Fibre Spectroscopy with Clear Process Vision - IFPAC · Fibre Spectroscopy with Clear Process...
Transcript of Fibre Spectroscopy with Clear Process Vision - IFPAC · Fibre Spectroscopy with Clear Process...
Fibre Spectroscopy Fibre Spectroscopy with Clear Process Visionwith Clear Process Vision
Viacheslav ArtyushenkoViacheslav ArtyushenkoJoachim MannhardtJoachim Mannhardt
Gary ColquhounGary Colquhoun
Fibre Photonics Ltd., Fibre Photonics Ltd., Livingston, ScotlandLivingston, Scotland
&& Berlin, GermanyBerlin, Germanywww.fibrephotonics.comwww.fibrephotonics.com
Cortona 2010Cortona 2010
Spectroscopy Systems Spectroscopy Systems for Full Automated Process Control for Full Automated Process Control
MTAC
Clear View for Optical Process Analysis Clear View for Optical Process Analysis
Research & DevelopmentResearch & DevelopmentDrug development, Process developmentDrug development, Process development
ProductionProductionReaction monitoring, Cleaning, Rinsing, Reaction monitoring, Cleaning, Rinsing, Blending, Dryer monitoring, Granulation, Blending, Dryer monitoring, Granulation, Compaction Compaction
Quality ControlQuality ControlEntrance QC of raw materials, QC of end Entrance QC of raw materials, QC of end products, Content uniformity, Dissolutionproducts, Content uniformity, Dissolution
PackagingPackagingControl, Identification and InspectionControl, Identification and Inspection
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acquire
process
analyse
manage
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Securing Data in ProcessSecuring Data in Process--Control Control
Portable SpectrometersPortable Spectrometers
TruDefender FT from Ahura-Scientific/Thermo
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Exoscan from A2TPHAZIR from Polychromix ReporteR from DeltaNU
Fiber Spectroscopy vs Portable SpectrometersFiber Spectroscopy vs Portable Spectrometers
1) Portable and Fiber Spectroscopy enables to analyze substance composition in gas, liquid or solid phase for many components in single test – faster and cheaper than by chromatography, X-ray or by chemical analysis methods;
2) Portable UV-vis-NIR, Raman and FTIR spectrometers are available for a fast non-contact inspection of material composition out of lab, but could not be used for many PAT applications where:a) reaction tracking is needed in critical points & multiplexed;b) reaction homogeneity control in volume of mixing reagents;c) safe control is required for toxic and radioactive substances;d) process must be controlled at harsh surrounding conditions – high or low temperature, vibrations, high pressure or vacuum, etc.
3) Fiber spectroscopy provides the most flexible solutions for PAT, could be used multiplexed and for all applications listed above, enables cost and time saving, being limited by fiber transmission ranges only
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Fibre Spectroscopy ComponentsFibre Spectroscopy Componentsfor Clear Process Visionfor Clear Process Vision
Fibre ProbesFibre ProbesSensor head design for bespoke spectroscopy methodFibre protection
Process InterfaceProcess InterfaceEnsure reliability by observation window control at any time during a process Enable fully automated implementationinto production equipment
Fibre MaterialFibre MaterialFibre type choice in broad spectral range - from UV to Mid IROptimized bending, etc.
Exciting FlexIR™ midIR from PIKE…
PITTCON 2010: Orlando BoundPITTCON 2010: Orlando Bound
By Jenni L. BriggsEach spring at PITTCON we highlight innovative accessories that the PIKE team… We have several exciting new products to show. Our featured product is the FlexIR™ midIR remote sampling probe accessory. Say goodbye to extremely fragile chalcogenide and halide fibers. The midIR FlexIR uses durable hollow waveguides and has newly designed highly efficient optics for maximized energy throughput. We believe our new FlexIR will revolutionize the midIR fiber optic accessories market.
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Attenuation PIR-fibers & Hollow Waveguides
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Experiment Description:Diamond – 20 FTIR SpectrometerDTGS DetectorBackground beam confocal 2” EFL parabolas with
1mm aperture at focusSample beam 2 2” EFL parabola fiber optic
launch/receive modules with SMA connectors
Experimental tests of PIR-fibers and Hollow Waveguides conducted by Prof. Bruce McIntosh, Orbital, Pomona, CA, USA, 2001
Preliminary ConclusionsThe PolyMicro fibers are unlikely to be suitable for many spectroscopic measurements. Specialized applications may exist in gas measurement. I Interpret the higher minimum absorbance to the low acceptance angle (NA~=0.11). The high absorbance peaks at 1740, 3290 and 5130 are presumably coating nulls in the multi-layer coating on the inside of the tube. The higher absorbance above about 1500 cm-1 when the tube was bent presumably is because of the larger number of reflections in the bent configuration.Nothing in this set of measurements suggests any problems in the major intended application of this fiber, CO2 laser delivery.
The Silver Halide fiber shows much more promise. It may have applications where Mid-IR fingerprint region measurements should be conducted from a vibrating or otherwise inaccessible location.
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Fiber Cables & Spectroscopy ProbesFiber Cables & Spectroscopy Probes
CablesUV-VIS, NIR and MIR
ProbesAttenuated Total Reflectance (ATR)
• Diamond, ZnSe, Si, ZrO, Fiber-Loop tips
Transmission ReflectanceTrans-ReflectionDiffuse ReflectionFluorescenseRaman
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Fibre Probes Contamination in Process Fibre Probes Contamination in Process
Examples ofwindow fouling
Clean in Place Solutions Clean in Place Solutions -- CIPCIP
• Ventilation + heater
• Micro controller
• Cooler
• Wipers
• CIP System components dayly used for clear view applications:
LightHouse ProbeLightHouse ProbeTMTM (LHP) (LHP) from GEA Pharma Systemsfrom GEA Pharma Systems
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Vacuum
2. Window wash2. Window wash
Reference
Wash connections
1. Measurement1. Measurement
3. Cleanness check & 3. Cleanness check & Calibration Calibration
Over pressure
4. Cleaning in Place 4. Cleaning in Place (CIP)(CIP)
Features and applications:for on-line spectroscopic processes measures diffuse reflectance NIR-spectra through 7 Sapphire windows multiple applications
• moisture content, composition, homogeneity• particle size distribution• process end-point detection etc.
windows self-cleaning without process interruption
Cleaning in Place for LHP in Process Cleaning in Place for LHP in Process
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Moisture 5% down to < 1%
Estimated error < 0,1%
Cleaning
Full Automated ProcessFull Automated Process--InterfaceInterface
Control unitControl unitUNICALUNICAL-- FOS FOS
FOSFOS--Interface Interface
with Fiber Probewith Fiber Probe
Containers & PumpsContainers & Pumpsfor Cleaning and for Cleaning and
Calibration SolutionsCalibration Solutions
Analyzer System Analyzer System
Process Control SystemProcess Control System
NIR & MIR AbsorptionNIR & MIR AbsorptionUVUV--VIS AbsorptionVIS AbsorptionRaman Scattering Raman Scattering
FluorescenceFluorescenceVideo imaging Video imaging Particle Size & Particle Size & ConcentrationConcentration
CIP Process Interfaces for Fiber Probes CIP Process Interfaces for Fiber Probes
IPACOS SensoGate-FOS Ceramat-FOS
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1. Probe carrier (Fitting)
2. Integrated Fiber Probes
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IPACOS from GEA Pharma SystemsIPACOS from GEA Pharma Systems
Probe window
Wash tubes
Movable Tip
Additional wash tube
Mirror
Process Interface for liquids and suspensions
Carries one up to four probesCleaning of probes and calibration of analyzer systems at any time during production processCIP capable
Spectroscopic probe for liquidstransmission and reflection modestuneable path lengthsupports UV-Vis, NIR, IR, Raman, Imaging, …ability to combine multiple techniques
Analysis in condense/ dispersive mediamilk, creams, greasefat content
CeramatCeramat--FOS & SensoGateFOS & SensoGate--FOS from KNICK FOS from KNICK
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Washing of Fiber Probes in Process InterfaceWashing of Fiber Probes in Process Interface
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Effective cleaning of sensorTurbular and nozzle effect in central configuration of the cleaning tubestangential incident flow of cleaning mediumhigh flow velocity
Circular slit
Cyclone-nozzle tangential
Probe head with observation window or ATR-Crystal
Fiber optical probe can be retracted pneumatically into washing and calibration chamber
Example: Cleaning of ATRExample: Cleaning of ATR--probe from Olive Oilprobe from Olive Oil
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Sensing Probe Heads with Diamond ATR-
Crystal
Fiber ATR-probe was retracted into the wash chamber to clean it in multi-functional, programmable washing cycles
Washing of Diamond ATR PIR-fiber probe contaminated with olive oil. Base line was reached again in result of 3 CIP cyclesunder real time monitoring by DiATR-probe connected with FTIR spectrometer
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Variety of ATRVariety of ATR--IRIR--Fiber ProbesFiber Probes
Diamond ATR-IR-Fiber Probe of 2.7mm diameter in NeSSI
Water Transmission measured with ATRWater Transmission measured with ATR--ProbesProbes
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Water Transmission Spectra measured with ZrO-ATR-probes - assembled with CIR-Fibers (blue) and NIR-Silica (red)
Fibre Probes for any Spectrometer & any range Fibre Probes for any Spectrometer & any range between 180nm and 18between 180nm and 18µµm (55000m (55000--550cm550cm--1)1)
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Multispectral Beer AnalysisMultispectral Beer Analysis
16 beer samples were analyzed with different fiber coupled spectrometers: FTIR- with ATR-PIR-fiber probes;Silica fiber coupled NIR-, Vis-& UV-spectrometers -
to replace Sensor Panel and common chemical analysis
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Optical Spectra of Beer SamplesOptical Spectra of Beer Samples
VisUV-Vis
IR58 (CIR ATR-probe) IR98 (PIR ATR-probe)
CO2
Fiber Spectroscopy Probes with Fiber Spectroscopy Probes with Full Automated ProcessFull Automated Process--InterfacesInterfaces
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Fiber optical probes can be used for single optical analysis method or for any combination of them:
• UV-VIS
• NIR
• MIR
• RAMAN
• Fluorescence
• Turbidity
• Particle Size & Concentration
• Imaging & Video
UNICAL 9000-FOS Connection to PLC/Prozess-Control (SIPAT, FW 800, etc.) + OPC-Interface & Feld/Profibus
UNICAL 9000-FOS Connection to Spectrometer program+ OPC-Interface &Implementation of commands (DLL)
LIGHTHOUSE Probe Connection to (SIPAT, FW 800, etc.)+ OPC-Interface & Feld/Profibus
and in the synergy with a fully automated Process–Interfaces!