Fibre Spectroscopy with Clear Process Vision

Transcription

1 Fibre Spectroscopy with Clear Process Vision Viacheslav Artyushenko Joachim Mannhardt Gary Colquhoun Cortona Fibre Photonics Ltd., Livingston, Scotland & Berlin, Germany

2 Spectroscopy Systems for Full Automated Process Control M T A C

3 Clear View for Optical Process Analysis Research & Development Drug development, Process development Production Reaction monitoring, Cleaning, Rinsing, Blending, Dryer monitoring, Granulation, Compaction Quality Control Entrance QC of raw materials, QC of end products, Content uniformity, Dissolution Packaging Control, Identification and Inspection

4 Securing Data in Process-Control IMS manage analyse x=! Expert process PAT Instrumental acquire

5 Portable Spectrometers PHAZIR from Polychromix ReporteR from DeltaNU Exoscan from A2T TruDefender FT from Ahura-Scientific/Thermo

6 Fiber 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

7 Fibre Material Fibre Material Fibre type choice in broad spectral range - from UV to Mid IR Optimized bending, etc. Fibre Spectroscopy Components for Clear Process Vision Fibre Probes Sensor head design for bespoke spectroscopy method Fibre protection Process Interface Ensure reliability by observation window control at any time during a process Enable fully automated implementation into production equipment

8 Fibre Material Solutions in µm m range

9 Exciting FlexIR midir from PIKE PITTCON 2010: Orlando Bound By Jenni L. Briggs Each 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.

10 Why to put integral MCT detector in FlexIR?..

11 Attenuation PIR-fibers & Hollow Waveguides Experiment Description: Diamond 20 FTIR Spectrometer DTGS Detector Background beam confocal 2 EFL parabolas with 1mm aperture at focus Sample beam 2 2 EFL parabola fiber optic launch/receive modules with SMA connectors

12 Experimental tests of PIR-fibers and Hollow Waveguides conducted by Prof. Bruce McIntosh, Orbital, Pomona, CA, USA, 2001 Preliminary Conclusions The 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.

13 Bending losses of PIR-fibers vs HW

14 Fiber Cables & Spectroscopy Probes Cables UV-VIS, NIR and MIR Probes Attenuated Total Reflectance (ATR) Diamond, ZnSe, Si, ZrO, Fiber-Loop tips Transmission Reflectance Trans-Reflection Diffuse Reflection Fluorescense Raman

15 Silica Fiber Spectroscopy Probes

16 Transmission of Isopropanol & Water Measured with TransReflex Probe

17 Water Content Control in Isopropanol measured with TransFlex probe

18 Fibre Probes Contamination in Process Examples of window fouling

19 Clean in Place Solutions - CIP CIP System components dayly used for clear view applications: Ventilation + heater Micro controller Cooler Wipers

20 LightHouse Probe TM (LHP) from GEA Pharma Systems 1. Measurement 2. Window wash Reference Wash connections 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 3. Cleanness check & Calibration 4. Cleaning in Place (CIP) Vacuum Over pressure

21 Cleaning in Place for LHP in Process Cleaning 6 5 Moisture 5% down to < 1% 4 Feuchte [%] Estimated error < 0,1% Versuche über 3 Tage

22 Full Automated Process-Interface Process Control System Analyzer System Control unit UNICAL- FOS NIR & MIR Absorption UV-VIS Absorption Raman Scattering Fluorescence Video imaging Particle Size & Concentration Containers & Pumps FOS-Interface for Cleaning and with Fiber Probe Calibration Solutions

23 CIP Process Interfaces for Fiber Probes IPACOS SensoGate-FOS Ceramat-FOS Probe carrier (Fitting) 2. Integrated Fiber Probes

24 IPACOS from GEA Pharma Systems Process Interface for liquids and suspensions Carries one up to four probes Cleaning of probes and calibration of analyzer systems at any time during production process CIP capable Spectroscopic probe for liquids transmission and reflection modes tuneable path length supports UV-Vis, NIR, IR, Raman, Imaging, ability to combine multiple techniques Analysis in condense/ dispersive media milk, creams, grease fat content Probe window Wash tubes Movable Tip Additional wash tube Mirror

25 Ceramat-FOS & SensoGate-FOS from KNICK

26 Washing of Fiber Probes in Process Interface Fiber optical probe can be retracted pneumatically into washing and calibration chamber Effective cleaning of sensor Turbular and nozzle effect in central configuration of the cleaning tubes tangential incident flow of cleaning medium high flow velocity Circular slit Probe head with observation window or ATR-Crystal Cyclone-nozzle tangential

27 Example: Cleaning of ATR-probe from Olive Oil Fiber ATR-probe was retracted into the wash chamber to clean it in multi-functional, programmable washing cycles Sensing Probe Heads with Diamond ATR- Crystal Washing of Diamond ATR PIR-fiber probe contaminated with olive oil. Base line was reached again in result of 3 CIP cycles under real time monitoring by DiATR-probe connected with FTIR spectrometer

28 Variety of ATR-IR IR-Fiber Probes Diamond ATR-IR-Fiber Probe of 2.7mm diameter in NeSSI

29 Water Transmission measured with ATR-Probes Water Transmission Spectra measured with ZrO-ATRprobes - assembled with CIR-Fibers (blue) and NIR-Silica (red)

30 Fibre Probes for any Spectrometer & any range between 180nm and 18µm m ( cm 550cm-1)

31 Multispectral 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 31

32 Optical Spectra of Beer Samples IR58 (CIR ATR-probe) IR98 (PIR ATR-probe) CO 2 UV-Vis Vis 32

33 Fiber Spectroscopy Probes with Full Automated Process-Interfaces 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 and in the synergy with a fully automated Process Interfaces! LIGHTHOUSE Probe Connection to (SIPAT, FW 800, etc.) + OPC-Interface & Feld/Profibus 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)

34 How to build fiber bridge from spectrometer to the process and to drive PAT