CAMSIZER XT - the latest in Dynamic Image Analysis

Transcription

1 CAMSIZER XT - the latest in Dynamic Image Analysis Webinar Wednesday, 14 th of September 2011 Speaker: Gert Beckmann Retsch Technology GmbH Host: Ian Treviranus HORIBA Instruments International

2 History of Retsch Technology GmbH 2

3 Content Instrument 1. Measurement principle 2. Results Applications 3. Markets and applications 4. Alternative analysis methods 3

4 Comparison between Static Dynamic Image Analysis ISO ISO

5 Measurement 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

6 Dispersion Modules Particle Size Range from 1µm to 3mm Three modes in 2 modules (dry and wet): X-Fall: for dry and free flowing particles X-Jet: air pressure dispersion for fine and agglomerated powders X-Flow: wet module for emulsions and suspensions, with ultrasonic probe, optional for organic solvents 6

7 Modular "X-Change" Concept Flexible configuration for a wide application range simple safe fast 7

8 Dispersion Modules Dry Dispersion Inserts (2 Plug-In Options) X- Fall (Gravity dispersion) X-Jet (Air pressure dispersion) 8

9 Dispersion Modules Dry Dispersion with X-Jet Measurement range from 1 µm to 1.5 mm For fine powders and agglomerating materials Dry Dispersion by pressurized air: pressure range from 0.2 bar to 4.5 bar, 3psi 66psi 9

10 Measurement principle X-Jet 10

11 Measurement results with X-Jet Q3 [%] , 150, 200, 300, 460kPa => particles break Lactose Powder lactose-20kpa_xc_min_009.rdf lactose-30kpa_xc_min_010.rdf lactose-50kpa_xc_min_011.rdf lactose-100kpa_xc_min_012.rdf lactose-150kpa_xc_min_005.rdf lactose-200kpa_xc_min_006.rdf lactose-300kpa_xc_min_007.rdf lactose-460kpa_xc_min_008.rdf , 30 and 50kPa air pressure => stable results / particles don t break xc_min [µm] 11

12 Results of Tin and Lead Solder Powder Q3 [%] q3 [%/µm] 9 Solder-Powder-#8-X-Jet-30kPa_vvv_xc_min_Mv.rdf Solder-Powder-#8-X-Jet-30kPa_TP1_vvv_xc_min_001.rdf Solder-Powder-#8-X-Jet-30kPa_TP2_vvv_xc_min_002.rdf 8 Solder-Powder-#13-X-Jet-30kPa_TP1_vvv_xc_min_001.rdf Solder-Powder-#13-X-Jet-30kPa_TP2_vvv_xc_min_002.rdf 7 Solder-Powder-#13-X-Jet-30kPa_vvv_xc_min_Mv.rdf Solder-Powder-#27-X-Jet-30kPa_TP1_vvv_xc_min_001.rdf 6 Solder-Powder-#27-X-Jet-30kPa_TP2_vvv_xc_min_002.rdf Solder-Powder-#27-X-Jet-30kPa_vvv_xc_min_Mv.rdf xc_min [µm] 0 Customer had sent 30 different samples to Retsch Technology but some of these samples were the same (red, blue and green). We found out the groups and showed to the customer the good reproducibility of CAMSIZER XT (and proofed his sample splitting as well) 12

13 Measurement principle X-Fall Dry Dispersion with X-Fall Measurement range from 10 µm to 3 mm For free flowing materials similar to standard CAMSIZER Sample recovery after analysis Complete sample recovery No contamination 13

14 Measurement principle X-Fall 14

15 Measurement principle X-Flow Wet Dispersion with X-Flow Measurement range from 1 µm to 600 µm for emulsions and suspensions stronger dispersion with ultrasonic module Optional for organic solvents 15

16 Measurement principle X-Flow 16

17 Pharmaceuticals using Wet Cell Cancer Pharmaceuticals 17

18 Measurement principle Advanced, patented optics design Sample flow Basic Camera Light source 2 Zoom Camera Light source 1 18

19 Measurement principle Advanced, patented optics design Sample flow Basic Camera Light source 2 Zoom Camera Light source 1 19

20 Measurement principle Advanced, patented optics design Sample flow Basic Camera Light source 2 Zoom Camera Light source 1 20

21 Measurement principle Advanced, patented optics design Sample flow Basic Camera Light source 2 Zoom Camera Light source 1 21

22 Features of the CAMSIZER XT Calibration Reticule 22

23 Features of the CAMSIZER XT Calibration Reticule 23

24 Physical Dynamic Partical Standards Whitehouse Glass Bead Standard XX030 for X-Dry and X-Fall 24

25 Results X-Flow Particle Size Distribution 2.5µm + 5µm, Wet Dispersion Particle size 25

26 Features of the CAMSIZER XT X-Change of wet and dry modules in < 1minute 26

27 Measurement principle Highlights of the optics setup design: More than 275 images per second Full frame cameras with > 1.3 Megapixel resolution Separate light sources for optimised brightness, homogenity, and contrast 2 Cameras: High resolution combined with excellent statistic for a wide dynamic range Image processing in real-time: Each particle in each image is analysed Hundreds of particles in each image: Excellent statistics in short time CAMSIZER XT can measure in a wider dynamic range with better statistics and reproducibility than any other image processing system 27

28 Advantages fast repeatable and reproducible precise maintenance free and robust 28

29 Content Instrument 1. Measurement principle 2. Results Applications 3. Markets and applications 4. Alternative analysis methods 29

30 Results For agglomerating powders - Metal powder -Coal dust - Wheat flour Particle size 30

31 Velocity Adaption When you illuminate the backlight two times within one photo you will see every particle two times on the image 31

32 Velocity Adaption v 1 Particles of different size have different speeds v 3 v 2 32

33 Velocity Adaption s 1 v 1 Particles of different size move different distances s 3 v 3 v 2 s 2 33

34 Velocity Adaption s 1 v 1 v = s/t s 3 v 3 v 2 s 2 34

35 Velocity Adaption Results with and without velocity adaption Q3 [%] Pharma-Product-30kPa_xc_min_1.rdf Pharma-Product--30kPa_xc_min_2.rdf Pharma-Product-30kPa_2_xc_min_4.rdf PharmaProduct-30kPa-VitesseAdaption_xc min_8.rdf PharmaProduct-30kPa-VitesseAdaption_xc min_9.rdf Pharma-Product-lot002-tamis-Sieve-Analysis.ref xc_min [µm] 35

36 Glass Recycling Q3 [%] Crushed glass in DM 200 (Retsch Disk Mill) Different gap settings of the disc mill _Ausgangsmaterial_kl200µm_30kPa_2mm_F0.3_vvv_x _Ausgangsmaterial_kl200µm_30kPa_2mm_F0.3_vvv_x _Ausgangsmaterial_kl200µm_30kPa_2mm_F0.3_vvv_x _Ausgangsmat_kl200µm_30kPa_2mm_Mahlspalt-100_ _Ausgangsmat_kl200µm_30kPa_2mm_Mahlspalt-100_ _Ausgangsmaterial_kl200µm_30kPa_2mm_Mahlspalt _Ausgangsmaterial_kl200µm_30kPa_2mm_Mahlspalt xc_min [µm] 36

37 Results X-Jet Detection of oversized particles Q3 [%] Q3 [%] Cumulative Distribution CA10 Feed 450 CA10 Feed 450 CA10 T18 C 45 CA10 T18 C 45 CA10 T18F-A 4 CA10 T18F-A 4 CA10 T18F-B 4 CA10 T18F-B 4 4 Samples: Red Green Blue Violet CA10 Red Feed with 450kpa_xc_min_av.rdf oversized particles CA10 Green T18F-B without 450kpa_xc_min_av.rdf oversize CA10 Blue T18 with C 450kpa_xc_min_av.rdf oversized particles CA10 Violet T18F-A without 450kpa_xc_min_av.rdf oversize xc_min [µm] ~ approx 0.5% Vol Particle size [µm] Sample: PMMA Beads 37

38 Results X-Jet Identical results to sieve analysis 38

39 Results X-Jet q3 [%/µm] Particle Size Distribution 1µm -10µm, Dry Dispersion 20 PR6 SIKA 4_xMamin_011.rdf PR6 SIKA 4_xMamin_010.rdf Particle size xma_min [µm] Sample: SiC At the lower resolution limit... 39

40 Results X-Flow (Calibration) Particle Size Distribution 10µm + 12µm, Wet Dispersion q3 [%/µm] Duke10um12um_gl0_xc_min_009.rdf Duke10um12um_gl0_xc_min_010.rdf 25Duke10um12um_gl0_xc_min_011.rdf xc_min [µm] 40

41 Results X-Flow (Calibration) Particle Size Distribution 10µm + 12µm, Wet Dispersion q3 [%/µm] Duke10um12um_gl0_xc_min_009.rdf Duke10um12um_gl0_xc_min_010.rdf Duke10um12um_gl0_xc_min_011.rdf Duke10um_xc_min_002.rdf Duke10um_xc_min_003.rdf Duke10um_xc_min_004.rdf Particle size xc_min [µm] 41

42 Results X-Jet Better Size Analysis due to Understanding of Particle Shape: Length, Width, Average Diameter 42

43 Shape Analysis with CAMSIZER XT Q3 [%] Pharma-Product-1-30kPa-bonne-forme-_xc_min_009.rdf Pharma-Product-1-30kPa_Vitesse-Adaption_xc_min_008.rdf lactose-30kpa_xfemax_003.rdf Pharma-Product-2-460_xc_min_008.rdf b l w l x x cmin Femax b/l Q3 [%] area of the particle Pharma-Product-1-30kPa-bonne-forme-_xc_min_009.rdf Pharma-Product-1-30kPa_Vitesse-Adaption_xc_min_008.rdf lactose-30kpa_xfemax_003.rdf Pharma-Product-2-460_xc_min_008.rdf circle with same area as particle perimeter of the particle SPHT 4 A 2 P diameter of circle of same area SPHT 43

44 Results X-Flow Shape analysis for detection of broken particles: What you see is what you get Length and shape numbers for single particles, from real pictures Q3 [%] A32L 2 xc_min_001.rdf A32L 2 xc_min_002.rdf A32L 2 xc_min_003.rdf A32L 2 xc_min_004.rdf A32L 2 xc_min_005.rdf broken round b/l Precise analysis of the amount of broken particles by shape detection 44

45 Results X-Fall Excellent repeatabilty and detection efficiency for large particles and small sample volumes Sample: Glass beads, multimodal 45

46 Advantages Digital image processing with patented 2-camera system (ISO ) wide dynamic range from 1µm to > 3mm newly developed optical system with ultra bright LEDs for sharp contrasts and large depth of focus short analysis time 1 3 minutes for few million particles safe detection of oversized and undersized modules for dry and wet dispersion analysis results optionally compatible to sieve analysis 46

47 Content Instrument 1. Measurement principle 2. Results Applications 3. Markets and applications 4. Alternative analysis methods 47

48 Application areas Industrial labs Research institutes Production control Quality control for final products Quality control of incoming raw materials Immediate control and optimisation of production processes 48

49 Application areas Typical sample materials Pharmaceutical powders, granules or small pellets Pulverized and granulated food, spices Detergents, enzymes, fillers for washing powders Metal or ore powders Abrasives (medium and small grit) Sand and cement, building materials, limestone Fibres 49

50 Content Instrument 1. Measurement principle 2. Results Applications 3. Markets and applications 4. Alternative analysis methods 50

51 Alternative Methods 51

52 Alternative Methods 52

53 Sieving CAMSIZER XT Sieving CAMSIZER XT Size range 10µm - 63mm 1µm 3mm Shape analysis no yes Detection of oversized particles each particle few big particles from < 0.1% Vol. Resolution poor high resolution Multi-modal distributions poor size resolution better resolution Repeatability and lab-to-lab comparison Comparison with sieving Handling difficult superior identical results possible simple, but time consuming easy and fast 53

54 Results X-Jet Identical results to sieve analysis Q3 [%] Ca-hydrogenphosphate_100kPa-T38567-vvv_xc_min_005.rdf Ca-hydrogenphosphate_100kPa-T38567-vvv_xc_min_003.rdf Ca-hydrogenphosphate_100kPa-T38567-vvv_xc_min_004.rdf T38567-Sieve-Analysis-Customer-Site.ref xc_min [mm] 54

55 Sieving CAMSIZER XT Spheroidal Particles Passing [%] Sample-1 xc_min_002.rdf Sample-1 xc_min_001.rdf Sieving-Nominal-S1.ref = d = Xc min x c min = particle-width x [µm] 55

56 Sieving CAMSIZER XT Influence of Mesh Width Mesh sizes warp Mesh sizes weft 1400µm 1400µm µm Theory: Reality: Nominal Sieve Mesh = 1400µm Real Sieve Mesh >1400=1455 only beads < 1400µm will pass the sieve mesh beads > 1400µm will not pass the sieve mesh Upper mesh size range ~1455µm sieve No (nominal 1400µm) 56

57 Sieving CAMSIZER XT Real Mesh Width Passing [%] Sample-1 xc_min_002.rdf Sieving-upper-range-S1.ref x [µm] 57

58 Results of Tin and Lead Solder Powder Q3 [%] Solder_Sample_G_xc_min_001.rdf Solder_Sample_G_xc_min_002.rdf Solder_Sample_G_xc_min_003.rdf Tin-Solder_Sample_G xc_min_001.rdf Tin-Solder_Sample_G xc_min_002.rdf Tin-Solder_Sample_G xc_min_003.rdf RT1763 Sieve-Analysis G customer-site-nominal.ref RT1763 Sieve-Analysis_G_AS200tap_real-sizes.ref xc_min [µm] Sample Reproducibility of CAMSIZER XT measurements of x c min (red, andblue) with Basic + Zoom or Zoom only, Retsch sieve result (real mesh sizes from optical inspection) AS 200 TAB (*black), Customer nominal sieve results (*blue) 58

59 Glass Recycling Crushed Glass Similar results to sieve analysis Q3 [%] _smaller 50µm-white_30kPa_2mm_vvv_xc_min_002.rdf _smaller 50µm-white-Lab_30kPa_2mm_vvv_xc_min_001.rdf RT1798_Customer-Sieve -Analysis smaller 50µm_white_Ha.ref xc_min [µm] 59

60 Applications: Metal powders Material: Cu Identical results to the sieve analysis Q3 [%] xc_min [mm] Automatic reports, many languages available 60

61 Digitale Imaging Sieving Q3 [%] 80 Sample A_BZ_0.2%_xc_min_001.rdf Sample A_.ref x [mm] 61

62 Glass Recycling Very Acicular and Angular Particles without and with Elementary Fitting Q3 [%] Q3 [%] µm-gray_30kPa_2mm_vvv_xc_min_001.rdf RT1798_Customer-Sieve-Analysis_50-100µm_gray.ref µm-gray_30kPa_2mm_vvv_xc_min_001.rdf RT1798_Customer-Sieve-Analysis_50-100µm_gray.ref xc_min [µm] xc_min [µm] 62

63 CAMSIZER XT Laser sizer Laser sizer CAMSIZER XT Size range down to 20nm > 1µm Shape analysis no yes Detection of oversized particles Resolution Multi-modal distributions percent range good for fines more difficult few big particles < 0.1% Vol. better resolution for large particles better volume model, better size resolution Comparison with sieving not possible identical results Information content black box + mathematics pictures 63

64 Results X-Jet Reliable results, closer to sieving Q3 [%] Cumulative Distribution PR Grov_xMamin_001.rdf RT1686_Elkem1_sieb.ref RT coarse M2000.ref CAMSIZER Sieving Laser diffraction (customer results) Particle size [µm] Q3 [%] Cumulative Distribution CAMSIZER Sieving (Retsch AS200) Sieving (customer results) PR Grov Senter_xMamin_0 RT coarse ELKEM.ref RT1686_Elkem4_sieb.ref Particle size [µm] Sample: Petrolcoke for Electrodes 64

65 CAMSIZER XT Optical Microscope Microscope CAMSIZER XT Size range µm 1 µm -3 mm Shape analysis Detection of oversized particles yes superior image quality no yes few big particles < 0.1% Vol. Resolution better good Statistics Comparison with sieving Low, few 1,000 particles not possible million particles/minute identical results possible Handling time consuming fast Representative Sample Amounts difficult, only narrow distributions yes, small and large amounts 65

66 CAMSIZER XT Optical Microscope 66

67 CAMSIZER XT Optical Microscope Q3 [%] PPO-646_xc_min_001.rdf RT1766_ppo646_sieve.ref xc_min [µm] 67

68 CAMSIZER XT CAMSIZER CAMSIZER CAMSIZER XT Size range 30 µm 30mm 1 µm -3 mm Shape analysis yes yes Detection of oversized particles Images / second Resolution CCD-Cameras 790,000 1,300,000 Comparison with sieving yes identical results possible yes identical results possible Handling fast fast Representative Sample Amounts yes, small and large amounts yes, small and large amounts 68

69 Comparison of CAMSIZER and CAMSIZER XT Results of Tin and Lead Solder Powder Q3 [%] Solder-XT-with-X-Jet-#30-Einzel-250kPa_xc_min_005.rdf Solder-XT-with-X-Jet-#30-Einzel-250kPa_xc_min_006.rdf Solder-XT-with-X-Jet-#30-Einzel-250kPa_xc_min_007.rdf Solder-XT-with-X-Jet-#30-Einzel-250kPa_xc_min_008.rdf #30-classic-CAMSIZER-Repeatability-xc_min_013.rdf #30-classic-CAMSIZER-Repeatability-xc_min_014.rdf #30-classic-CAMSIZER-Repeatability-xc_min_015.rdf #30-classic-CAMSIZER-Repeatability-xc_min_Mv.rdf xc_min [µm] Results of CAMSIZER (black) and CAMSIZER-XT (red) of sample #30 CAMSIZER distribution is wider, the results are not that accurate and repeatable as results from CAMSIZER XT. 69

70 Thank you for your attention!