Measuring Catalysts with the CAMSIZER
 

Measuring Catalysts with the CAMSIZER

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Gert Beckmann of Retsch Technology and HORIBA Scientific discuss how the CAMSIZER measures the particle size and shape of catalyst beads and extrudates in a manner of minutes.

Gert Beckmann of Retsch Technology and HORIBA Scientific discuss how the CAMSIZER measures the particle size and shape of catalyst beads and extrudates in a manner of minutes.

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Measuring Catalysts with the CAMSIZER Measuring Catalysts with the CAMSIZER Presentation Transcript

  • CAMSIZER CAMSIZER® Dynamic Image Analysis ISO 13322-2 conform Catalyst Beads, Powders, Extrudates Presentation© Retsch Technology 2012 - 1 Speaker: Dipl.-Ing. Gert Beckmann Retsch Technology GmbH Host: Ian Treviranus HORIBA Scientific Inc.
  • © Retsch Technology 2012 - 2 Catalysts
  • © Retsch Technology 2012 - 3 CAMSIZER & CAMSIZER XT
  • Benefits for the Catalyst Industry using the CAMSIZER® • Instead of size measurement with sieve shaker or roller grader and shape analysis by visual inspection you can do a CAMSIZER analysis of both in a much shorter time (reduce labour costs and get better results) • Reproducible results because of high statistics and accurate calibration (less headaches) • Measuring easily in compliance of specifications of grain size, oversize and dust (<0.1%), roundness and sphericity and measure the dust content before and after a crush resistance test • Measure the increase of layer coating thickness of noble© Retsch Technology 2012 - 4 (precious) metals and change of roundness because of the layer coating of Al2O3, SiO2 or ceramic catalyst carriers • Additional benefit: Measuring different diameters and length of extrudates
  • Measuring Principle Measuring Principle© Retsch Technology 2012 - 5
  • Measuring Principle CAMSIZER for Extrudated Catalysts Feeder© Retsch Technology 2012 - 6 CCD-Basic-Image and Particles Falling direction
  • Evaluation of the Results© Retsch Technology 2012 - 7 Measuring Principle © Retsch Technology GmbH
  • Measuring Principle Two-Camera-System© Retsch Technology 2012 - 8 Basic-Camera Zoom-Camera
  • Measurement Results Particle Size xc min xarea xFe max “width” “diameter over “length” projection surface” A xc min xFe max© Retsch Technology 2012 - 9 CAMSIZER results are compatible xarea with A‘ = A sieve analysis
  • Measurement Results Comparison of Size Definitions xc min  xArea  xFe max Q3 [%] Sample A_Basic_0.2%_xc_min_001.rdf Sample A_Basic_0.2%_x_area_001.rdf Sample A_Basic_0.2%_xFemax_001.rdf 80 70 60 50 40 30© Retsch Technology 2012 - 10 20 10 0 0.2 0.4 0.6 1 2 [mm] x x[mm] different different size definitions results
  • Measurement Results Volume Definition Q3 ellipsoid width ellipsoid-volume length  max Vellipsoid   xFe max  xc 2 min xFe 6 xc min© Retsch Technology 2012 - 11 xc min width xc min Ellipsoid model leads to better results
  • © Retsch Technology 2012 - 12 Roller Graders
  • See and Show Small Differences (Product 1, 2 and 3)© Retsch Technology 2012 - 13
  • See and Show Small Differences (3, 4, 5 and 6) q3 [%/mm] 3_15mm_LB_B-x_area_004.rdf 4_15mm_LB_B-x_area_005.rdf 5_15mm_LB_B-x_area_007.rdf 6_15mm_LB_B-x_area_009.rdf 700 7_15mm_LB_B-x_area_010.rdf 8_15mm_LB_B-x_area_011.rdf 9_15mm_LB_B-x_area_012.rdf 0_15mm_LB_B-x_area_003.rdf 600 500 400© Retsch Technology 2012 - 14 300 200 100 0 1.40 1.45 1.50 1.55 1.60 1.65 1.70 x_area [mm]
  • CAMSIZER Measuring Principle for elongated particles (extrudates) A 2 A/2 xMa min A xFe max 2 A/2 xc min© Retsch Technology 2012 - 15 xMa min
  • Measurementg Results Length and Width definitions for elongated extrudates Q3 [%] q3 [%/mm] CoMo2-0,1%Absch_xc_min_001.rdf CoMo2-0,1%Absch_xFemax_001.rdf 90 180 80 160 70 140 60 120 50 100© Retsch Technology 2012 - 16 40 80 30 60 20 40 10 20 0 0 1 2 4 10 x [mm]
  • Length measurement Extrudates Particle Size of Extrudates xFe min xc min A/ 2 Limits xlength > xMa min xMa min A Limits xstretch > xMa min xFe max Xstretch = A© Retsch Technology 2012 - 17 xMa min xlength A/ 2 Area / Diameter xstretch Xlength = x Fe max 2  xMa min 2 Pythagoras Xlength is the best length for extrudates
  • Particle Size of Extrudates xFe min xc min A xMa min xMa min is best xFe max diameter© Retsch Technology 2012 - 18 for xstretch extrudates area / diameter A Xstretch = xMa min
  • Diameters and Length Quadralobes Q3 [%] q3 [%/mm] Extrudate Diameters 90 180 80 160 D1 70 140 D2 Extrudate Length 60 L 120 50 100 40 80© Retsch Technology 2012 - 19 30 60 20 40 CoMo2-Diameter_xc_min_001.rdf CoMo2-Length_xFemax_001.rdf 10 20 0 0 0.4 1 2 4 10 x [mm]
  • CAMSIZER® length definitions for elongated particles (extrudates) xFe max xlength xstretch xFe max xlength xstretch A© Retsch Technology 2012 - 20 xMa min xMa min A Xlength = x Fe max2  xMa min2 Xstretch = xMa min
  • CAMSIZER® length definitions for elongated particles (extrudates) xFe max xlength xFe rec xFe rec = xlength xFe rec = xlength xMa min xMa min© Retsch Technology 2012 - 21 xFe rec xMa min
  • Reference Particles Calibration validation with steel rods of the same dimensions as particles© Retsch Technology 2012 - 22 reticle implant
  • © Retsch Technology 2012 - 23 Reference Particles
  • © Retsch Technology 2012 - 24 Reference Particles
  • © Retsch Technology 2012 - 25
  • © Retsch Technology 2012 - 26
  • © Retsch Technology 2012 - 27
  • © Retsch Technology 2012 - 28
  • © Retsch Technology 2012 - 29
  • CAMSIZER for Extrudated Catalysts Feeder© Retsch Technology 2012 - 30 CCD-Basic-Image and Particles Falling direction
  • CAMSIZER for Extrudated Catalysts Feeder Motorized Feed Guide orients the extrudates© Retsch Technology 2012 - 31 CCD-Basic-Image and Particles Falling direction
  • Applications – Pharmaceuticals Length + Diameter of Implants Length measurement xlength ~ 26mm Diameter measurement Ø ~ 0.85mm© Retsch Technology 2012 - 32 validation and test measurements of 1. with plastic and produced 2. steel cylinders implants (release time 1 month)
  • Quadralube Diameters CAMSIZER® width definitions for elongated bended extrudates Q3 [%] q3 [%/mm] CoMo2-0,1%Absch_xc_min_001.rdf 90 180 x2 max 80 160 70 140 x1 max 120 60 50 100© Retsch Technology 2012 - 33 40 80 30 60 20 40 10 20 0 0 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 x [mm] x1 max x2 max
  • Diameter 1 ~ “xmax 1”, Dia 2 ~ “xmax 2” Q3 [%] q3 [%/mm] 90 450 80 400 70 350 60 300 xmax = volume based 50 250 Dia = number based 40 200 30 RT647_602_Z_LB_0.3%_xc_min_001.rdf 150 RT647_602_Z_LB_0.3%_x_len_001.rdf 20 100 10 50 0 0 1 2 3 4 5 6 7 x [mm] Q3 [%] q3 [%/mm] 90 450© Retsch Technology 2012 - 34 80 400 RT647_600_Z_LB_0.3%_xc_min_001.rdf RT647_600_Z_LB_0.3%_x_len_002.rdf 70 350 Quadralobes 60 300 50 250 40 200 30 150 20 100 10 50 0 0 1 2 3 4 5 6 7 x [mm]
  • diameter d Symmetrical Regular Trilobes w  iw  d height of equilateral trilobe w  d  iw h  ih  d inner height ih h diameter d height of trilobe inner height iw inner width of trilobe ih h w width of equilateral trilobe sin 60  ih / iw h  iw  sin 60  d iw iw  sin 60  ih inner width of trilobe© Retsch Technology 2012 - 35 h  w  d   sin 60  d w h  w  d   0.866  d width of trilobe h  w  0.866  d  0.866  d h  w  0.866  d  0.134 It’s possible to recalculate the height from the width and the diameter of an equilateral trilobe (one peak in the q3 frequency distribution). For this you need the width (result of mode value xmax) and the diameter of the lobes. It’s also possible to see the height on the left side of the distribution at about x(Q3=0.5%)
  • Irregular Trilobes diameter d sh  sih  d lw  liw  d equal-sided trilobe of an isosceles or shortest height inner height shorter sw  siw  d sih sh liw longest inner width of an isosceles / equal-sided trilobe lw longest width of an isosceles or equal-sided trilobe© Retsch Technology 2012 - 36  2 siw2  sih 2  liw 2 It’s possible to recalculate the height from 2 the width and the diameter of a non  liw  equilateral trilobe (two peaks in the q3 sh  siw   2  d  2  frequency distribution). For this you need the result values of the two  lw  d  2 peaks and the diameter of the lobes. sh  sw  d     d 2  2 
  • length measurement methods without and with motorized feed guide (sample director) Q3 [%] length measurement Rod 2mm_1-1 B_xFemax_002.rdf Without Guidance Sheet 90 Rod Rod Rod 3mm_1-1 4mm_1-1 5mm_1-1 B_xFemax_002.rdf B_xFemax_002.rdf B_xFemax_002.rdf Rod 7mm_1-1 B_xFemax_002.rdf Rod 9mm_1-1 B_xFemax_002.rdf 80 for non orientated minipellets 70 60 correct length 50 40 30 short 20 length 10 0 1 2 3 4 5 6 7 8 9 x [mm] Q3 [%] With Guidance Sheet© Retsch Technology 2012 - 37 90 80 length measurement 70 for orientated rods + extrudates 60 50 Rod 2mm_1-3 B_LB_xFemax_001.rdf Rod 3mm_1-3 B_LB_xFemax_001.rdf 40 Rod 4mm_1-3 B_LB_xFemax_001.rdf Rod 5mm_1-3 B_LB_xFemax_001.rdf Rod 7mm_1-3 B_LB_xFemax_001.rdf Rod 9mm_1-3 B_LB_xFemax_001.rdf 30 20 correct length 10 0 1 2 3 4 5 6 7 8 x [mm]
  • Length measurement Short Catalyst Carriers without guidance sheet (sample director)© Retsch Technology 2012 - 38
  • CAMSIZER® length measurements for elongated particles (extrudates) correct length short length xFe max Ø 2mm φ© Retsch Technology 2012 - 39 xlength xMa min Xlength = x Fe max2  xMa min2
  • Length Measurement without feed guide (sample director) q3 [%/mm] q3 [%/mm] 200 120 Kaneka_160H_Z_1%-mit-Ausblndng099_xFemax_002.rdf Z-Ausbl-conv0985-160H-1-3Part_xFemax_002.rdf 100 Z-Ausbl-conv0985-200H-1-3Part_xFemax_001.rdf correct length 150 80 100 short length correct length 60 40 50 20 0 0 1.0 1.5 2.0 2.5 3.0 3.5 x [mm] 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 x [mm]© Retsch Technology 2012 - 40 Right side of distribution
  • Shape Measurement Short Catalyst Carriers Sharp  Rounded© Retsch Technology 2012 - 41
  • Measurement Results Particle Shape • width/ length = xc min aspect ratio x c min xFe max x Fe max • Roundness P 4 A A 2 P • Symmetry r2 1  © Retsch Technology 2012 - 42 1  min r1  S 2 r  r1   2  • Convexity A convex A real A convex A real
  • CAMSIZER - Advantages • measurement range 30 µm – 30 mm • easy operation • very direct particle definition - via particle width (analogue to sieving) - via particle length - or projection surface • insensitive, maintenance-free, robust© Retsch Technology 2012 - 43 • particle shape- density measurement, counting of particles • high density of information
  • © Retsch Technology 2012 - 44 Online-Applications
  • Online Application (Process Control) Process Part of Sample Partial flow Manipulated Controlled variable variable© Retsch Technology 2012 - 45 Typical on-line arrangement LIMS System Control center Online Application Control Circuit
  • CAMSIZER® online (housing open) • Double Housing • Industrial PC • UPS (uninterruptable power supply) • 4-20mA interface • Profibus interface • Analogue + digital I/O • Automatic cleaning© Retsch Technology 2012 - 46 • Lab or test measurements possible
  • CAMSIZER® OnLine (closed) • Double safe • Overpressure or negative pressure • Air condition • Bulk bypass • Remote control or direct control© Retsch Technology 2012 - 47
  • CAMSIZER® Online (housing closed) sample entrance and light signals are showing • Dust protected by funnel the operation status compressed air • Air condition portable PC. Only used during • Funnel shaker installation and testing of • Automatic interfaces cleaning • Remote control© Retsch Technology 2012 - 48 • Communication tests with portable PC funnel shaker CAMSIZER-online (final check at manufacturer)
  • Automatic Sampling from a Pipe sampling© Retsch Technology 2012 - 49 product stream to big bag sample dividing pipeline to the CAMSIZER®
  • Customized sample feeding solution • Automatic sampling (from right) • Manual sampling (on the left) • Level control© Retsch Technology 2012 - 50 • Dust protection • Vacuum (negative pressure)
  • Applications – Enzymes and Coal Online applications with automatic sample taking sample from pipe sample from belt© Retsch Technology 2012 - 51 sample from pipe sample from pipe
  • CAMSIZER online Dust protection / Ionization • Air filters • Exhaustion • Cleaning© Retsch Technology 2012 - 52 • Ionisation
  • Interfaces for CAMSIZER Online • Profi-Bus Interface • Digital in- and outputs o 18 CAMSIZER® internal signals o External connection to facilitate control and status reports • Analog 4-20mA interfaces to connect the device to the PCS • LAN Network connection© Retsch Technology 2012 - 53 o Supplementary data export to LIMS o Task file configuration o Calibration o Service
  • CAMSIZER Application Fields • Catalysts • Metal powders • Extrudates • Drugs • Sand, Refractory • Carbon black • Glass • Salt • Ceramics • Abrasives • Coal • Detergents • Plastics • Sugar • Food • Fertilizer© Retsch Technology 2012 - 54 Field installations for CAMSIZER® • Quality laboratories • Industrial environment locations • Research and development / Universities • Automatic process control and interaction
  • End Thank you for your attention!© Retsch Technology 2012 - 55
  • Counting with CAMSIZER® Correct Particle Counting possible with CAMSIZER Sphere 1 Sphere 2© Retsch Technology 2012 - 56 Falling Direction
  • CAMSIZER for Extrudated Catalysts Feeder© Retsch Technology 2012 - 57 CCD-Basic-Image and Particles Falling direction
  • CAMSIZER for Counting particles counted and measured particles not counted and not measured© Retsch Technology 2012 - 58 Feeder, CCD-Basic-image and particles in reality Falling direction