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-1 HORIBA Scientific & Retsch Technology
CAMSIZER Fertilizer Webinar
November 16th 2011
Host: Ian Treviranus, HORIBA InstrumentsSpeaker: Dipl.-Ing. Gert Beckmann
Retsch Technology GmbH
CAMSIZER
CAMSIZER®
Particle Size and Shape using Dynamic Image Analysis
ISO 13322-2 conform
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Device1. Measuring Principle
2. Measurement Results
Content
Application3. CAMSIZER Applications
in the Fertilizer Industry
4. Competing Measuring Methods
* CAMSIZER measurement principle* Intelligent matching of sieve results* SGN, UI and other calculations* Q & A session
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Development of CAMSIZER &
CRYSTALSIZER
19
99
20
03
20
01
Announcement of
Particle size analyzers in Europe
Development of AutoSampler System
20
02
New shape functions of CAMSIZER,
first Online-Installations
Retsch Technology
20
06
Improvement of CAMSIZER®
with AutoHeight, LED technology, Software, improved resolution,
sharpness and contrast
Development of CAMSIZER XT
for agglomerating powders 1µm-3000µm
History
20
11
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Comparison between Static Dynamic Image Analysis
ISO 13322-1 ISO 13322-2
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Device1. Measuring Principle
2. Measurement Results
Device1. Measuring Principle
- Two Camera-System- Resolution
Content
Application3. CAMSIZER Applications
in the Fertilizer Industry
4. Competing Measuring Methods
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Two-Camera-System
Basic
Zoom
Basic-Camera
Measuring Principle
Zoom-Camera
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CCD - Basic CCD - Zoom
Measuring Principle
Detection of particles
One pixel is element of a projection when at least half of the pixelis covered.
Resolution
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One Camera Setup
Drawback: tight dynamic range
Dynamic Range: xmin to 50 •xmin
Measuring Principle
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CAMSIZER Principle (Two Cameras)
Advantages• Precise full-frame images• Wide dynamic range: 30µm to 30mm
Dynamic Factor:
Measuring Principle
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Content
Device1. Measuring Principle
2. Measurement Results
- Size
- Shape
Application3. CAMSIZER Applications
in the Fertilizer Industry
4. Competing Measuring Methods
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What is the size of this particle?
Measurement Results
Particle Size
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Measuring Principle: Sieving
Sphere
Sti
ck
Coin
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6000100050010050
20
30
40
60
70
80
4.5 g6 g
15 g
30 g
48 g
22.5 g
15 g6 g 3 g
Visualization
45 63 140 250 2000 4000
Cumulative distribution
Particle size x[µm]
Q3 [%]
10
50
90
3%4%
10%
10%
32%
15%
4% 2%
20%
150 g
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6000100010050
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60
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60
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Visualization
Particle size x[µm]
Q3 [%]
10
50
90
p3 [%]
Cumulative distribution
100045 63 140 250 2000 4000500
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6000100010050
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Visualization
Particle size x[µm]
Q3 [%]
10
50
90
p3 [%]
Cumulative distribution
100045 63 140 250 2000 4000500
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6000100010050
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Visualization
Particle size x[µm]
Q3 [%]
10
50
90
p3 [%]
Cumulative distribution
100045 63 140 250 2000 4000500
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6000100010050
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Visualization
Particle size x[µm]
Q3 [%]
10
50
90
p3 [%]
Cumulative distribution
100045 63 140 250 2000 4000500
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6000100010050
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Visualization
Particle size x[µm]
Q3 [%]
10
50
90
p3 [%]
Cumulative distribution
100045 63 140 250 2000 4000500
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6000100010050
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20
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40
50
60
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Visualization
Particle size x[µm]
Q3 [%]
10
50
90
p3 [%]
Cumulative distribution
100045 63 140 250 2000 4000500
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6000100010050
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Visualization
Particle size x[µm]
Q3 [%]
10
50
90
p3 [%]
Cumulative distribution
100045 63 140 250 2000 4000500
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6000100010050
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Visualization
Particle size x[µm]
Q3 [%]
10
50
90
p3 [%]
Cumulative distribution
100045 63 140 250 2000 4000500
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6000100010050
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Q3 [%]
10
20
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50
60
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Q3(36)
250 µm
Particles < 250 µm
Particle size x[µm]
p3 [%]
Visualisierung
Cumulative distribution & FractionsVisualization
100045 63 140 250 2000 4000500
330 µm
Q3( ) Particles < 330 µm
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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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Reproducibility
Calibration with traceable standard
=> Absolute accuracy
Measurement Results
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Whitehouse Standard XX030Calibration Results
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Maintenance-Free byVenturi-Flushing
Features
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Device1. Measuring Principle
2. Measurement Results
Content
Application3. CAMSIZER Applications
in the Fertilizer Industry
4. Competing Measuring Methods
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• laboratories
• next to manufacturing line
• optimized quality control of product and process
• research institutes / universities
Places of Installation
Examples of Applications
Areas of Application
• fertilizer• salt• crop protection• pharmaceuticals• food (human and animals)
••
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Features
Quality Control
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*100
UI and SGN values (Literature)Specific Fertilizer Features
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SGN and UI values also with CAMSIZER
Specific Fertilizer Features
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Analysis of size and shape of
broken granulated coated
fertilizers
CAMSIZER-Advantages FertilizerApplications - Fertilizer
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Different Production Methods, as well as Different Sizes and Shapes
Applications – Fertilizer
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Sample Quantity in Mass or Volume in Relation to the Particle Size
A Sufficient Sample Quantity is Based on the Number of Particles
ISO 13322-1
Sampling and Sample Splitting
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Separation of fine and coarse particles
Separation happens during- Transport processes (container, train and truck)- Feeding processes (funnels, vibration feeders, belts)- and Storage (bulk pile, silo)
Sampling and Sample Splitting
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Separation of fine and coarse particlesSeparation happens because of different sizes
Particles having different sizes
separate
Particles with similar sizes keep homogenety in
mix
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Separation of fine and coarse particles
Segregation (separation by size) happens during- Filling processes (silo)- Feeding processes (bulk pile)- Accumulation of fines in the middle of the pile
Sampling and Sample Splitting
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Dust sticks to particle because of the Coating
Dust Agglomerate
Large Granule
Large Granule with Coating
How to attach small „Dust“ Particles to the larger Granules to get a „better“ Product?
Applications – Fertilizer
Fertilizer producer coats the granules with petrochemical oil and amine to bind the
dust to the granules for better handling to avoid accumulation of dust
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Applications - Fertilizer
Only complete Fertilizing provides good Nutrition
Plant availability
Optimum soil condition
Anything else is wasted money
and pollution
of our environment
Chalk / Calcium
1st fertilizing
2nd fertilizing
potash
nitro
gen
phos
phor
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id
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A German Fertilizer Producer is mining and producing KCl, MgSO4 and KSO4
Before 2000 => Sieve analysis 0.05 – 2.5 mmAfter 2000 => CAMSIZER analysis
Applications – Fertilizer
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Applications – Fertilizer Shaft Mining of Potash KCl
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Applications – Fertilizer Handling of Potash KCl
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Chalk / Calcium
1st fertilizing
2nd fertilizing
potash
nitro
gen
Bulk Blending Companies and Farmers want the Same Size of the Components
phos
phor
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id
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Fertilizer in the SiloApplications – Fertilizer
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Applications – Fertilizer
Railcar Loading
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Urea Fertilizer (also for AdBlue/BlueTec)Applications – Fertilizer
OC(NH2)2
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Prilling Wheel Prilling = Multiple Core Encapsulation
Applications – Fertilizer Prilling
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Fluidized Bed Granulation
Top-Spray Bottom-Spray Tangential-Spray
Applications – Fertilizer
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Applications – Fertilizer
Urea Agglomerates
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CAMSIZER for FertilizerApplications - Fertilizer
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Previous Size Measurement System
Applications – Fertilizer
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Previous Roundness Measurement System
Applications - Fertilizer
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CAMSIZER Test FertilizerApplications - Fertilizer
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Sample Taking FertilizerApplications - Fertilizer
with spoon from bag
not
repr
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tati
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Extreme Segregation because of Bimodal Size
Applications - Fertilizer
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Sample SplittingSampling and Sample Splitting
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Sample Splitting
not
Representativerepr
esen
tati
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Sampling and Sample Splitting
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Sample SplittingSampling and Sample Splitting
Representative
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Sample SplittingSampling and Sample Splitting
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Sample Splitting Fertilizer MixApplications - Fertilizer
Riffle Splitter
Representative
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Mixture of FertilizersApplications - Fertilizer
Sample
SampleSample
Blue = bimodal sampleGreen = monomodal Poly SRed = 3-modal Mixture
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3-Size MixtureApplications - Fertilizer
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Improved Product FertilizerApplications - Fertilizer
Sample
Sample
Sample
Blue = monomodal Poly SGreen = “1.5”-modal Urea + PhosphateRed = “1.5”- modal Mixture of 3 products
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Slow Release Fertilizer Particulates
• Urea Core• Sulfur Layer• Polymer Coating
Urea Core + Sulfur layer
+ Polymer Coating
Urea Core + Sulfur layer
Urea Core
Applications – Fertilizer
Outer Polymer Coating
Inner Sulfur Coating
Urea Nutrient Core
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Coating Layer Thickness
Urea Pellets are a solid round form of nitrogen fertilizer. The individual pellets are almost spherical with diameters usually between 1000µm and 3000μm, sometimes 5000µm.
Coatings can be measured with an accuracy of 2µm layer coating thickness
Applications – Pharmaceuticals
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Outer External Polymer Coating
Inner Sulfur Coating
Urea Nutrient Core
Problems during Fluid Bed ProcessingApplications – Fertilizer
Particles stick together
during the coating and
drying
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30% – 60% of nutrition applicationcan be solved with depot fertilizer
Type and amount of fertilizer is dependent on the soil content, the water quality, the type of plant, and the developing process of the specific plant,
Time diagram of Salt Content during Interval Fertilizingadditional fluid fertilizing two times a week
Time diagram of Salt Content after single Depot Fertilizingbasic fertilizing of standard soil
Applications – Fertilizer
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Slow Release Fertilizer Particulates
• NPK + Traces Core• Polymer Resin Layer• “Glue” Layer
NPK+ Core + Polymer Resin Layer+ Glue Coating Layer
NPK+ Core + Polymer Resin Layer
NPK+ Core
Applications – Fertilizer
Outer „Glue“ Coating
Inner Polymer Resin Coating
NPK Nutrient Core
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• Breadth-/Length-ratio
• Roundness
• Symmetry
• Convexity
xFe max
xc min
A
r1
r2
C
A convex
A real
Particle ShapeMeasurement Results
P
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Optical Process Controlanalysis for size and shape
Measurement Results
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Measurement Results
b/l0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.90
10
20
30
40
50
60
70
80
90
Q3 [%]AK_22,15g_0,3%_BZ_LB_n Ü_xc_min_001.rdfIA_22,15g_0,3%_BZ_LB_n Ü_mit Aerosil_xc_min_001.rdfIA + AK_je 22,15g_0,3%_BZ_LB_n Ü_als Mischung_xc_min_001.rdf
B
A
80
90
Q3 [%]
A B A + B
B A
Amounts of urea beads and pressed /crushed potash granules in a mixture
Urea with Granular Potash
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32.8%
67.2%
xFe max
xc min
Measurement Results
Q3 (round particles) =
CAMSIZER can find the mixing ratio of components of Urea Beads and Granular Potash
Urea with Granular Potash
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Traditional Measurement PelletsApplications - Urea
• Sieve analysis 1.0 – 3.0 mm
• Vibrating plate and weighting(amount of broken particles)
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r rbroken particle
good product
Symm0.948 0.949 0.950 0.951 0.952
15
16
17
18
19
20
21
22
Q3 [%]TP-WS 0525_Probe1_BZ_0.5%_xc_min_001.rdfTP-WS 0525_Probe2_BZ_0.5%_xc_min_001.rdfTP-WS 0525_Probe3_BZ_0.5%_xc_min_001.rdfTP-WS 0525_Probe4_BZ_0.5%_xc_min_001.rdfTP-WS 0525_Probe5_BZ_0.5%_xc_min_001.rdfTP-WS 0525_Probe6_BZ_0.5%_xc_min_001.rdfTP-WS 0525_Probe7_BZ_0.5%_xc_min_001.rdfTP-WS 0525_Probe8_BZ_0.5%_xc_min_001.rdfTP-WS 0525_Probe9_BZ_0.5%_xc_min_001.rdfTP-WS 0525_Probe10_BZ_0.5%_xc_min_001.rdf
2
1min~rr
17.4% broken
20% broken
Symmetry
r1 r2
CAMSIZER – Advantages Measuring Broken Beads
Applications - Urea
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Spreading Fertilizer ParticulatesApplications – Fertilizer
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Larger pellets can be thrown further than
smaller pellets
The exact size is important to get
controlled spreading conditions
Spreading Fertilizer Particulates
Applications – Fertilizer
machine track 1
tractor track 1
tractor track 1
tractor track 2
tractor track 2
tubu
le h
eigh
t (m
m)
tubu
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eigh
t (m
m)
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xc_min [mm]0.5 1.0 1.5 2.0 2.5 3.00
10
20
30
40
50
60
70
80
90
Q3 [%]
Sample1_xc_min_001.rdfSample2_xc_min_002.rdfSample3_xc_min_004.rdfSample4_xc_min_007.rdfSample5_xc_min_002.rdfSample6_xc_min_002.rdfSample7_xc_min_001.rdfSample8_xc_min_001.rdf
Samples 1-8, following samples show identical results (split samples ?) 1=7, 3=5, 2=8, 4=6
Calcium PhosphateApplications – Fertilizer
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b/l0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.90
10
20
30
40
50
60
70
80
90
Q3 [%]
Sample1_xc_min_001.rdfSample2_xc_min_002.rdfSample3_xc_min_004.rdfSample4_xc_min_007.rdf
Samples 1-4 b/l = aspec ratio, 2 groups “1+4” and “2+3”
Calcium PhosphateApplications – Fertilizer
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xc_min [mm]0.2 0.4 0.6 0.8 1.0 1.2 1.40
10
20
30
40
50
60
70
80
90
Q3 [%]
Sample4_xc_min_004.rdfSample4_xc_min_003.rdfSample4_xc_min_005.rdfSample4_xc_min_006.rdfSample4_xc_min_007.rdf
Repeatability: 5 consecutive measurements
Calcium PhosphateApplications – Fertilizer
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CAMSIZER sieve correlation using Elementary Fitting one single sieve class and entire sample
Sieve Correlation Calcium Phosphate
xc_min [µm]200 400 6000
10
20
30
40
50
60
70
80
90
passing [%]
SAMPLE 1_xc_min_001.rdfSAMPLE 1_xc_min_002.rdfSAMPLE 1_xc_min_003.rdfPhosphate Sample 1.ref
Applications – Fertilizer
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Competing Measuring MethodsCompeting Measuring Methods
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Comparison of Methods: Sieving
• robust and industrial-suited• easy handling• references available from user
Advantages
Disadvantages• high amount of time and work• low resolution,
small number of investigatable classes• limited sample amount• no shape analysis possible
Competing Measuring Methods
Worn out sieves
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F2
F1
1. Move
2. Sliding friction
3. Static friction
xc_min [mm]0.5 0.6 0.7 0.8 0.9 1.00
10
20
30
40
50
60
70
80
90
Q3 [%]
0
50
100
150
200
250
300
350
400
450
q3 [%/mm]5454_PT100_xc_min_008.rdf5454_random_xc_min_009.rdf5454_Huntsman-sieve.ref
Round particles are
captured without
rerelease
Applications - Urea
Sieving problems
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fitted result
CAMSIZER-measurement x (red)to sieving * (blue)
Competing Measuring Methods
Fitting of CAMSIZER result to Sieving
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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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x [µm]200 400 600 8000
10
20
30
40
50
60
70
80
90
Q3 [%]
RT669_3993_Z_LB_05%_xc_min_001.rdfRT669_RT_3993.ref
Digital Imaging SievingCubes / Angular Particles
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fitted result
CAMSIZER-measurement x (red)to sieving * (blue)
Competing Measuring Methods
Fitting of CAMSIZER result to Sieving
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xc_min [mm]1.0 1.5 2.0 2.5 3.00
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
Q3
Digital Imaging Sieving
Elementary - Fitting
New elementary fitting with single (narrow) sieve class and entire distribution{
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xc_min [mm]1.0 1.5 2.0 2.5 3.00
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
Q3
xc_min [mm]1.0 1.5 2.0 2.5 3.00
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
Q3
xc_min [mm]1.0 1.5 2.0 2.5 3.00
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
Q3
Digital Imaging Sieving
Q3 – Fitting
Elementary - Fitting
©Ret
sch
Tech
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12 Years CAMSIZER550 installed Instruments
worldwide:Nearly on all continents
For many applications/industries:Ammonium phosphate, Bulk blending companies, Crop
protection, Dicalcium phosphate, Explosives Fertilizer........
©Ret
sch
Tech
nolo
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End
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