Der CAMSIZER XT – Partikelcharakterisierung mittels ... · CAMSIZER® P4 Meet the New CAMSIZER P4 DynamicImageAnalyzer - Why Image Analysis? - Features of the CAMSIZER P4 - Benefits

CAMSIZER® P4

Meet the New CAMSIZER P4 Dynamic Image Analyzer

- Why Image Analysis? - Features of the CAMSIZER P4 - Benefits of the CAMSIZER P4

Jeff Bodycomb HORIBA Scientific

Gert Beckmann

Retsch Technology GmbH

Why Image Analysis: Images of Particles

What information can we get from this image?

• Shape

• Size

• Transparency

• Surface Texture

• …………

• in excellent resolution!

• on a single particle!

Why Image Analysis: Sample Single Particle

What do we want to characterize?

• Particle ?

• Sample ?

• Product ?

What information of the sample or the product do we need ?

• Particle size distribution

• Shape characteristics

• Differences between product samples (uncoated coated or new used, etc)

• Agreement with quality specifications (good bad)

• Amount of a part of the product (% component 1 % component 2)

using size, shape or transparency parameters


Requirements:

• Measurement of many particles

• Complete measurement of the entire sample

• Quick measurement

• Objective and reproducible

• Limited manual effort

Automatic Image Capturing and computer aided processing of data!


Measuring Principle

6 © Retsch Technology GmbH

Digital Image Analysis

STATIC (ISO 13322-1) • Particles do not move during measurement • High resolution > 0,5 μm • Low statistic (few 100 particles are analyzed)

• Limited measurement range • Time consuming • Particles detected in stable orientation

(2 Dimensions)

DYNAMIC (ISO 13322-2)

• Particles in motion relative to camera

• Resolution > 1 μm • Few million particles are analyzed

(representative measurement) • Wide measurement range • Fast • Particles can be measured in all random

orientations (3 Dimensions)

Image Analysis

ISO 13322-2

Orientated 2D

Random 3D

Dynamic

ISO 13322-1

Static

x [mm]1 2 3 4 5 6 7 80

10

20

30

40

50

60

70

80

90

Q3 [%]

Rod 2mm_1-3 B_LB_xFemax_001.rdf






Messwertdiagramm:

C:\...mme\CAMSIZER_0162_3.30\CAMDAT\Rods 2 x 2mm\Rod 2mm_1-3 B_LB_xFemax_001.rdf

Messaufgabe: Rod 2mm_1-3 B_LB.afgx [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.rdf






Messwertdiagramm:

C:\Programme\CAMSIZER_0162_3.30\CAMDAT\Rods 2 x 2mm\Rod 2mm_1-1 B_xFemax_002.rdf

Messaufgabe: Rod 2mm_1-1 B.afg

Without Guidance Sheet

With Guidance Sheet

length measurement for orientated rods + extrudates

length measurement for non orientated minipellets

correct length

short

length

correct length

length measurement methods without and with flexible guidance sheet (sample director)

Measurement Results


Particle Size


xc min

xc min

“width”

A

A‘ = A

xare

a

“diameter over

projection surface”

xarea

“length”

xFe max

xFe max

CAMSIZER results

are

compatible

with

sieve analysis

Results of Dynamic Image Analsis


Better Size Analysis due to Understanding of Particle Shape: Length, Width, Average Diameter


Test Sieves that comply with standards

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

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

test agent monitoring.

w = mesh width d = wire diameter

Tolerance for mean value (Y):

The mean value of the mesh width must not differ from the nominal value w by more than the tolerance ± Y.

w

w

Ø d

Ø d

Technical requirements & testing according to ISO 3310

Results of Dynamic Image Analysis


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

Graph of measurement results: C:\Program Files\CAMSIZER\CAMDAT\M247-3_TEST\Sample-1__xc_min_002.rdf Task file: Code-M247-3.afg

xc min = = d = Xc min

particle-width

Basic-Camera Zoom-Camera

CAMSIZER P4

Small particles in high resolution

Large particles in high representation

CAMSIZER P4 Wide Measurement Range because of 2 Camera-System


Advanced, Patented Optics Design

Sample Flow

Light Source 2

Light Source 1

Basic Camera

Zoom Camera

Measurement Principle (CAMSIZER XT)

CAMSIZER P4 Introduction

1. New Hardware

2. New Software

3. Application Examples

4. Options and Accessories

Content CAMSIZER P4


Whats New?

CAMSIZER P4 Introduction

1. New Hardware

2. New Software



Content CAMSIZER P4


Whats New?

CAMSIZER P4 (What‘s new) New CAMSIZER P4


CCD - Basic CCD - Zoom

Detection of particles

One pixel is element of a projection when at least half of the pixel is covered.

Measurement principle

Resolution

Sieving Aids Sieving and Imaging (free fall)

21 © Retsch GmbH

• Aerosil®

• Aeroxide ®

Aluminiumoxid

•Talcum (only sieving)

Powders

• Wet sieving

• Remove grease:

Benzines

Alcohols

Fluid sieving aids

• Chain rings

• Brushes

• Cubes

• Rubber balls

• Achat balls

• Steatite balls

Mechanical sieving aids

and CAMSIZER Dispersion Aids

CAMSIZER® P4

The New Generation

Two Camera-System CAMSIZER P4


Large dynamic measuring range:

Size-Range: Factor of 1500 within one measurement

Particle size

A B

C D

20 μm 30 mm

Lower limit Upper limit

CAMSIZER P4 market introduction

1. New Hardware

2. New Software


4. Options and accessories

Content CAMSIZER P4


Whats New?

New Software: Image Database CAMSIZER P4


New Tool for improved understanding and documentation Typically ~100.000 single particle pictures per measurement

New Software: Scattergrams CAMSIZER P4


3D-Cloud

3D-Display of Data points Powerful tool for distinguishing particles with different size and / or different shapes

New Software: Particle Library CAMSIZER P4


The Particle Library is a software package separate from the CAMSIZER software. It includes the data presentation: 3D-cloud, image database, and filtering


Stability of Size and Shape Parameters

xc min

“width”

xc min

=> stable parameter

for good sieve correlation

even when particles overlap

For detection of twins and triplets

=> xFe max length or w/l aspect ratio can be used

New Software: New Shape Descriptors CAMSIZER P4


Krumbeins Roundness and Sphericity

For proppants, sands, and other non-round, angular particles Compatible with ISO 13503-2 and API

Krumbein Sphericity SPHT_K

measures the elongation of the particles (like w/l = b/l). Calculation based on W/L_perp = B/Lrec, with a different scaling

Average diameter of all corners divided by diameter of maximum inscribed circle

Krumbein Roundness RDNS_C

measures the „angularity“, or „corner curvature radius“


Clumps (are „Round“) => Stability

RDNS_C => stable parameter

for good microscope correlation

even when particles overlap


1. New Hardware

2. New Software



Content CAMSIZER P4


Whats New?

Application Examples CAMSIZER P4


Whats New?

•Higher Resolution of Zoom and Basic •Higher Brightness of the LED

Better image quality

More depth of focus

Precise shape detection for small particles

more pixels and more optical resolution

Transparent plastic extrudates: Measurement of length and diameter with the motorized guidance sheet



Whats New? New Specification: 20µm instead of 30µm lower limit •Higher Resolution of Zoom and Basic •Higher Brightness of the LED More precise detection of small particles < 100µm Tungsten Carbide powder in the size range from 20µm - 300µm.

Laser diffraction results are shown for comparison.



Whats New? •Higher Resolution of Zoom and Basic •Higher Brightness of the LED

Better statistics

More particles per second

Wider size range

Refractory materials with extremely wide particle size distribution: Same results as the sieve analysis


1. New Hardware

2. New Software



Content CAMSIZER P4


Whats New?

Same range of accessories as for the CAMSIZER:

• Calibration reticle

• Guidance sheet

• Chutes and funnels

• De-Ionizer

• Dust filter

• Air filter

• IQ/OQ/PQ

•21CFR Part 11 software

Options and Accessories


CAMSIZER P4

Whats New?

AutoSampler


CAMSIZER P4

CAMSIZER P4 AutoSampler for 12 – 60 cups

CAMSIZER Online CAMSIZER P4


CAMSIZER P4 can be configured as „Online“ or „Online light“

CAMSIZER P4

1. New Hardware

2. New Software



Content CAMSIZER P4


Whats New?

CAMSIZER & CAMSIZER XT Petroleum Coke, Carbon / Graphite Powders


CAMSIZER XT for Carbon Graphite Powders


Motor electrodes and sample containers

CAMSIZER XT for Carbon Powders


Correlation with Laser Analysis

Correlation with sieve analysis

CAMSIZER XT with X-Fall for Graphite Powder


xc_min [mm]0.6 1 2 40

10

20

30

40

50

60

70

80

90

Q3 [%]

0

5

10

15

20

25

30

35

40

45

p3 [%]

RC-6900-1mm8---6mm-GRC-X-Fall_xc_min_001.rdf

RC6900-1mm8--6mm-GRC.ref

Résultats graphique de mesure:

C:\...6\CAMDAT\Carbone-Savoie-grain\RC-6900-1mm8---6mm-GRC-X-Fall_xc_min_001.rdf

Fichier méthode: Coke-Grain-X-Fall.afg

Features of the CAMSIZER®


Calibration Reticule

- Traceble to an International Standard - Covering the Whole Measurement Range - Instrument to Instrument Agreement

Static Calibration

3D Printing of Metal Construstions


3D printing with metal:

The final frontier

of additive

manufacturing


• Breadth-/ Length-Ratio

• Roundness

• Symmetry

• Convexity

xFe max

xc min

A

r1

r2

C

A convex

A real

Particle Shape (CAMSIZER and CAMSIZER XT)

P

Reports and Warnings



Optical Process Control Analysis for Size and Shape

Calcium-Bentonite


xc_min [µm]600 800 1000 1200 1400 1600 1800 2000 2200

0

10

20

30

40

50

60

70

80

90

passing [%]

Oil-Dri-BZ-GS-L-10-030-STD-2-times_xc_min_001.rdf


Oil-Dri-BZ-GS-L-10-032-STD-1-time_xc_min_002.rdf




Graph of measurement results:

D:\...A-USA-3GB\Oil-Dri\CAMDAT\Oil-Dri-BZ-GS-L-10-030-STD-2-times_xc_min_001.rdf

Task file: Oil-Dri-BZ-GS.afg

SPHT0.75 0.80 0.85 0.90 0.95

0

10

20

30

40

50

60

70

80

90

Q3 [%] Oil-Dri-BZ-GS-L-10-030-STD-2-times_xc_min_001.rdf







D:\...A-USA-3GB\Oil-Dri\CAMDAT\Oil-Dri-BZ-GS-L-10-030-STD-2-times_xc_min_001.rdf

Task file: Oil-Dri-BZ-GS.afg

Fused Silica


xc_min [mm]0.2 0.4 0.6 0.8 1.00

10

20

30

40

50

60

70

80

90

Q3 [%]

Minco-30-50 003217H-1_xc_min_007.rdf

mesh30-50-003217H-1.ref


D:\...10-January\CAMDAT\Mesh-30-50-February\Minco-30-50 003217H-1_xc_min_007.rdf

Task file: RT1594_Minco_10mm-GS_convex.afg

xc_min [mm]0.05 0.10 0.15 0.20 0.25 0.30 0.350

10

20

30

40

50

60

70

80

90

Q3 [%]

Minco50-100_BZ_fix35_10mmGS_convex_xc_min_009.rdf

RT1549_50-100_rec_sieve.ref


D:\...nuary\CAMDAT\Mesh-50-100\Minco50-100_BZ_fix35_10mmGS_convex_xc_min_009.rdf

Task file: RT1594_Minco30-50_convex_10mm-GS.afg

0.1 – 0.35mm

0.2 – 0.7mm

xc_min [mm]0.1 0.2 0.3 0.40

100

200

300

400

500

600

q3 [%/mm]Minco-50-100_Sample-4-05%_xc_min_001.rdf

Minco-50-100_Sample-3-05%_xc_min_006.rdf

Minco-50-100_Sample 1 Half Repeat_xc_min_005.rdf


C:\...-3-16\CAMDAT\Mesh-50-100-Sample-4\Minco-50-100_Sample-4-05%_xc_min_001.rdf

Task file: RT1594_Minco50-100_10mm-GS.afg

Silicon seeds and beads


xc_min [mm]0.2 0.4 0.6 0.8 1.00

10

20

30

40

50

60

70

80

90

Q3 [%]

Sample 3_Z_xc_min_003.rdf

RT1541_Seed3_sieve.ref


C:\...m Files\CAMSIZER_REC_HD\CAMDAT\RT1541_Rec_z-only\Sample 3_Z_xc_min_003.rdf

Task file: RT1541_sample3_Z.afg

CAMSIZER Counting with

Stepped feeder and CCD- Zoom

Counting and Sieve Correlation

of fine silicon seeds and beads

Size Distribution of Cadmium,

Cadmium Sulfate, and Cadmium Tellurite

with CAMSIZER XT + X-Dry + X-Jet

xMa_min [mm]0.5 1.0 1.5 2.0 2.50

10

20

30

40

50

60

70

80

90

Q3 [%]

REC-#4_xMamin_001.rdf

RT1524_REC#4_sieve.ref


E:\...AMSIZER-HORIBA-USA-3GB\REC-Silicon\RT1524_REC\CAMDAT\REC-#4_xMamin_001.rdf

Task file: RT1524_REC4_1%.afg

Benefits of the CAMSIZER P4 Comparison


CAMSIZER P4 Benefits

1. Two Camera System

2. Unique Calibration

3. Better Hardware (light source, cameras, interfaces)

=> faster measurements, higher reproducibility

4. New Software (specific tools to solve quality requirements

for example RDNS_C Roundness)

5. New Features (Automatic Feed Guide, Particle Library

CAMSIZER® P4

1998 => 2004 => 2006 => 2015 CAMSIZER P4 Fourth Generation of Dynamic Image Analyzer

CAMSIZER® P4

1998 => 2004 => 2006 => 2015 CAMSIZER P4 Fourth Generation of Dynamic Image Analyzer


CAMSIZER 1998 CAMSIZER 2004 CAMSIZER 2006 CAMSIZER P4

Lightsource Ccfl 100µs Ccfl/cont.LED 100µs 90Hz LED-30µs 120Hz LED-20µs

exposure time with Dimming (50%) (On Off) (On Off)

Source life time 2 years 4 years 20 years 25 years

Light intensity factor 1 factor 1 / 2 factor 20 factor 50

Cameras (pixels) 425,000 425,000 780,000 1,300,000

Resolution (Zoom) 20µm 20µm 15µm (7.5µm) 10µm (5µm)

Image rate 50/s 50/s 56/s 60/s

Orientation (Basic) vertical vertical horizontal horizontal

Feeder control ISA-Bus RS 232 RS 232 USB or RS 232

Funnel adjustment manual AutoHeight AutoHeight AutoHeight

30mm 50mm 50mm

12 Volt 24 Volt 24 Volt

Vacuum manual manual automatic automatic

Motorized Feedguide - - manual automatic

CAMSIZER® Models 1998 - 2015 Specifications

New Hardware CAMSIZER P4


Feature

CAMSIZER 2006

CAMSIZER P4

Difference

Camera resolution Basic [Pixel] 1024 x 768 1296 x 966 +60%

Image resolution Basic [µm / Pixel] 87 66 +25%

Field of view Basic [mm x mm] 82 x 62 82 x 62 -

Frames per second Basic [fps] 28 30 +6%

Camera resolution Zoom [Pixel] 1024 x 786 1296 x 966 +60%

Image resolution Zoom [µm / Pixel] 15 10 +33,3%

Field of view Zoom [mm x mm] 15 x 12

15 x 12

-

Frames per second Zoom [fps] 28 30 +6%

Comparison Chart Technical Specifications

Better camera resolution and larger number of pixels improves statistics and reproducibility

New Hardware in CAMSIZER P4 CAMSIZER P4


New Cameras • Higher resolution 1296 x 966 pixel • Faster interface: more pixel / second

New Lenses • Higher resolution for Zoom camera • Larger depth of focus (Sharpness)

New light source • Brighter, better contrast

Lighted Switch at Front • Better control

New Hardware in CAMSIZER P4 CAMSIZER P4


New camera interface: GigE •Ethernet cables and Ethernet interface card

Different PC • more performance for database and 3D CAMSIZER Cloud • faster harddisk: SSD • standard GigE Interface card replaces old framegrabber board

New power supply and control board • more Amps for brighter LED • more flexible (pulse length, frequency etc.) • USB interface instead of RS232

Benefits of the CAMSIZER P4 Comparison


CAMSIZER P4 Benefits

1. Two Camera System

2. Unique Calibration

3. Better Hardware (light source, cameras, interfaces)

=> faster measurements, higher reproducibility

4. New Software (specific tools to solve quality requirements for example

RDNS_C Roundness)

5. New Features (Automatic Feed Guide, Particle Library

Alternative Methods



Particle Shape: Mixture of Activated Carbon and Ion Exchanger

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

Graph of m easurement results:C: \...h-3jhwpy ax\Camdat\Messungen 030603\AK_22,15g_0,3%_BZ_LB_n Ü_xc_min_001. rdfTask f ile: R T 502 IA_BZ_LB_0,7%_R40-Trocknung_.af g

B

A

b/l 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 0

10

20

30

40

50

60

70

80

90

Q3 [%]

A B A + B

B A


32.8%

67.2%

xFe max

xc min

Q3 (round particles) =

Particle Shape: Mixture of Activated Carbon and Ion Exchanger (Water Purifier)


pelletized carbon black

• Particle size of pelletized carbon black

sieve analysis 0.1 – 2.0 mm (approx. 2 min.)

abrasion analysis (approx. 3 * 6 min.)

Traditional Measurement (Carbon Black)


Traditional Measurement (Granulated Carbon)

Sensitive carbon black pellets are destroyed by sieving, conveyance and storing


CAMSIZER measures

size and shape

without destroying sensitive

carbon black granules

CAMSIZER - Advantages

x [mm]0.5 1.0 1.5 2.0 2.50

10

20

30

40

50

60

70

80

Q3 [%]

Ruß_ölgeperlt_ES34_001.rdf


Ruß_N660_001.rdf

Ruß_N660_002.rdf

Messwertdiagramm:

C:\...2GB\CAMSIZER-Degussa-Ruß-Kalscheuren-Hanau-13MB\Ruß_ölgeperlt_ES34_001.rdf

Messaufgabe: Degussa Ruß ES 34.afg

Particle Size

SPHT0.3 0.4 0.5 0.6 0.7 0.8 0.9

0

10

20

30

40

50

60

70

80

90

Q3 [%]Ruß_ölgeperlt_ES34_001.rdf


Ruß_N660_Form_002.rdf

Ruß_N660_Form_001.rdf

Messwertdiagramm:

C:\...2GB\CAMSIZER-Degussa-Ruß-Kalscheuren-Hanau-13MB\Ruß_ölgeperlt_ES34_001.rdf

Messaufgabe: Degussa Ruß ES 34.afg

Roundness

x [mm] 0.5 1.0 1.5 2.0 2.5 0

10

20

30

40

50

60

70 80

Q3 [%]

Carbon black_ES34_001.rdf Carbon black_ES34_002.rdf Carbon black_N660_001.rdf Carbon black_N660_002.rdf

x [mm] 0.5 1.0 1.5 2.0 2.5 0

10

20

30

40

50

60

70 80

Q3 [%]

Carbon black_ES34_001.rdf Carbon black_ES34_002.rdf Carbon black_N660_001.rdf Carbon black_N660_002.rdf


Activated Carbon (Powder, Granules & Extrudates)


xc_min [µm]100 200 300 400 500 6000

10

20

30

40

50

60

70

80

90

Q3 [%]

0

5

10

15

20

25

30

35

40

45

p3 [%]

Messwertdiagramm:

M:\...ann&Hummel\CAM-Installation_FM\CamSizer\CAMDAT\18_901_00_253\61003_004.rdf

Messaufgabe: 18_901_00_253.afg

CAMSIZER Sieve Analysis

Sieve Correlation Activated Carbon (Granules)

x [mm] 6 8 10 12 14 16 18 20 22 0

10

20

30

40

50

60

70

80

90

Q3 [%]

L_BZ_LB_1zu3_05%_xc_min_004.rdf L_BZ_LB_1zu3_05%_xc_min_005.rdf L_BZ_LB_1zu3_05%_xFemax_004.rdf L_BZ_LB_1zu3_05%_xFemax_005.rdf

Diameter and Length Results of Wood Fibers measured with CAMSIZER P4

xc min xFe min xMa min

xc min

xFe min

xMa min

2

A

2

A

CAMSIZER® width definitions for elongated particles (extrudates)

xFe max xlength xstretch

xMa min

xFe max

xlength

A xstretch

Xlength = Xstretch =

xMa min

CAMSIZER® length definitions for elongated particles (extrudates)

Ma min x

A 2 2

max Ma min Fe x x -

xFe max xlength xFe rec

xMa min

xF

e r

ec =

xle

ngth

CAMSIZER® length definitions for elongated particles (extrudates)

xMa min

xF

e r

ec =

xle

ngth

xMa min

xF

e r

ec

xFe rec xFe max

Length measurement without guidance sheet (sample director)

φ

Ø 2mm

Xlength =

xMa min x

length

xF

e m

ax

correct length short length

CAMSIZER® length measurements for elongated particles (extrudates)

( ) ( ) 2

min

2

max Ma Fe x x -

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


C:\...DAT\Kaneka_Probe-PP66-226\Kaneka_160H_Z_1%-mit-Ausblndng099_xFemax_002.rdf

Task file: Reis-LK.afg

x [mm]1.0 1.5 2.0 2.5 3.0 3.5

0

50

100

150

200

q3 [%/mm]

Z-Ausbl-conv0985-160H-1-3Part_xFemax_002.rdf

Z-Ausbl-conv0985-200H-1-3Part_xFemax_001.rdf


C:\... \Messungen-am-21-Februar-2005\Z-Ausbl-conv0985-160H-1-3Part_xFemax_002.rdf

Task f ile: Govatec-Z-Ausbl-conv-0985.afg

Right side

of distribution

correct length short length

correct length

length measurement without guidance sheet (sample director)

Reference particles Calibration validation with steel rods of the same

dimensions as particles

reticle implant

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 1 month)

Applications – Pharmaceuticals

Reference particles

Calibration validation with steel rods of the same

dimensions as particles

Applications – Pharmaceuticals

reticles of „short

extrudates to

homogenise

the product“ reticle implant

implant reticles

Thank you for your attention!

Documents

Der CAMSIZER XT – Partikelcharakterisierung mittels ... · CAMSIZER® P4 Meet the New CAMSIZER P4 DynamicImageAnalyzer - Why Image Analysis? - Features of the CAMSIZER P4 - Benefits