Sequip 04/2013. PIA - Particle Image Analyser. In-situ imaging/video probes for in-line particle analysis and crystal morphology

Transcription

1 Sequip 04/2013 PIA - Particle Image Analyser In-situ imaging/video probes for in-line particle analysis and crystal morphology

2 PIA Particle Image Analyser modular image analysis Content PIA Advantages and overview 3 Crystallisation PIA IVM PAT 4 Comparison PIA IVM 5 PIA / IVM system description 6 PIA / IVM sensor 7 Applications 8 Software 9 Technical data 11 2

3 PIA Advantages and Overview Advantages of in-line image analysis with PIA Unfortunately not all particles are round. But most of the measurement systems think this. For example measurement systems based on the principle of Fraunhofer Diffraction or the method to sort and measure particles by sieving. All these measurement principles are not able to recognize and take into account the unknown shape of a particle. The diameter of the sieve to discriminate spheres with a diameter of 5 mm or less will also let pass a cylinder of 10 mm long a diameter of 5 mm. But this cylinder is a much larger particle than the largest sphere with a completely different shape. The daily view through the microscope of a laboratory assistant proves that particles are not only round. Only 2D imaging, enables the viewer to get information about the shape of a particle: spherical, cylinder or polyhedron. This technology is developed since 1998 and protected by a patent. High lights Detection of discrete particles concerning size and shape In-line sensor for particle observation and analysis High resolution, rugged system Instant information and control on Particle shape Particle size Crystal inclusions, agglomerations Turbidity 3

4 PIA IVM PAT-Sensor A lot of different information are needed to control a crystallisation process. The operation of PIA and IVM Insitu Video Microscope together with the PAT-sensor system by Sequip delivers all relevant data in real time. PAT Sensor-System: Evaluation: size distribution trend of crystals / particles PIA: Evaluation: Shape and size evaluation Morphologyparameter of discrete particles IVM: Display of crystals with insitu image grabbing in real time Process System Evaluation Start of crystallisation precipitation Seeding of solution inside discrete particle concentration Up to < 5 Vol % PIA Particle Image Analyser Evaluation of size and shape of discrete particles Crystallisation process Up to 30 Vol % IVM Insitu Video Microscope Image grabbing Viewing of particle shape under process conditions Particle size measurement during Process PAT CSD Sensor systems Particle and crystal size distribution from 0.5 up to 1000 µm in concentrations up to < 40 Vol% in real time 4

5 Comparison PIA IVM with common methods PIA / IVM Common methods Type of imaging Transmission mode Reflection mode Illumination Flash high power LED Laser (produces speckles) Shutter speed High (<20μs), low noise Moderate, more noise Image quality Excellent Moderate Measurement (size / shape) Yes, software suite available No Polymorph detection Possible No Low particle concentration Excellent Poor High particle concentration Limited Moderate Different models Yes No Customized solutions Yes No Crisp High contrast Low noise No motion blur of moving particles A cut-out part of an image 5

6 PIA - IVM System Description Systems at work PAT IVM Measurement of crystal sizes under discrete in line options Image analysis of: Real sieve data Elongation relationship Relationship between concavity and roundness Relation of crystalline angularity of the crystalline structure or of abrasion Evaluation of satellite structures Evaluation of holes, notches etc. Evaluation of broken particles Verification accuracy and linearity Based on pixel resolution of the modular camera system and the optics Evaluation of discrete available particles and crystals in well known concentration ranges of lab application 6

7 PIA Technical design PIA- Sensor Lab version Process version Unique features: Direct imaging Excellent image quality Backlight illumination: high contrast accurate quantitative information detection of inclusions Small in-line probe Designed for aggressive environments ATEX proofed 7

8 Applications Pharmaceutical intermediate Lactose Salt crystals Melamin Ammonium Nitril Sugar research Crystallisation Crystals Eutectic freezing Hormon Crystallisation Crystallisation Ice Emulsion Enzym Aspartaam Protein 8

9 PIA / IVM Software Software impression during measurement Software IVM Insitu Video Microscope : Viewing Software Image grabbing in real time without analysis PIA Particle Image Analyser: Viewing & Analysis Software: Size and shape distribution of discrete particles Specification 8/10 bit digitization Real-time uncompressed video storage Manual and automatic tools Enhancement Analysis Real-time viewing On-line measurements On-line control of illumination Report generation MS Excel interface 9 Image enhancement Contrast filtering Deblurring Contour enhancement Noise reduction Image analysis PSD (shape & size) Pollution removal Trend analysis Detection of anomalies

10 PIA Set up Modular Software- and instrument configurations for extended analysis requirements Miscellaneous optional modules give the possibility of extended measurement requirements. Allows the analysis of grain shape modification during the process or directly during the crystallization Correlation of the Coherency of segregation as a function of grain shape and grain size. Easy- to-use in the daily Work In-situ measurement No sample drawing The software has an easy GUI, 24h online operation under in situ conditions Exposition of trends 100% Screening Application areas: Research and development Process control Quality control Application examples: Surface characteristics of catalysts Investigation /control of crystal shapes Formation / nucleation of particles Production of granulate sugar crystals, pharmaceuticals intermediates, resins and microcapsules PIA process sensor stirrer 10

11 PIA Technical data Processing unit Interface module: connection for sensor head, power supply, light source, cooling. Computer: Industrial high-performance PC and frame grabber Software: Capture and illumination control Image capture Image enhancement Particle detection and analysis Hardware specifications ICH Internal Camera EAC External Camera Measuring range µm µm Field of view Resolution 8.0 x 6.0 mm (standard model) 2.0 x1.5 mm (macro model) ~10 µm (macro model) ~40 µm (standard) 10.0 x 7.5 mm (standard model) 2.5 x 1.75 mm (zoom model) 1.0 x 0.75 mm (ultra zoom model for 1.4 Mpixel) 10 µm (standard) 2.5 µm (zoom model) 1.0 µm (ultra zoom model) Exposure time Frame speed 5 10 µs < 10 µs 25 frames /s Avg. 15 frames /s Image Black/white, progressive scan 610 x 480 pixel Black/white, progressive scan, 0.7 Mpixel; 1.4Mpixel, 2 Mpixel, 5 Mpixel Temperature range - 20 C. 125 C - 20 C. 125 C Material Hasteloy, sapphire windows Hasteloy, sapphire windows Specifies Separate power supply No framegrabber at the PC No interface module 11 Sequip S+E GmbH Angermunder Str. 22 D Düsseldorf Tel.: +49 (0) Fax: +49 (0) Contact: info@sequip.de