Introduction to the CAMSIZER XT
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Transcript of Introduction to the CAMSIZER XT
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CAMSIZER XT - the latest in Dynamic Image Analysis
WebinarWednesday, 14th of September 2011
Speaker: Gert BeckmannRetsch Technology GmbH
Host: Ian TreviranusHORIBA Instruments International
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2© Retsch Technology GmbH
History of Retsch Technology GmbH
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Content
InstrumentInstrument
1.1. Measurement Measurement principleprinciple
2.Results
Applications
3.Markets and applications
4.Alternative analysis methods
3© Retsch Technology GmbH
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Comparison between Static Dynamic Image Analysis
4© Retsch Technology GmbH
ISO 13322-1 ISO 13322-2
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CCD - Basic CCD - ZoomDetection of particles
One pixel is element of a projection when at least half of the pixelis covered.
Measurement principle
Resolution
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Dispersion Modules
6© Retsch Technology GmbH
Particle Size Range from 1µm to 3mm
Three modes in 2 modules (dry and wet): X-Fall: for dry and free flowing particlesX-Jet: air pressure dispersion for fine and agglomerated powdersX-Flow: wet module for emulsions and suspensions,
with ultrasonic probe, optional for organic solvents
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Modular "X-Change" Concept
7© Retsch Technology GmbH
Flexible configuration for a wide application range
simple • safe • fast
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Dispersion Modules
8© Retsch Technology GmbH
Dry Dispersion Inserts (2 Plug-In Options)
X- Fall (Gravity dispersion)
X-Jet (Air pressure dispersion)
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Dispersion Modules
9© Retsch Technology GmbH
Dry Dispersion with X-Jet
Measurement range from 1µm to 1.5mm
For fine powders and agglomerating materials
Dry Dispersion by pressurized air: pressure range from 0.2bar to 4.5bar,
3psi – 66psi
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Measurement principle – X-Jet
10© Retsch Technology GmbH
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11© Retsch Technology GmbH
xc_min [µm]50 100 150 200 250 300 3500
10
20
30
40
50
60
70
80
90
Q3 [%]
lactose-20kPa_xc_min_009.rdflactose-30kPa_xc_min_010.rdflactose-50kPa_xc_min_011.rdflactose-100kPa_xc_min_012.rdflactose-150kPa_xc_min_005.rdflactose-200kPa_xc_min_006.rdflactose-300kPa_xc_min_007.rdflactose-460kPa_xc_min_008.rdf
Measurement results with – X-Jet
20, 30 and 50kPa air pressure => stable results / particles don‘t break
100, 150, 200, 300,
460kPa =>
particles break
Lactose Powder
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12© Retsch Technology GmbH
Results of Tin and Lead Solder Powder
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)
xc_min [µm]10 15 20 25 30 35 40 45 500
10
20
30
40
50
60
70
80
90
Q3 [%]
0
1
2
3
4
5
6
7
8
9
q3 [%/µm]
Solder-Powder-#8-X-Jet-30kPa_vvv_xc_min_Mv.rdfSolder-Powder-#8-X-Jet-30kPa_TP1_vvv_xc_min_001.rdfSolder-Powder-#8-X-Jet-30kPa_TP2_vvv_xc_min_002.rdfSolder-Powder-#13-X-Jet-30kPa_TP1_vvv_xc_min_001.rdfSolder-Powder-#13-X-Jet-30kPa_TP2_vvv_xc_min_002.rdfSolder-Powder-#13-X-Jet-30kPa_vvv_xc_min_Mv.rdfSolder-Powder-#27-X-Jet-30kPa_TP1_vvv_xc_min_001.rdfSolder-Powder-#27-X-Jet-30kPa_TP2_vvv_xc_min_002.rdfSolder-Powder-#27-X-Jet-30kPa_vvv_xc_min_Mv.rdf
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Measurement principle – X-Fall
13© Retsch Technology GmbH
Measurement range from 10µm to 3mm
For free flowing materials
similar to standard CAMSIZER
Sample recovery after analysis
• Complete sample recovery
• No contamination
Dry Dispersion with X-Fall
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Measurement principle – X-Fall
14© Retsch Technology GmbH
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Measurement principle – X-Flow
15© Retsch Technology GmbH
Measurement range from 1 µm to 600 µm for emulsions and suspensions
stronger dispersion with ultrasonic module
Optional for organic solvents
Wet Dispersion with X-Flow
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Measurement principle – X-Flow
16© Retsch Technology GmbH
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17© Retsch Technology GmbH
Pharmaceuticals using Wet Cell
Cancer Pharmaceuticals
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Measurement principle
18© Retsch Technology GmbH
Advanced, patented optics design
Sample flow
Light source 2
Light source 1
Basic Camera
Zoom Camera
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Measurement principle
19© Retsch Technology GmbH
Advanced, patented optics design
Sample flow
Light source 2
Light source 1
Basic Camera
Zoom Camera
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Measurement principle
20© Retsch Technology GmbH
Advanced, patented optics design
Sample flow
Light source 2
Light source 1
Basic Camera
Zoom Camera
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Measurement principle
21© Retsch Technology GmbH
Advanced, patented optics design
Sample flow
Light source 2
Light source 1
Basic Camera
Zoom Camera
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22© Retsch Technology GmbH
Features of the CAMSIZER XT
Calibration Reticule
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23© Retsch Technology GmbH
Features of the CAMSIZER XT
Calibration Reticule
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Physical Dynamic Partical Standards
24© Retsch Technology GmbH
Whitehouse Glass Bead Standard XX030for X-Dry and X-Fall
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25© Retsch Technology GmbH
Particle size
Results X-Flow
Particle Size Distribution 2.5µm + 5µm, Wet Dispersion
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X-Change of wet and dry modules in < 1minute
Features of the CAMSIZER XT
26© Retsch Technology GmbH
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Measurement principle
27© Retsch Technology GmbH
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
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Advantages
fast repeatable and reproducible
maintenance free and robust
precise
28© Retsch Technology GmbH
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Content
29© Retsch Technology GmbH
InstrumentInstrument
1.Measurement principle
2.2. ResultsResults
Applications
3.Markets and applications
4.Alternative analysis methods
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Results
30© Retsch Technology GmbH
For agglomerating powders
- Metal powder- Coal dust- Wheat flour
Particle size
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Velocity Adaption
31© Retsch Technology GmbH
When you illuminate the backlight two times within one photo you will see every particle two times on the image
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32© Retsch Technology GmbH
v1
v2
v3
Velocity Adaption
Particles of different size have different speeds
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33© Retsch Technology GmbH
v1s1
v2
v3
s2
s3
Velocity Adaption
Particles of different size move different distances
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34© Retsch Technology GmbH
v1s1
v2
v3
s2
s3
v = s/t
Velocity Adaption
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35© Retsch Technology GmbH
Velocity Adaption
Results with and without velocity adaption
xc_min [µm]100 200 300 400 500 600 700 8000
10
20
30
40
50
60
70
80
Q3 [%]
Pharma-Product-30kPa_xc_min_1.rdfPharma-Product--30kPa_xc_min_2.rdfPharma-Product-30kPa_2_xc_min_4.rdfPharmaProduct-30kPa-VitesseAdaption_xc min_8.rdfPharmaProduct-30kPa-VitesseAdaption_xc min_9.rdfPharma-Product-lot002-tamis-Sieve-Analysis.ref
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Glass Recycling
36© Retsch Technology GmbH
xc_min [µm]20 40 60 80 100 120 140 1600
10
20
30
40
50
60
70
80
90
Q3 [%]
17-12-10_Ausgangsmaterial_kl200µm_30kPa_2mm_F0.3_vvv_x17-12-10_Ausgangsmaterial_kl200µm_30kPa_2mm_F0.3_vvv_x17-12-10_Ausgangsmaterial_kl200µm_30kPa_2mm_F0.3_vvv_x17-12-10_Ausgangsmat_kl200µm_30kPa_2mm_Mahlspalt-100_17-12-10_Ausgangsmat_kl200µm_30kPa_2mm_Mahlspalt-100_17-12-10_Ausgangsmaterial_kl200µm_30kPa_2mm_Mahlspalt-117-12-10_Ausgangsmaterial_kl200µm_30kPa_2mm_Mahlspalt-1
Crushed glass in DM 200 (Retsch Disk Mill)
Different gap settings of the disc mill
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Results X-Jet
37© Retsch Technology GmbH
Sample: PMMA Beads
Detection of oversized particles
8 10 12 140
10
20
30
40
50
60
70
80
90
Q3 [%]
CA10 Feed 450CA10 Feed 450CA10 T18 C 45CA10 T18 C 45CA10 T18F-A 4CA10 T18F-A 4CA10 T18F-B 4CA10 T18F-B 4
Cu
mu
lati
ve D
istr
ibu
tio
n
Particle size [µm]
4 Samples:RedGreenBlueViolet
xc_min [µm]13 14 15 16 17 18
99.0
99.2
99.4
99.6
99.8
100.0
Q3 [%]
CA10 Feed 450kpa_xc_min_av.rdfCA10 T18F-B 450kpa_xc_min_av.rdfCA10 T18 C 450kpa_xc_min_av.rdfCA10 T18F-A 450kpa_xc_min_av.rdf
∆ ~ approx 0.5% Vol.
Red with oversized particlesGreen without oversizeBlue with oversized particlesViolet without oversize
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Results X-Jet
38© Retsch Technology GmbH
Identical results to sieve analysis
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Results X-Jet
39© Retsch Technology GmbH
xMa_min [µm]1 2 4 60
5
10
15
20
q3 [%/µm]
PR6 SIKA 4_xMamin_011.rdfPR6 SIKA 4_xMamin_010.rdf
Sample: SiC At the lower resolution limit ........
Particle Size Distribution 1µm -10µm, Dry Dispersion
Particle size
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40© Retsch Technology GmbH
xc_min [µm]2 4 6 8 10 12 140
5
10
15
20
25
q3 [%/µm]
Duke10um12um_gl0_xc_min_009.rdfDuke10um12um_gl0_xc_min_010.rdfDuke10um12um_gl0_xc_min_011.rdf
Particle Size Distribution 10µm + 12µm, Wet Dispersion
Results X-Flow (Calibration)
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xc_min [µm]4 6 8 10 120
5
10
15
20
25
30
35
40
45
50
q3 [%/µm]
Duke10um12um_gl0_xc_min_009.rdfDuke10um12um_gl0_xc_min_010.rdfDuke10um12um_gl0_xc_min_011.rdfDuke10um_xc_min_002.rdfDuke10um_xc_min_003.rdfDuke10um_xc_min_004.rdf
41© Retsch Technology GmbH
Particle size
Results X-Flow (Calibration)
Particle Size Distribution 10µm + 12µm, Wet Dispersion
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Results X-Jet
42© Retsch Technology GmbH
Better Size Analysis due to Understanding of Particle Shape:Length, Width, Average Diameter
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Shape Analysis with CAMSIZER XT
43© Retsch Technology GmbH
area of the particle
perimeter of the particle
circle with same area as particle
diameter of circle of
same area
2
4P
ASPHT
max
min
Fe
c
xx
lw
lb
b/l0.4 0.5 0.6 0.7 0.80
10
20
30
40
50
60
70
80
90
Q3 [%]
Pharma-Product-1-30kPa-bonne-forme-_xc_min_009.rdfPharma-Product-1-30kPa_Vitesse-Adaption_xc_min_008.rdflactose-30kPa_xFemax_003.rdfPharma-Product-2-460_xc_min_008.rdf
SPHT0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.90
10
20
30
40
50
60
70
80
90
Q3 [%]
Pharma-Product-1-30kPa-bonne-forme-_xc_min_009.rdfPharma-Product-1-30kPa_Vitesse-Adaption_xc_min_008.rdflactose-30kPa_xFemax_003.rdfPharma-Product-2-460_xc_min_008.rdf
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Results X-Flow
44© Retsch Technology GmbH
b/l0.4 0.5 0.6 0.7 0.8 0.90
10
20
30
40
50
60
70
80
90
Q3 [%]
A32L 2__xc_min_001.rdfA32L 2__xc_min_002.rdfA32L 2__xc_min_003.rdfA32L 2__xc_min_004.rdfA32L 2__xc_min_005.rdf
Shape analysis for detection of broken particles:„What you see is what you get“
broken round
Length and shape numbers for single particles, from real pictures
Precise analysis of the amount of broken particles by shape
detection
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Sample: Glass beads, multimodal
Results X-Fall
45© Retsch Technology GmbH
Excellent repeatabilty and detection efficiency for „large particles“ and small sample volumes
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• Digital image processing with patented 2-camera system (ISO 13322-2)
• 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
Advantages
46© Retsch Technology GmbH
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Content
47© Retsch Technology GmbH
Instrument
1.Measurement principle
2.Results
ApplicationsApplications
3.3. Markets and applicationsMarkets and applications
4.Alternative analysis methods
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• Industrial labs
• Research institutes
• Production control
• Quality control for final products
• Quality control of incoming raw materials
• Immediate control and optimisation of
production processes
Application areas
48© Retsch Technology GmbH
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Application areas
49© Retsch Technology GmbH
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
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Content
50© Retsch Technology GmbH
Instrument
1.Measurement principle
2.Results
ApplicationsApplications
3.Markets and applications
4.4. Alternative analysis methodsAlternative analysis methods
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Alternative Methods
51© Retsch Technology GmbH
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Alternative Methods
52© Retsch Technology GmbH
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Sieving CAMSIZER XTSize range 10µm - 63mm 1µm – 3mmShape analysis no yesDetection 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 „difficult“ superior
Comparison with sieving identical results possible
Handling simple, but time consuming easy and fast
Sieving CAMSIZER XT
53© Retsch Technology GmbH
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Results X-Jet
54© Retsch Technology GmbH
Identical results to sieve analysis
xc_min [mm]0.1 0.2 0.3 0.4 0.5 0.6 0.70
10
20
30
40
50
60
70
80
90
Q3 [%]
Ca-hydrogenphosphate_100kPa-T38567-vvv_xc_min_005.rdfCa-hydrogenphosphate_100kPa-T38567-vvv_xc_min_003.rdfCa-hydrogenphosphate_100kPa-T38567-vvv_xc_min_004.rdfT38567-Sieve-Analysis-Customer-Site.ref
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55© Retsch Technology GmbH
Sieving CAMSIZER XT
Spheroidal Particles
x [µm] 200 400 600 800 1000 1200 0
10
20
30
40
50
60
70
80
90 Passing [%]
Sample-1__xc_min_002.rdf Sample-1__xc_min_001.rdf Sieving-Nominal-S1.ref
xc min = = d = Xc min
particle-width
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56© Retsch Technology GmbH
Sieving CAMSIZER XT
Influence of Mesh Width
1400µm 1400µm 1429.5µm
Mesh sizes warpMesh sizes weft
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. 03033531 (nominal 1400µm)
Theory: Reality:
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57© Retsch Technology GmbH
Sieving CAMSIZER XT
Real Mesh Width
x [µm] 200 400 600 800 1000 1200 0
10
20
30
40
50
60
70
80
90 Passing [%]
Sample-1__xc_min_002.rdf Sieving-upper-range-S1.ref
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58© Retsch Technology GmbH
Sample Reproducibility of CAMSIZER XT measurements of xc min (red, and blue) with Basic + Zoom or Zoom only, Retsch sieve result (real mesh sizes from optical inspection) AS 200 TAB (*black), Customer nominal sieve results (*blue)
Results of Tin and Lead Solder Powder
xc_min [µm]10 20 30 40 500
10
20
30
40
50
60
70
80
90
Q3 [%]Solder_Sample_G_xc_min_001.rdfSolder_Sample_G_xc_min_002.rdfSolder_Sample_G_xc_min_003.rdfTin-Solder_Sample_G__xc_min_001.rdfTin-Solder_Sample_G__xc_min_002.rdfTin-Solder_Sample_G__xc_min_003.rdfRT1763 Sieve-Analysis G customer-site-nominal.refRT1763 Sieve-Analysis_G_AS200tap_real-sizes.ref
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59© Retsch Technology GmbH
Glass Recycling
Crushed GlassSimilar results to sieve analysis
xc_min [µm]20 40 60 80 100 120 1400
10
20
30
40
50
60
70
80
90
Q3 [%]
17-12-10_smaller 50µm-white_30kPa_2mm_vvv_xc_min_002.rdf15-12-10_smaller 50µm-white-Lab_30kPa_2mm_vvv_xc_min_001.rdfRT1798_Customer-Sieve -Analysis smaller 50µm_white_Ha.ref
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Applications: Metal powdersMaterial: Cu
60© Retsch Technology GmbH
Identical results to the sieve analysis
xc_min [mm]0.04 0.1 0.2 0.4 1 20
10
20
30
40
50
60
70
80
90
Q3 [%]
Automatic reports,many languages
available
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61© Retsch Technology GmbH
x [mm]0.2 0.4 0.6 10
10
20
30
40
50
60
70
80
Q3 [%]
Sample A_BZ_0.2%_xc_min_001.rdfSample A_.ref
Digitale Imaging Sieving
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62© Retsch Technology GmbH
Glass Recycling
Very Acicular and Angular Particles
without and with Elementary Fitting
xc_min [µm]100 200 300 400 500 6000
10
20
30
40
50
60
70
80
90
Q3 [%]
15-12 50-100µm-gray_30kPa_2mm_vvv_xc_min_001.rdfRT1798_Customer-Sieve-Analysis_50-100µm_gray.ref
xc_min [µm]100 200 300 400 5000
10
20
30
40
50
60
70
80
90
Q3 [%]
15-12 50-100µm-gray_30kPa_2mm_vvv_xc_min_001.rdfRT1798_Customer-Sieve-Analysis_50-100µm_gray.ref
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CAMSIZER XT Laser sizer
63© Retsch Technology GmbH
Laser sizer CAMSIZER XTSize range down to 20nm > 1µmShape analysis no yesDetection of oversized particles percent range few big particles
< 0.1% Vol.
Resolution good for fines better resolution for large particles
Multi-modal distributions more difficult better volume model, better size resolution
Comparison with sieving not possible identical results
Information content black box + mathematics pictures
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Results X-Jet
64© Retsch Technology GmbH
200 400 600 800 1000 1200 14000
10
20
30
40
50
60
70
80
90
Q3 [%]
PR1 10089 Grov_xMamin_001.rdfRT1686_Elkem1_sieb.refRT1686 1089 coarse M2000.ref
Sample: Petrolcoke for Electrodes
Reliable results, closer to sieving
Particle size [µm]
Cum
ulat
ive
Dis
tribu
tion
CAMSIZERSievingLaser diffraction (customer results)
100 200 300 400 500 600 700 8000
10
20
30
40
50
60
70
80
90
Q3 [%]
PR4 10086 Grov Senter_xMamin_0RT1686 10086 coarse ELKEM.refRT1686_Elkem4_sieb.ref
CAMSIZERSieving (Retsch AS200)Sieving (customer results)
Particle size [µm]
Cum
ulat
ive
Dis
tribu
tion
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CAMSIZER XT Optical Microscope
65© Retsch Technology GmbH
Microscope CAMSIZER XTSize range 0.5 – 500 µm 1 µm -3 mm
Shape analysis yessuperior image quality yes
Detection of oversized particles no few big particles
< 0.1% Vol.Resolution better good
Statistics Low,few 1,000 particles million particles/minute
Comparison with sieving not possible identical results possible
Handling time consuming fastRepresentative Sample Amounts
difficult, only narrow distributions
yes, small and large amounts
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66© Retsch Technology GmbH
CAMSIZER XT Optical Microscope
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67© Retsch Technology GmbH
xc_min [µm]200 400 600 800 10000
10
20
30
40
50
60
70
80
90
Q3 [%]
PPO-646_xc_min_001.rdfRT1766_ppo646_sieve.ref
CAMSIZER XT Optical Microscope
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68© Retsch Technology GmbH
CAMSIZER XT CAMSIZER
CAMSIZER CAMSIZER XTSize range 30 µm – 30mm 1 µm -3 mmShape analysis yes yesDetection of oversized particles yes yes
Images / second 60 277Resolution CCD-Cameras 790,000 1,300,000
Comparison with sieving identical results possible
identical results possible
Handling fast fastRepresentative Sample Amounts
yes, small and large amounts
yes, small and large amounts
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69© Retsch Technology GmbH
Comparison of CAMSIZER and CAMSIZER XT
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.
Results of Tin and Lead Solder Powder
xc_min [µm]15 20 25 30 35 40 45 500
10
20
30
40
50
60
70
80
90
Q3 [%]
Solder-XT-with-X-Jet-#30-Einzel-250kPa_xc_min_005.rdfSolder-XT-with-X-Jet-#30-Einzel-250kPa_xc_min_006.rdfSolder-XT-with-X-Jet-#30-Einzel-250kPa_xc_min_007.rdfSolder-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
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Thank you for your attention!