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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.
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©Re
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-1 Speaker: Dipl.-Ing. Gert Beckmann
Retsch Technology GmbH
Host: Ian TreviranusHORIBA Scientific Inc.
CAMSIZER
CAMSIZER®Dynamic Image Analysis
ISO 13322-2 conform
Catalyst Beads, Powders, ExtrudatesPresentation
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Catalysts
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CAMSIZER & CAMSIZER XT
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• Instead of size measurement with sieve shaker or roller graderand 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 (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
Benefits for the Catalyst Industry using the CAMSIZER®
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Measuring PrincipleMeasuring Principle
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CCD-Basic-Image and Particles
CAMSIZER for Extrudated Catalysts
Falling direction
Feeder
Measuring Principle
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Evaluation of the Results
© Retsch Technology GmbH
Measuring Principle
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Two-Camera-System
Basic-Camera
Measuring Principle
Zoom-Camera
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Particle SizeMeasurement Results
xcmin
xc min
“width”
A
A‘ = A
x are
a
“diameter overprojection surface”
xarea“length”
xFe max
xFemax
CAMSIZER results are
compatible with
sieve analysis
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Comparison of Size Definitions
differentsize definitions
differentresults
xcmin xArea xFemax
Measurement Results
x [mm]0.2 0.4 0.6 10
10
20
30
40
50
60
70
80
Q3 [%] Sample A_Basic_0.2%_xc_min_001.rdfSample A_Basic_0.2%_x_area_001.rdfSample A_Basic_0.2%_xFemax_001.rdf
2 x[mm]
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xc min
width
xc min
xc min
leng
th
x Fe
max
Q3 ellipsoid
ellip
soid
-vol
ume
min2
maxellipsoid 6V cFe xx
width
Ellipsoid model leads to better results
Measurement Results
Volume Definition
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Roller Graders
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See and Show Small Differences
(Product 1, 2 and 3)
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See and Show Small Differences (3, 4, 5 and 6)
x_area [mm]1.40 1.45 1.50 1.55 1.60 1.65 1.700
100
200
300
400
500
600
700
q3 [%/mm] 3_15mm_LB_B-x_area_004.rdf4_15mm_LB_B-x_area_005.rdf5_15mm_LB_B-x_area_007.rdf6_15mm_LB_B-x_area_009.rdf7_15mm_LB_B-x_area_010.rdf8_15mm_LB_B-x_area_011.rdf9_15mm_LB_B-x_area_012.rdf0_15mm_LB_B-x_area_003.rdf
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CAMSIZERfor elongated particles (extrudates)
xMa min
xc min
x Fe
max
A/2
A/2
xMa min
2A
2A
Measuring Principle
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x [mm]1 2 4 100
10
20
30
40
50
60
70
80
90
Q3 [%]
0
20
40
60
80
100
120
140
160
180
q3 [%/mm]CoMo2-0,1%Absch_xc_min_001.rdfCoMo2-0,1%Absch_xFemax_001.rdf
Length and Width definitionsfor elongated extrudates
Measurementg Results
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xlength
Xlength =
Xstretch =
Length measurement Extrudates
xFe min
xc min
xMa min
xFe max
xFe min
xc min
xMa min
xFe max
xlength
xstretchxstretch
A/2
A/2
A
Area/Diameter
Pythagoras
Particle Size of Extrudates
Limits xlength > xMa min
Limits xstretch > xMa min
minMaxA
2min2
max MaFe xx
Xlength is the best length for extrudates
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xstretch
xFe min
xc min
xMa min
xFe max
Particle Size of Extrudates
xFe min
xc min
xMa min
xFe max
Xstretch = minMax
A
xstretch
A
area/diameter
xMa min
is bestdiameter
forextrudates
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Diameters and LengthQuadralobes
x [mm]0.4 1 2 4 100
10
20
30
40
50
60
70
80
90
Q3 [%]
0
20
40
60
80
100
120
140
160
180
q3 [%/mm]
CoMo2-Diameter_xc_min_001.rdfCoMo2-Length_xFemax_001.rdf
Extrudate LengthL
Extrudate Diameters
D1
D2
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xFe max xlength xstretch
xMa min
xFe max
xlength
Axstretch
Xlength = Xstretch =
xMa min
CAMSIZER® length definitionsfor elongated particles (extrudates)
Ma minxA22
max Ma minFe xx
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xFe max xlength xFe rec
xMa min
x Fe
rec =
xle
ngth
CAMSIZER® length definitionsfor elongated particles (extrudates)
xMa min
x Fe
rec
= x
leng
th
xMa min
x Fe
rec
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Reference ParticlesCalibration validation with steel rods of
the same dimensions as particles
reticle implant
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Reference Particles
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Reference Particles
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CCD-Basic-Image and Particles
CAMSIZER for Extrudated Catalysts
Falling direction
Feeder
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CCD-Basic-Image and Particles
CAMSIZER for Extrudated Catalysts
Falling direction
Feeder
Motorized Feed Guide orients the extrudates
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Length + Diameter of Implants
Length measurement xlength ~ 26mm
Diameter measurement Ø ~ 0.85mm
validation and test 1. with plastic and 2. steel cylinders
measurements of produced
implants (release time 1month)
Applications – Pharmaceuticals
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x [mm]1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.80
10
20
30
40
50
60
70
80
90
Q3 [%]
0
20
40
60
80
100
120
140
160
180
q3 [%/mm]
CoMo2-0,1%Absch_xc_min_001.rdf
x1 max x2 max
CAMSIZER® width definitionsfor elongated bended extrudates
x1 max
x2 max
Quadralube Diameters
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x [mm]1 2 3 4 5 6 70
10
20
30
40
50
60
70
80
90
Q3 [%]
0
50
100
150
200
250
300
350
400
450
q3 [%/mm]
RT647_602_Z_LB_0.3%_xc_min_001.rdfRT647_602_Z_LB_0.3%_x_len_001.rdf
x [mm]1 2 3 4 5 6 70
10
20
30
40
50
60
70
80
90
Q3 [%]
0
50
100
150
200
250
300
350
400
450
q3 [%/mm]
RT647_600_Z_LB_0.3%_xc_min_001.rdfRT647_600_Z_LB_0.3%_x_len_002.rdf
Diameter 1 ~ “xmax 1”, Dia 2 ~ “xmax 2”
Quadralobes
xmax = volume based Dia = number based
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diameterd
width of equilateral trilobew
heig
ht o
f equ
ilate
ral t
rilob
e
h
iwinner width of trilobe
inne
r hei
ght
ih diameterd
width of trilobew
heig
ht o
f tril
obe
h
iwinner width of trilobe
inne
r hei
ght
ih
It’s possible to recalculate the height from the width and the diameter of an equilateral trilobe (one peak in the q3frequency 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%)
diww
iwdw
dihh
iwih /60sin
ihiw 60sindiwh 60sin
ddwh 60sin ddwh 866.0
ddwh 866.0866.0134.0866.0 dwh
Symmetrical Regular Trilobes
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diameterd
lw
shor
test
hei
ght
of a
n is
osce
les o
r eq
ual-s
ided
trilo
be
sh
liw
shor
ter
inne
r hei
ght
sih
longest width of an isosceles or equal-sided trilobe
longest inner width of an isosceles / equal-sided trilobe
dsihsh
dliwlw
dsiwsw
222
2liwsihsiw
dliwsiwsh
22
2
ddlwdswsh
2
2
2
It’s possible to recalculate the height from the width and the diameter of a non equilateral trilobe (two peaks in the q3frequency distribution).For this you need the result values of the two peaks and the diameter of the lobes.
Irregular Trilobes
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x [mm]1 2 3 4 5 6 7 80
10
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30
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50
60
70
80
90
Q3 [%]
Rod 2mm_1-3 B_LB_xFemax_001.rdfRod 3mm_1-3 B_LB_xFemax_001.rdfRod 4mm_1-3 B_LB_xFemax_001.rdfRod 5mm_1-3 B_LB_xFemax_001.rdfRod 7mm_1-3 B_LB_xFemax_001.rdfRod 9mm_1-3 B_LB_xFemax_001.rdf
x [mm]1 2 3 4 5 6 7 8 90
10
20
30
40
50
60
70
80
90
Q3 [%]Rod 2mm_1-1 B_xFemax_002.rdfRod 3mm_1-1 B_xFemax_002.rdfRod 4mm_1-1 B_xFemax_002.rdfRod 5mm_1-1 B_xFemax_002.rdfRod 7mm_1-1 B_xFemax_002.rdfRod 9mm_1-1 B_xFemax_002.rdf
Without Guidance Sheet
With Guidance Sheet
length measurementfor orientated rods + extrudates
length measurementfor non orientated minipellets
correct length
short length
correct length
length measurement methodswithout and with motorized feed guide (sample director)
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Length measurementwithout guidance sheet (sample director)
Short Catalyst Carriers
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φ
Ø 2mm
Xlength =
xMa min
x len
gth
x Fe
max
correct length short length
CAMSIZER® length measurementsfor elongated particles (extrudates)
22max Ma minFe xx
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x [mm]1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.00
20
40
60
80
100
120
q3 [%/mm]
Kaneka_160H_Z_1%-mit-Ausblndng099_xFemax_002.rdf
x [mm]1.0 1.5 2.0 2.5 3.0 3.50
50
100
150
200
q3 [%/mm]
Z-Ausbl-conv0985-160H-1-3Part_xFemax_002.rdfZ-Ausbl-conv0985-200H-1-3Part_xFemax_001.rdf
Right side of distribution
correct lengthshort lengthcorrect length
Length Measurementwithout feed guide (sample director)
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Shape MeasurementShort Catalyst Carriers
Sharp Rounded
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• width/length =aspect ratio
• Roundness
• Symmetry
• Convexity
xFe max
xc min
A P
r1
r2
S
A convex
A real
Particle ShapeMeasurement Results
maxFe
minc
xx
PA2
4
2
1
rrmin1
21
convex
real
AA
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CAMSIZER - Advantages
• measurement range 30µm – 30mm• easy operation• very direct particle definition
- via particle width (analogue to sieving)- via particle length- or projection surface
• insensitive, maintenance-free, robust• particle shape- density measurement, counting of
particles• high density of information
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Online-Applications
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Online Application (Process Control)
Typical on-line arrangement
Process
LIMS System
Part of SamplePartial flow
Controlled variable
Manipulated variable
Control center
Online Application Control Circuit
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• Double Housing• Industrial PC• UPS (uninterruptable
power supply)• 4-20mA interface• Profibus interface• Analogue + digital I/O• Automatic cleaning• Lab or
test measurements possible
CAMSIZER® online (housing open)
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CAMSIZER® OnLine (closed)
• Double safe• Overpressure or
negative pressure• Air condition• Bulk bypass• Remote control or
direct control
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• Dust protected by compressed air
• Air condition• Funnel shaker• Automatic
cleaning• Remote control• Communication
tests with portable PC
CAMSIZER® Online (housing closed)
sample entrance and funnel
portable PC. Only used during installation and testing of interfaces
light signals are showing the operation status
funnel shaker
CAMSIZER-online (final check at manufacturer)
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Automatic Sampling from a Pipe
sampling
sample dividing
pipeline to the CAMSIZER®
product stream to big bag
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Customized sample feeding solution
• Automatic sampling(from right)
• Manual sampling(on the left)
• Level control
• Dust protection
• Vacuum (negativepressure)
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Online applications with automatic sample taking
sample frompipe
sample from pipe
sample from beltsample from pipe
Applications – Enzymes and Coal
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• Air filters
• Exhaustion
• Cleaning
• Ionisation
CAMSIZER online Dust protection / Ionization
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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
o Supplementary data export to LIMS
o Task file configuration
o Calibration
o Service
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CAMSIZER Application Fields
• Quality laboratories
• Industrial environment locations
• Research and development / Universities
• Automatic process control and interaction
Field installations for CAMSIZER®
• Catalysts• Extrudates• Sand, Refractory• Glass• Ceramics• Coal• Plastics• Food
• Metal powders• Drugs• Carbon black• Salt• Abrasives• Detergents• Sugar• Fertilizer
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End
Thank you for your attention!
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Sphere 1
Sphere 2
Falling Direction
Counting with CAMSIZER®
Correct Particle Counting possible with CAMSIZER
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CCD-Basic-Image and Particles
CAMSIZER for Extrudated Catalysts
Falling direction
Feeder
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Feeder, CCD-Basic-image and particles in reality
particles counted and measured
particles not counted and
not measured
CAMSIZER for Counting
Falling direction
