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© 2015 HORIBA, Ltd. All rights reserved. 1 © 2015 HORIBA, Ltd. All rights reserved. 1 How the CAMSIZER Solves Sieving Problems HORIBA Scientific Particle Characterization Ian Treviranus February 18, 2015

How the CAMSIZER Solves Sieving Problems February · PDF file ... If sieve analysis is used for ... How the CAMSIZER Solves Sieving Problems February

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Page 1: How the CAMSIZER Solves Sieving Problems February  · PDF file  ... If sieve analysis is used for ... How the CAMSIZER Solves Sieving Problems February

© 2015 HORIBA, Ltd. All rights reserved. 1© 2015 HORIBA, Ltd. All rights reserved. 1

How the CAMSIZER SolvesSieving Problems

HORIBA ScientificParticle Characterization

Ian Treviranus

February 18, 2015

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© 2015 HORIBA, Ltd. All rights reserved. 2

What we’ll talk about

• Review of common sieving challenges

• CAMSIZER technology

• Simple, intelligent sieve correlation

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© 2015 HORIBA, Ltd. All rights reserved. 3

Size analysis via sieving

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Sieves go way back

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© 2015 HORIBA, Ltd. All rights reserved. 5

Labs can look like this

Image courtesy of Tom Gapinske and Summit Envirosolutions*original located here: www.horiba.com/fileadmin/uploads/Scientific/Documents/PSA/Webinar_Slides/AP034.pdf

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•(A) Low accuracy, low precision measurements form a diffuse, off-center cluster; (B) Low accuracy, high precision measurements form a tight off-center cluster; (C) High accuracy, low precision measurements form a cluster that is evenly distributed but distant from the center of the target; (D) High Accuracy, high precision measurements are clustered in the center of the target.

LOW ACCURACYLOW PRECISION LOW ACCURACY

HIGH PRECISION HIGH ACCURACYLOW PRECISION HIGH ACCURACY

HIGH PRECISION

Accuracy vs. precision

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© 2015 HORIBA, Ltd. All rights reserved. 7

Sampling

Sample division

Test Sieves

Sieve shakers

Evaluation

Accessories& cleaning

Sieve measurement workflow

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© 2015 HORIBA, Ltd. All rights reserved. 8

Separation happens during- Transport processes (container, train and

truck)- Feeding processes (funnels, vibration feeders,

belts)- and Storage (bulk pile, silo)

Sampling and Sample Splitting

Segregation

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© 2015 HORIBA, Ltd. All rights reserved. 9

Hell

Sampling and Sample Splitting

Sampling & sample splitting

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© 2015 HORIBA, Ltd. All rights reserved. 10

0

10

20

30

40

50

60

70

80

90

100

Q3

(x)

/ %

50 100 500 1000 5000 10000Particle size / µm

Quartz

Sample 1Sample 2Sample 3

Randomsampling

3 accurate analyses = 3 different results!

Consequence of sampling

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© 2015 HORIBA, Ltd. All rights reserved. 11

If sieve analysis is used for quality controlwithin the context of DIN EN ISO 9000:2000

then both the sieve shaker and thetest sieves must be subjected to

test agent monitoring.

w = mesh widthd = wire diameter

Tolerance for mean value (Y):The mean value of the mesh width must not differ from thenominal value w by more than the tolerance ± Y.

w

w

Ø d

Ø d

Technical requirements & testingaccording to ISO 3310

Standards compliant sieves

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100 200 300 40040 50 60 70 80 90Particle size x[µm]

10

20

30

40

50

60

70

80

90

Q3 [%]

10

20

30

40

50

60

70

80

90

Q3 [%]

44%

+Y 66.7

36%

-Y 59.3

63 µmTolerance ± Y = 3.7 µm

40%

Importance of mesh width

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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

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1400µm 1400µm 1429.5µm

Mesh sizes warp Mesh 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 ~1455µmsieve No. 03033531 (nominal 1400µm)

Theory: Reality:

Influence of mesh width

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© 2015 HORIBA, Ltd. All rights reserved. 15

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

Real mesh width

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0

10

20

30

40

50

60

70

80

90

100Q

3(x)

/ %

10 50 100 500 1000 5000Particle size / µm

Identifiers

AMP- 2AMP- 0.5AMP- 1.2

Quartz sand, Sieving time: 2 min.

Effect of amplitude

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© 2015 HORIBA, Ltd. All rights reserved. 17

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

Roundparticles

arecapturedwithout

rerelease

Applications - Proppants

Overloading sieves

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© 2015 HORIBA, Ltd. All rights reserved. 18

- robust and accepted- easy handling- references available from user

Advantages

Disadvantages- high amount of time and work- low resolution, small number of classes available

- limited sample amount- no shape analysis possible

Competing Measuring Methods

Worn out sieves

Sieving pros & cons

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© 2015 HORIBA, Ltd. All rights reserved. 19

Sieve support issues

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Processing during Ro-Tap

• Resin-coated sands may be altered by mechanical energy– Clusters break, hiding potential issue– Resin abrades, overstating dust

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• Sampling problems:wrong sampling (pouring and “spooning“)

• Sieve problems: overloading of sieves (blinding / blocking), cross contamination from trapped material, nominal size real sizes of meshes (wide specification and worn out sieves), sieving machines are not calibrated

• Balance problems:low resolution (0.1 grams), not sensitive for small weights (contamination) of joints and moving parts, interference with air flow

• Time problems:Sieve analysis too long to meet business requirements

Issues with sieving

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© 2015 HORIBA, Ltd. All rights reserved. 22

Sieves aren’t always fast enough

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© 2015 HORIBA, Ltd. All rights reserved. 23

What we’ll talk about

• Review of common sieving challenges

• CAMSIZER technology

• Simple, intelligent sieve correlation

Page 24: How the CAMSIZER Solves Sieving Problems February  · PDF file  ... If sieve analysis is used for ... How the CAMSIZER Solves Sieving Problems February

© 2015 HORIBA, Ltd. All rights reserved. 24

Featured technologies• LA-960

Laser Diffraction

• SZ-100Dynamic Light Scattering & Zeta Potential

• CAMSIZER & CAMSIZER XTDynamic Image Analysis

• PSA300Static Image Analysis

• SA-9600Flowing Gas BET Surface Area

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© 2015 HORIBA, Ltd. All rights reserved. 25

CAMSIZER Dynamic Image Analyzers

• High resolution size & shape• Intelligent sieve correlation• Patented dual capture• CAMSIZER

– 20 µm – 30 mm– Free flowing powders, granules

• CAMSIZER XT – 1 µm – 8 mm– Cohesive or free flowing

powders– Suspensions with

accessory

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© 2015 HORIBA, Ltd. All rights reserved. 26

Take a picture,

measure for size

Measurement Results

Image analysis in a nutshell

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© 2015 HORIBA, Ltd. All rights reserved. 27

Two camera system

Basic-Camera Zoom-Camera

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© 2015 HORIBA, Ltd. All rights reserved. 28

Use gravity, or, better, vacuum (from a compressed air supply and venturi) in order to draw particles through instrument. Vacuum helps keep the windows clean.

Moving particles

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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.

Resolution

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Resolution

mixture of six sizes of grinding balls

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Advantage of image analysisBetter Size Analysis due to Understanding of Particle Shape:

Length, Width, Average Diameter

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Shape analysis

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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Statistical sledgehammerCAMSIZER easily measures tens and hundreds of thousands of particles

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© 2015 HORIBA, Ltd. All rights reserved. 34

What we’ll talk about

• Review of common sieving challenges

• CAMSIZER technology

• Simple, intelligent sieve correlation

Page 35: How the CAMSIZER Solves Sieving Problems February  · PDF file  ... If sieve analysis is used for ... How the CAMSIZER Solves Sieving Problems February

© 2015 HORIBA, Ltd. All rights reserved. 35

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

CAMSIZER Sieving

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Comparison to results from sieve analysis

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Particles can slip through a mesh although it is not expected!

Comparison to results from sieve analysis

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“Width”, measured with CAMSIZER xc min (red)Results from sieving (* black)

xc min

CAMSIZER size distribution is wider than thedistribution from sieve analysis

… this effect is caused by how a sieve will pass coarser particles than you think!

Comparison to results from sieve analysis

Page 39: How the CAMSIZER Solves Sieving Problems February  · PDF file  ... If sieve analysis is used for ... How the CAMSIZER Solves Sieving Problems February

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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

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

Elementary fitting function

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© 2015 HORIBA, Ltd. All rights reserved. 40

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

One fitting file works for multiple samples!

Digital Imaging Sieving

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© 2015 HORIBA, Ltd. All rights reserved. 41

Requirements for correlation

Reliable sieve dataCustomers may have un-calibrated test sieves and / or sieve shakers. Bad

sieving practice such as overloaded sieve pans also affect the accuracy of sieving. Test analyses need to be closely monitored according to ISO 3310.

Good sampling

Good CAMSIZER measurementsMeasurements are only good if it is (1) repeatable and (2) reproducible.

xc min particle size model should be used for fitting files.

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DankeБольшое спасибо

Grazie

اُشْكر

Σας ευχαριστούμε

감사합니다

Obrigado

谢谢

ขอบคุณครับ

ありがとうございました

ध यवाद

நன்ற

Cảm ơn

Dziękuję

Tack ska ni ha

Thank you

Merci

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