Cutting Edge Series The CAMSIZER

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1 CAMSIZER Cutting Edge Series The CAMSIZER Dynamic Digital Imaging ISO conform Retsch Technology Presenter: Dipl.-Ing. Gert Beckmann Retsch Technology GmbH Host: Ian Treviranus HORIBA Instruments International Irvine, CA

2 History Retsch / Retsch Technology Founding by F. Kurt Retsch in Düsseldorf Development of Milling and Sieving machines, for the work in quality labs Founding of Solutions in particle sizing as a Profit Center of RETSCH s 1998 Retsch Technology Development of the first Retsch mill 1989 RETSCH becomes part of the Verder group

3 History Retsch Technology Development of CRYSTALSIZER & CAMSIZER Development of AutoSampler System Announcement of Particle size analyzers in Europe Retsch Technology Retsch Technology becomes an independent company as part from & 2002 New shape functions of CAMSIZER first Online- Installations 2006 Improvement of CAMSIZER (2006) with AutoHeight, LED technology, Software, improved resolution, sharpness and contrast

4 Content Device 1. Measuring Principle 2. Measurement Results Retsch Technology Application 3. Range of Application 4. Competing Measuring Methods

5 Content Device 1. Measuring Principle - Two Camera-System - Resolution 2. Measurement Results Retsch Technology Application 3. Range of Application 4. Competing Measuring Methods

6 Comparison between Static Dynamic Image Analysis Retsch Technology ISO ISO

7 Measuring Principle Measuring Principle Retsch Technology

8 Two-Camera-System Zoom Basic Measuring Principle Basic-Camera Zoom-Camera Retsch Technology

9 Features Reproducibility by Auto-Height Retsch Technology Filling in sample Conveying sample

10 Features Maintenance-Free by Venturi-Flushing Retsch Technology

11 Features LED Light Source Measurement Stand By Retsch Technology

12 More Light => better Sharpness weaker light source => wider aperture blurry images = bad resolution Retsch Technology wider depth of focal plane stronger light source => smaller aperture sharper images = more resolution

13 Capture time influence CCD-Basic pixel raster ISO conform Retsch Technology CCD-Zoom pixel raster 15µm Height of fall during illumination time New CAMSIZER model 2006 (10µs)

14 Size Matters Retsch Technology

15 Measuring Principle Resolution Detection of particles One pixel is element of a projection when at least half of the pixel is covered. CCD - Basic CCD - Zoom Retsch Technology

16 Measuring Principle Resolution Zoom Basic Retsch Technology Advantages precise frame taking of particle projections large dynamic measuring range: 30µm to 30mm

17 Measuring Principle Range of use Shape Size Retsch Technology µm to 30 mm

18 Measuring Principle Advantages fast reproducible precise Retsch Technology maintenance-free & robust

19 Content Device 1. Measuring Principle 2. Measurement Results -Size -Shape Retsch Technology Application 3. Areas of Application 4. Competing Measuring Methods

20 Measurement Results Particle Size Retsch Technology What is the size of this particle?

21 Measurement Results Particle Size x cmin width x area diameter over projection surface A x Fe max length x cmin x Fe max Retsch Technology CAMSIZER results are compatible with sieve analysis A = A x area

22 Measurement Results Comparison of Size Definitions x cmin x Area x Fe max Q3 [%] 80 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 Retsch Technology different size definitions 2 x [mm] x[mm] different results

23 Basics Statistical lenghts and particle size x Fe x c x Ma A x Fe = distance between two tangents perpendicular to the measuring direction Retsch Technology Measurement direction A` = A x area x Ma x c = length of the area bisector in the measuring direction = maximum chord perpendicular to the measuring direction x area = equivalent diameter of a sphere with the same characteristics

24 Measurement Results Particle scanning in multi - directions Retsch Technology x cmin x Fe max X Fe = FERET Diameter = outer Diameter

25 Particle scanning in multi - directions Retsch Technology A / 2 xma min A / 2 Measurement Results x Fe max

26 Measurement Results Volume Definition Q 3 ellipsoid ellipsoid-volume V ellipsoid = π x 6 Fe max x 2 c min x Fe max width x cmin length Retsch Technology Ellipsoid model leads to better results width x cmin x cmin

27 Measurement Results Reproducibility Retsch Technology Calibration with traceable standard => Absolute accuracy

28 Calibration Results Glass Bead-Standard 500µm 2000µm Q3 [%] p3 [%] ,25mm ± 24µm 95% (* Q 3 75% ) written in the calibration certificate CAMSIZER and Sieving (72%) done with calibrated sieve by hand Polydisperse-Particle-Std-trnspnt_xc_min_002.rdf Polydisperse-Particle-Std-trspnt_xc_min_001.rdf Polydisperse-Particle-Std-trspnt2_xc_min_001.rdf Sieving-Kyoto-1-25mm-2.ref Mean.ref Retsch Technology CAMSIZER * Sieving x [mm]

29 Whitehouse Standard XX030 Retsch Technology

30 Measurement Results Resolution Capacity Retsch Technology mixture of six sizes of grinding balls

31 Features AutoSampler Retsch Technology

32 Areas of Application Trend Analysis Retsch Technology

33 Applications - Rice Particle Size Models length x Fe max for amount of broken rice Whole Grain Rice ¾- Grain Broken Rice Retsch Technology ¼- Grain ½- Grain

34 Applications - Rice Old technique to measure diameter and length of the rice grains Retsch Technology

35 Applications - Rice One CAMSIZER for the lab Retsch Technology

36 Applications - Rice Ionizer to remove the static charge Retsch Technology

37 Applications - Rice Rice grains are oriented to be measured correctly in the length Retsch Technology

38 Applications - Rice Mixture of different rice qualities Retsch Technology

39 Applications - Rice AutoSampler for production control Retsch Technology

40 Applications - Rice Unlimited throughput Retsch Technology

41 Applications - Rice Different cups for different tasks Retsch Technology

42 Applications - Rice Cups on the belt are read by the bar code reader Retsch Technology

43 Applications - Rice Thai Rice Q0 [%] Reis Thai fixgs 07% 2zu3_xFemax_007.rdf Thai.re Retsch Technology xfe_max [mm] Perfect agreement with hand measurement

44 Applications - Rice Wild Rice Q0 [%] 90 Reis wild fixgs 07% 2zu3_xFemax_012.rdf Wild.re Retsch Technology xfe_max [mm] Perfect agreement with hand measurement

45 Applications - Rice Basmati Rice Q0 [%] 90 Reis basmati fixgs 07% 2zu3_xFemax_013.rdf basmati.re Retsch Technology xfe_max [mm] Perfect agreement with hand measurement

46 Measurement Results Particle Shape matters as well Breadth-/ Lengthratio x Fe max x cmin Roundness A P Retsch Technology Symmetry Convexity r 1 C r 2 A convex A real

47 Measurement Results Size- & Shape Results amount size + size distribution - amount by size shape + shape distribution - shape by size - amount by shape Retsch Technology shape size

48 Measurement Results Particle Shape: Amounts in a Mixture Q3 [%] AK_22,15g_0,3%_BZ_LB_n Ü_xc_min_001.rdf IA_22,15g_0,3%_BZ_LB_n A Ü_mit Aerosil_xc_min_001.rdf IA + AK_je B 22,15g_0,3%_BZ_LB_n Ü_als Mischung_xc_min_001.rdf A + B B A B 50 Retsch Technology A b/l

49 Measurement Results Particle Shape: Amounts in a Mixture Q 3 (round particles) = 32.8% x cmin Retsch Technology x Fe max 67.2%

50 Measurement Results Optical Process Control analysis for size and shape Retsch Technology

51 Measurement Results Data-Storage classes in measurement Retsch Technology size classes in storage 50 classes displayed

52 Measurement Results Advantages measurement of very broad particle distributions measurement of very narrow particle distributions Retsch Technology easy operation highly direct particle definition - by width (analogue to sieving) - by length - or projection surface non-sensitive, fail-safe, robust ideal for particle shape analyses measurement of density, transparency and counting of particles

53 Content Device 1. Measuring Principle 2. Measurement Results Retsch Technology Application 3. Areas of Application Features Applications 4. Competing Measuring Methods

54 Areas of Application Places of Installation laboratories next to manufacturing line optimized quality control of product and process research institutes / universities Retsch Technology Applications fertilizer pharmaceuticals food salt sugar washing powder plastics coal carbon black metal powder fireproof products glass (reflex) ceramic-granules abrasives sand construction materials

55 Features Quality Control Retsch Technology

56 Applications Glass Beads Traditional Measurement Particle size distribution sieve analysis Particle shape (roundness) microscope or Round-O-Meter Retsch Technology

57 Applications Glass Beads Traditional Measurement Retsch Technology Round-O-Meter Sieve Shaker Microscope

58 Applications Glass Beads CAMSIZER - Advantages α 1 Retsch Technology α 2 β 2 β 1 CCD CAMSIZER measurement of particle size distribution and particle shape of transparent reflective glass beads

59 Applications Glass Beads Bead Embedment HEAD LIGHT Retsch Technology Road Surface Stripe

60 Applications Glass Beads Proper Bead Embedment Retsch Technology

61 Applications Glass Beads Gulf Line Inverted Profile Thermoplastic Retsch Technology Ribbon Gun Application Double Drop Bead Dispensers Profile Wheel

62 Applications - Pharmaceuticals Q3 [%] Transparency 60 α 1 α 2 β β 1 CCD cumulative volume distribution Sample No3-yellow_xc_min_013.rdf Sample-yellow-white-1_xc_min_002.rdf Sample-yellow-white-2_xc_min_002.rdf Sample-white-21st-November-12h_xc_min_001.rdf Sample-yellow-white-2_xc_min_001.rdf Sample-yellow-white-1_xc_min_001.rdf Transb Retsch Technology Transparency

63 Applications - EPS Traditional Measurement Traditional measurement: Sieve analysis 0,4 1,6 mm Sufficient statistics in short time necessary until now: optical system with poor statistics Retsch Technology

64 Applications - EPS 1. Move 2. Sliding friction F 1 3. Static friction F 2 Retsch Technology Q3 [%] _PT100_xc_min_008.rdf 5454_random_xc_min_009.rdf 5454_Huntsman-sieve.ref xc_min [mm] q3 [%/mm] Round particles with low density are captured but there is no rerelease

65 Applications - EPS CAMSIZER - Advantages Q3 [%] Grade Test II Measurement NSP ausblenden_002.rdf Grade Test II Measurement NSP ausblenden_001.rdf 90 Grade Test-o rdf III Measurement Grade 21319_ III Measurement 455_2_Haan_001.rdf Grade 21319_ III Measurement 455_2_Haan-Xc_001.rdf Retsch Technology high resolution CAMSIZER measurement of particle size distribution, save measurement time, more information, improved measurement equipment monitoring x [mm]

66 Applications Carbon Black Traditional Measurement Retsch Technology pelletized carbon black Particle size of pelletized carbon black sieve analysis mm (approx. 2 min.) abrasion analysis (approx. 3 * 6 min.)

67 Applications Carbon Black Traditional Measurement Sensitive carbon black pellets are destroyed by sieving, conveyance and storing Retsch Technology

68 Applications Carbon Black CAMSIZER - Advantages Q3 [%] Particle Size Ruß_ölgeperlt_ES34_001.rdf Carbon black_es34_001.rdf Ruß_ölgeperlt_ES34_002.rdf Carbon black_es34_002.rdf Ruß_N660_001.rdf Carbon black_n660_001.rdf Ruß_N660_002.rdf Carbon black_n660_002.rdf x [mm] Retsch Technology CAMSIZER measures size and shape without destroying sensitive carbon black particles Q3 [%] Carbon Ruß_ölgeperlt_ES34_001.rdf black_es34_001.rdf Carbon Ruß_ölgeperlt_ES34_002.rdf black_es34_002.rdf Carbon Ruß_N660_Form_002.rdf black_n660_001.rdf Carbon Ruß_N660_Form_001.rdf black 002.rdf Roundness SPHT

69 Applications - Fertilizer Traditional Measurement Retsch Technology Sieve analysis mm

70 Applications - Fertilizer CAMSIZER - Advantages Analysis of size and shape of Retsch Technology broken grained coated fertilizers

71 Applications - Desiccant Traditional Measurement Retsch Technology Sieve analysis mm Vibrating plate and weighting (amount of broken particles)

72 Applications - Desiccant CAMSIZER - Advantages good product r r broken particles Retsch Technology Q3 [%] TP-WS 0525_Probe1_BZ_0.5%_xc_min_001.rdf TP-WS 0525_Probe2_BZ_0.5%_xc_min_001.rdf TP-WS 0525_Probe3_BZ_0.5%_xc_min_001.rdf TP-WS 0525_Probe4_BZ_0.5%_xc_min_001.rdf TP-WS 0525_Probe5_BZ_0.5%_xc_min_001.rdf TP-WS 0525_Probe6_BZ_0.5%_xc_min_001.rdf TP-WS 0525_Probe7_BZ_0.5%_xc_min_001.rdf TP-WS 0525_Probe8_BZ_0.5%_xc_min_001.rdf TP-WS 0525_Probe9_BZ_0.5%_xc_min_001.rdf TP-WS 0525_Probe10_BZ_0.5%_xc_min_001.rdf 20% broken 17.4% broken Symm Symmetry r 1 r 2 r ~ min r 1 2

73 Applications - Sugar Traditional Measurement Sieve analysis mm Retsch Technology

74 Applications - Sugar CAMSIZER - Advantages Size analysis of fine sugar, household sugar, granular rock candy and rock candy Retsch Technology Shape analysis of granular rock candy

75 Applications - Sugar Online-Measurement Bypass CAMSIZER print out Retsch Technology Samples for truck driver and quality stock

76 CAMSIZER Online solution for the packing and loading process Size Control of Sugar CAMSIZER online Retsch Technology

77 Applications Food Freeze dried Coffee Rice Corn ρ Expansion Grade/Ratio = mass V CAMSIZER Retsch Technology Expansion of Plastics Rice Puffed Rice Sugar coated Corn Popcorn rd = ρ = g ρ = 1.9 cm 3 convex mass V CAMSIZER g ρ = 0.19 cm 3 automatic balance connection to CAMSIZER g ρ = 0.25 cm 3 Measuring expansion grade with sample density

78 Freeze Dried Coffee, Size, Shape, Particle Density ρ Q3 [%] 90 Q3 [%] Nestle-BZ-Sample grams_xMamin_001.rdf Nestle-BZ-Sample2-42-9grams_xMamin_001.rdf Nestle-BZ-Sample grams_xMamin_001.rdf Nestle-BZ-Sample grams_xMamin_001.rdf Retsch Technology Particle Density (apparent density = ρ = m/v CAM ) Sample No. Sample1_ xc_min_mv.rdf Sample2_ xc_min_mv.rdf Sample3_ xc_min_mv.rdf Sample4_ xc_min_mv.rdf size x [mm] Sample 1 Sample 2 Sample 3 Sample Size : x cmin RD [g/cm³] Volume: Ellipsoid Particle density shape SPHT

79 Minerals for Roofing Fabric Retsch Technology

80 #231 Good Product Compact particles have high UV stability Retsch Technology

81 Minerals #181 flaky angular Retsch Technology

82 Minerals #181 Retsch Technology additional ball milling for rounding of the particles

83 #181 ballmilled Q3 [%] #181-Conveyor_xc_min_002.rdf #181-Ballmilled_xc_min_001.rdf #231-Conveyor_xc_min_001.rdf Retsch Technology SPHT

84 CAMSIZER for elongated particles (extrudates) A 2 x cmin x Ma min Retsch Technology A/2 xfe max A/2 x Ma min A 2

85 Length and Width definitions for elongated extrudates Q3 [%] CoMo2-0,1%Absch_xc_min_001.rdf CoMo2-0,1%Absch_xFemax_001.rdf q3 [%/mm] Retsch Technology x [mm]

86 CAMSIZER length definitions for elongated particles (extrudates) x Fe max x length x stretch x Fe max Retsch Technology x length x stretch x cmin 2 X length = ( ) ( x ) 2 x X stretch = Fe max c min A x cmin A x c min

87 Diameter 1 and Diameter 2 Quadralobe Extrudates Q3 [%] Extrudate Diameters q3 [%/mm] D D 2 Extrudate Length L Retsch Technology CoMo2-Diameter_xc_min_001.rdf 40 CoMo2-Length_xFemax_001.rdf x [mm]

88 length measurement methods without and with flexible guidance sheet (sample director) Without Guidance Sheet Q3 [%] Rod 2mm_1-1 B_xFemax_002.rdf Rod 3mm_1-1 B_xFemax_002.rdf Rod 4mm_1-1 B_xFemax_002.rdf Rod 5mm_1-1 B_xFemax_002.rdf Rod 7mm_1-1 B_xFemax_002.rdf Rod 9mm_1-1 B_xFemax_002.rdf length measurement for non orientated minipellets correct length short length x [mm] Retsch Technology With Guidance Sheet Q3 [%] length measurement for orientated rods + extrudates Rod 2mm_1-3 B_LB_xFemax_001.rdf Rod 3mm_1-3 B_LB_xFemax_001.rdf 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 correct length x [mm]

89 Old Measurement of EPP Minipellets Separator Retsch Technology

90 Old Measurement System of Minipellets Retsch Technology Separator and Balance

91 Applications - EPP Expanded Polypropylene pre expanded beads minipellets Retsch Technology

92 Applications - EPP EPP Expandable Polypropylene Retsch Technology Car bumpers Car bumpers

93 CAMSIZER length measurements for elongated particles (extrudates) correct length short length x Fe max x Fe max x Fe max Ø2mm φ x Fe max Retsch Technology X length = x length x cmin 2 ( x ) ( x ) 2 Fe max c min

94 length measurement without guidance sheet (sample director) q3 [%/mm] q3 [%/mm] Kaneka_160H_Z_1%-mit-Ausblndng099_xFemax_002.rdf Z-Ausbl-conv H-1-3Part_xFemax_002.rdf Z-Ausbl-conv H-1-3Part_xFemax_001.rdf short length correct length correct length x [mm] x [mm] Retsch Technology Right side of distribution

95 Size, Shape and Density Measurement of Beads Retsch Technology

96 Applications Pharmaceuticals Length + Diameter of Implants Length measurement x length ~ 26mm Diameter measurement Ø ~ 0.85mm Retsch Technology validation and test 1. with plastic and 2. steel cylinders measurements of produced implants

97 Applications Pharmaceuticals Reference particles Calibration validation with steel rods of the same dimensions as particles implant reticles Retsch Technology reticles of short extrudates to homogenise the product reticle implant

98 Applications Pharmaceuticals Measuring Implants Flexible guidance sheet (sample director, feed guide) feeder Retsch Technology better extrudate dispersion/ feeding with moving sheet

99 Applications Pharmaceuticals Sugar Spheres Pellets are a multi-particle, solid form of medication. The individual pellets are almost spherical with diameters usually between 100 µm and 2000 μm. Retsch Technology Their history is related to two important development trends in pharmaceutical technology: the hard gelatine capsule as an alternative to tablets, and biopharmacy and its concept of modified release.

100 Applications Pharmaceuticals Control the agglomerates with d 90 / x 90 Single Retsch Technology Agglomerate agglom single Agglomerate

101 Applications Pharmaceuticals Fluidized Bed Granulation Retsch Technology Top-Spray Bottom-Spray Tangential-Spray

102 Applications Pharmaceuticals Multi-particulates Inert Core Drug + Binder Polymer Coating Drug release Sugar Sphere Sugar Sphere Plus Drug Layer Retsch Technology Sugar Sphere Plus Drug Layer Plus Polymer Layer Ghost After Dissolution, Expansion Noticeable

103 Applications Pharmaceuticals measuring shadows Zoom Basic Retsch Technology

104 Applications Pharmaceuticals Size and shape Retsch Technology

105 Applications Pharmaceuticals Typical data Retsch Technology

106 Applications Pharmaceuticals Drug layering Retsch Technology

107 Applications Pharmaceuticals Measuring coat thickness Retsch Technology

108 Investigating drug release Retsch Technology Polymer insoluble Swelling and stretching Coat thickness effects Core dependent Temperature independent Media dependent

109 Coat thickness and swelling Retsch Technology

110 Content Device 1. Measuring Principle 2. Measurement Results Retsch Technology Application 3. Areas of Application 4. Competing Measuring Methods

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