvantageKey Advantage–– Operators View Process Operators View Process
in Real Timein Real Time–– Suspect data can be Suspect data can be
verified by viewing verified by viewing imagesimages
nn R & DR & D–– Recording FilesRecording Files
(AVI & MPEG4)(AVI & MPEG4)–– Images (BMP)Images (BMP)–– Data (.TXT .CSV .XLS)Data (.TXT .CSV .XLS)–– All data has File name All data has File name
and time stampand time stamp
Practical Uses:Practical Uses:
CrystallizationCrystallizationnn Imaging online and pilot units allow detection and Imaging online and pilot units allow detection and
monitoring of seed pointmonitoring of seed pointnn Polymorph control via size, shape and colorPolymorph control via size, shape and colornn Nucleation can be viewed and measured down to 1 Nucleation can be viewed and measured down to 1
micronmicronnn Size and count is output Size and count is output nn Count monitors for Fines and AgglomerationsCount monitors for Fines and Agglomerationsnn Size distribution and % solids continually through Size distribution and % solids continually through
crystallizationcrystallizationnn ONLINE VIEWONLINE VIEW…… You can make sense of the dataYou can make sense of the data
Practical Uses:Practical Uses:
Monitoring of seed pointMonitoring of seed point
nn You can view down to .7 micron with You can view down to .7 micron with front or back lightingfront or back lighting
nn Software can detect and count number Software can detect and count number of particles (particle image density)of particles (particle image density)
nn Particle Shape is can help to detect:Particle Shape is can help to detect:–– polymorphs (everything is not a sphere)polymorphs (everything is not a sphere)–– AgglomerationsAgglomerations–– FinesFines
Practical Uses:Practical Uses:
Solid Particle AnalysisSolid Particle Analysisnn AgglomerationsAgglomerationsnn ClassifiersClassifiersnn ScreeningScreeningnn CrushingCrushingnn Grinding / MillingGrinding / Milling
Practical Uses:Practical Uses:
Particle ColorParticle Color
nn Particle Color data along with size and Particle Color data along with size and shape data is used to monitor shape data is used to monitor sensitive dryingsensitive drying
nn Allows research into coating in fluid Allows research into coating in fluid beds and tablet coatingbeds and tablet coating
nn Contamination in Bioreactors Contamination in Bioreactors /fermentation/fermentation
IMAGE ANALYSIS SYSTEM IMAGE ANALYSIS SYSTEM --OnOn--Line MeasurementLine Measurement
nn Reduce Lab SamplesReduce Lab Samplesnn Repeatable/AccurateRepeatable/Accuratenn Improve QualityImprove Qualitynn Response TimeResponse Time
PaybackPayback
nn Online Crystallization determined Online Crystallization determined that the agitation in production that the agitation in production was damaging Crystals. was damaging Crystals.
nn As a result Agitation Reduced As a result Agitation Reduced nn Cake detection in Cake detection in NuestchNuestch filter filter
increased product yield by 3 %increased product yield by 3 %nn Interface detection determined Interface detection determined
organic product loss due to gels organic product loss due to gels earlier resulting in increased earlier resulting in increased recovery. recovery.
SummarySummary
nn LAB,PILOT and PRODUCTION use LAB,PILOT and PRODUCTION use same methodology and identical same methodology and identical equipment equipment
nn R & D needs to accommodate the size R & D needs to accommodate the size issues.issues.
nn PAT can be research,developemnt or PAT can be research,developemnt or production orientatedproduction orientated
IMAGE IMAGE ANALYSISANALYSIS SYSTEM SYSTEM -- Colour SpeckColour Speck
IMAGE IMAGE ANALYSISANALYSIS SYSTEM SYSTEM -- Turbidity, % Solid and Turbidity, % Solid and Interface ControlInterface Control
