Accurate Measurement of Fertilizer with the CAMSIZER

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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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- Two Camera-System- Resolution

Content




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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



- Size

- Shape




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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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Visualization


Q3 [%]

10

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90

p3 [%]


100045 63 140 250 2000 4000500

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6000100010050

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Visualization


Q3 [%]

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p3 [%]


100045 63 140 250 2000 4000500

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6000100010050

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Visualization


Q3 [%]

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p3 [%]


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6000100010050

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Visualization


Q3 [%]

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p3 [%]


100045 63 140 250 2000 4000500

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6000100010050

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Visualization


Q3 [%]

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p3 [%]


100045 63 140 250 2000 4000500

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6000100010050

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Visualization


Q3 [%]

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p3 [%]


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6000100010050

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Visualization


Q3 [%]

10

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p3 [%]


100045 63 140 250 2000 4000500

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6000100010050

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Visualization


Q3 [%]

10

50

90

p3 [%]


100045 63 140 250 2000 4000500

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6000100010050

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Q3 [%]

10

20

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80

90

Q3(36)

250 µm

Particles < 250 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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Content




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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)


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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


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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?


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

ic ac

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


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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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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


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Urea Agglomerates

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CAMSIZER for FertilizerApplications - Fertilizer

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Previous Size Measurement System


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Previous Roundness Measurement System


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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


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Sample SplittingSampling and Sample Splitting

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Sample Splitting

not

Representativerepr

esen

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Representative

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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


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


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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


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


machine track 1

tractor track 1

tractor track 1

tractor track 2

tractor track 2

tubu

le h

eigh

t (m

m)

tubu

le h

eigh

t (m

m)

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xc_min [mm]0.5 1.0 1.5 2.0 2.5 3.00

10

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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”


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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


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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


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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)


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)


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

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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........

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End

Thank you for your attention!