Fibre Spectroscopy with Clear Process Vision - IFPAC · Fibre Spectroscopy with Clear Process Vision Viacheslav Artyushenko Joachim Mannhardt Gary Colquhoun Fibre Photonics Ltd.,

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

. .. ….. ….

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

www.fibrephotonics.com

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


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.

Fibre Material Solutions in 0.2Fibre Material Solutions in 0.2--1818µµm rangem range

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.


Why to put integral MCT detector in FlexIR?..


Attenuation PIR-fibers & Hollow Waveguides


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.


Bending losses of PIR-fibers vs HW


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



Silica Fiber Spectroscopy ProbesSilica Fiber Spectroscopy Probes

Transmission of Isopropanol & Water Measured with TransReflex Probe


Water Content Control in Isopropanolmeasured with TransFlex probe


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


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

0

1

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1 201 401 601 801 1001 1201 1401 1601 1801 2001 2201 2401 2601 2801 3001 3201 3401

Versuche über 3 Tage

Feuc

hte

[%]

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


1. Probe carrier (Fitting)

2. Integrated Fiber Probes

1

21

2

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


Washing of Fiber Probes in Process InterfaceWashing of Fiber Probes in Process Interface


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


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


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


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


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!

How to build fiber bridge fromHow to build fiber bridge fromspectrometer to the process spectrometer to the process

and to drive PATand to drive PAT……


Documents

Fibre Spectroscopy with Clear Process Vision - IFPAC · Fibre Spectroscopy with Clear Process Vision Viacheslav Artyushenko Joachim Mannhardt Gary Colquhoun Fibre Photonics Ltd.,