Accurate Measurement of Fertilizer with the CAMSIZER

-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

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

Development of CAMSIZER &

CRYSTALSIZER

Announcement of

Particle size analyzers in Europe

Development of AutoSampler System

New shape functions of CAMSIZER,

first Online-Installations

Retsch Technology

Improvement of CAMSIZER®

with AutoHeight, LED technology, Software, improved resolution,

sharpness and contrast

Development of CAMSIZER XT

for agglomerating powders 1µm-3000µm

History

Comparison between Static Dynamic Image Analysis

ISO 13322-1 ISO 13322-2

- Two Camera-System- Resolution

Content

Two-Camera-System

Basic-Camera

Measuring Principle

Zoom-Camera

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

One Camera Setup

Drawback: tight dynamic range

Dynamic Range: xmin to 50 •xmin

Measuring Principle

CAMSIZER Principle (Two Cameras)

Advantages• Precise full-frame images• Wide dynamic range: 30µm to 30mm

Dynamic Factor:

Measuring Principle

Content

- Size

- Shape

What is the size of this particle?

Measurement Results

Particle Size

Measuring Principle: Sieving

Sphere

6000100050010050

4.5 g6 g

22.5 g

15 g6 g 3 g

Visualization

45 63 140 250 2000 4000

Cumulative distribution

Particle size x[µm]

Q3 [%]

6000100010050

Visualization

Q3 [%]

p3 [%]

100045 63 140 250 2000 4000500

6000100010050

Visualization

Q3 [%]

p3 [%]

100045 63 140 250 2000 4000500

6000100010050

Visualization

Q3 [%]

p3 [%]

100045 63 140 250 2000 4000500

6000100010050

Visualization

Q3 [%]

p3 [%]

100045 63 140 250 2000 4000500

6000100010050

Visualization

Q3 [%]

p3 [%]

100045 63 140 250 2000 4000500

6000100010050

Visualization

Q3 [%]

p3 [%]

100045 63 140 250 2000 4000500

6000100010050

Visualization

Q3 [%]

p3 [%]

100045 63 140 250 2000 4000500

6000100010050

Visualization

Q3 [%]

p3 [%]

100045 63 140 250 2000 4000500

6000100010050

Q3 [%]

Q3(36)

250 µm

Particles < 250 µm

p3 [%]

Visualisierung

Cumulative distribution & FractionsVisualization

100045 63 140 250 2000 4000500

330 µm

Q3( ) Particles < 330 µm

Particle SizeMeasurement Results

xc min

“width”

A‘ = A

“diameter overprojection surface”

xarea“length”

xFe max

xFemax

CAMSIZER results are

compatible with

sieve analysis

Comparison of Size Definitions

differentsize definitions

differentresults

xcmin xArea xFemax

Measurement Results

x [mm]0.2 0.4 0.6 10

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]

Reproducibility

Calibration with traceable standard

=> Absolute accuracy

Measurement Results

Whitehouse Standard XX030Calibration Results

Maintenance-Free byVenturi-Flushing

Features

Content

• 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)

••

Features

Quality Control

UI and SGN values (Literature)Specific Fertilizer Features

SGN and UI values also with CAMSIZER

Specific Fertilizer Features

Analysis of size and shape of

broken granulated coated

fertilizers

CAMSIZER-Advantages FertilizerApplications - Fertilizer

-34Different Fertilizer Product Types,

Different Production Methods, as well as Different Sizes and Shapes

Applications – Fertilizer

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

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)

Separation of fine and coarse particlesSeparation happens because of different sizes

Particles having different sizes

separate

Particles with similar sizes keep homogenety in

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

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?

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

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

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 Shaft Mining of Potash KCl

Applications – Fertilizer Handling of Potash KCl

Chalk / Calcium

1st fertilizing

2nd fertilizing

potash

Bulk Blending Companies and Farmers want the Same Size of the Components

Fertilizer in the SiloApplications – Fertilizer

Railcar Loading

Urea Fertilizer (also for AdBlue/BlueTec)Applications – Fertilizer

OC(NH2)2

Prilling Wheel Prilling = Multiple Core Encapsulation

Applications – Fertilizer Prilling

Fluidized Bed Granulation

Top-Spray Bottom-Spray Tangential-Spray

Urea Agglomerates

CAMSIZER for FertilizerApplications - Fertilizer

Previous Size Measurement System

Previous Roundness Measurement System

CAMSIZER Test FertilizerApplications - Fertilizer

Sample Taking FertilizerApplications - Fertilizer

with spoon from bag

Extreme Segregation because of Bimodal Size

Sample SplittingSampling and Sample Splitting

Sample Splitting

Representativerepr

Representative

Sample Splitting Fertilizer MixApplications - Fertilizer

Riffle Splitter

Representative

Mixture of FertilizersApplications - Fertilizer

Sample

SampleSample

Blue = bimodal sampleGreen = monomodal Poly SRed = 3-modal Mixture

3-Size MixtureApplications - Fertilizer

Improved Product FertilizerApplications - Fertilizer

Sample

Blue = monomodal Poly SGreen = “1.5”-modal Urea + PhosphateRed = “1.5”- modal Mixture of 3 products

Slow Release Fertilizer Particulates

• Urea Core• Sulfur Layer• Polymer Coating

Urea Core + Sulfur layer

+ Polymer Coating

Urea Core + Sulfur layer

Urea Core

Outer Polymer Coating

Inner Sulfur Coating

Urea Nutrient Core

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

Outer External Polymer Coating

Inner Sulfur Coating

Urea Nutrient Core

Problems during Fluid Bed ProcessingApplications – Fertilizer

Particles stick together

during the coating and

drying

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

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

Outer „Glue“ Coating

Inner Polymer Resin Coating

NPK Nutrient Core

• Breadth-/Length-ratio

• Roundness

• Symmetry

• Convexity

xFe max

xc min

A convex

A real

Particle ShapeMeasurement Results

Optical Process Controlanalysis for size and shape

Measurement Results

b/l0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.90

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

Q3 [%]

A B A + B

Amounts of urea beads and pressed /crushed potash granules in a mixture

Urea with Granular Potash

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

Traditional Measurement PelletsApplications - Urea

• Sieve analysis 1.0 – 3.0 mm

• Vibrating plate and weighting(amount of broken particles)

r rbroken particle

good product

Symm0.948 0.949 0.950 0.951 0.952

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

1min~rr

17.4% broken

20% broken

Symmetry

CAMSIZER – Advantages Measuring Broken Beads

Applications - Urea

Spreading Fertilizer ParticulatesApplications – Fertilizer

Larger pellets can be thrown further than

smaller pellets

The exact size is important to get

controlled spreading conditions

Spreading Fertilizer Particulates

machine track 1

tractor track 1

tractor track 2

xc_min [mm]0.5 1.0 1.5 2.0 2.5 3.00

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

b/l0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.90

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”

xc_min [mm]0.2 0.4 0.6 0.8 1.0 1.2 1.40

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

CAMSIZER sieve correlation using Elementary Fitting one single sieve class and entire sample

Sieve Correlation Calcium Phosphate

xc_min [µm]200 400 6000

passing [%]

SAMPLE 1_xc_min_001.rdfSAMPLE 1_xc_min_002.rdfSAMPLE 1_xc_min_003.rdfPhosphate Sample 1.ref

Competing Measuring MethodsCompeting Measuring Methods

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

1. Move

2. Sliding friction

3. Static friction

xc_min [mm]0.5 0.6 0.7 0.8 0.9 1.00

Q3 [%]

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

fitted result

CAMSIZER-measurement x (red)to sieving * (blue)

Fitting of CAMSIZER result to Sieving

x [mm]0.2 0.4 0.6 10

Q3 [%]

Sample A_BZ_0.2%_xc_min_001.rdfSample A_.ref

Digitale Imaging Sieving

x [µm]200 400 600 8000

Q3 [%]

RT669_3993_Z_LB_05%_xc_min_001.rdfRT669_RT_3993.ref

Digital Imaging SievingCubes / Angular Particles

fitted result

CAMSIZER-measurement x (red)to sieving * (blue)

Fitting of CAMSIZER result to Sieving

xc_min [mm]1.0 1.5 2.0 2.5 3.00

Digital Imaging Sieving

Elementary - Fitting

New elementary fitting with single (narrow) sieve class and entire distribution{

xc_min [mm]1.0 1.5 2.0 2.5 3.00

Digital Imaging Sieving

Q3 – Fitting

Elementary - Fitting

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........

Thank you for your attention!

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