camsizer xt - horiba · camsizer xt - the latest in dynamic image analysis webinar wednesday, 14th...

CAMSIZER XT - the latest in Dynamic Image Analysis

WebinarWednesday, 14th of September 2011

Speaker: Gert BeckmannRetsch Technology GmbH

Host: Ian TreviranusHORIBA Instruments International

2© Retsch Technology GmbH

History of Retsch Technology GmbH

Content

InstrumentInstrument

1.1. Measurement Measurement principleprinciple

2.Results

Applications

3.Markets and applications

4.Alternative analysis methods


Comparison between Static Dynamic Image Analysis


ISO 13322-1 ISO 13322-2

CCD - Basic CCD - ZoomDetection of particles

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

Measurement principle

Resolution

Dispersion Modules


Particle Size Range from 1µm to 3mm

Three modes in 2 modules (dry and wet): X-Fall: for dry and free flowing particlesX-Jet: air pressure dispersion for fine and agglomerated powdersX-Flow: wet module for emulsions and suspensions,

with ultrasonic probe, optional for organic solvents

Modular "X-Change" Concept


Flexible configuration for a wide application range

simple • safe • fast

Dispersion Modules


Dry Dispersion Inserts (2 Plug-In Options)

X- Fall (Gravity dispersion)

X-Jet (Air pressure dispersion)

Dispersion Modules


Dry Dispersion with X-Jet

Measurement range from 1µm to 1.5mm

For fine powders and agglomerating materials

Dry Dispersion by pressurized air: pressure range from 0.2bar to 4.5bar,

3psi – 66psi

Measurement principle – X-Jet



xc_min [µm]50 100 150 200 250 300 3500

10

20

30

40

50

60

70

80

90

Q3 [%]

lactose-20kPa_xc_min_009.rdflactose-30kPa_xc_min_010.rdflactose-50kPa_xc_min_011.rdflactose-100kPa_xc_min_012.rdflactose-150kPa_xc_min_005.rdflactose-200kPa_xc_min_006.rdflactose-300kPa_xc_min_007.rdflactose-460kPa_xc_min_008.rdf

Measurement results with – X-Jet

20, 30 and 50kPa air pressure => stable results / particles don‘t break

100, 150, 200, 300,

460kPa =>

particles break

Lactose Powder


Results of Tin and Lead Solder Powder

Customer had sent 30 different samples to Retsch Technology but some of these samples were the same (red, blue and green). We found out the groups and showed to the customer the good reproducibility of CAMSIZER XT (and proofed his sample splitting as well)

xc_min [µm]10 15 20 25 30 35 40 45 500

10

20

30

40

50

60

70

80

90

Q3 [%]

0

1

2

3

4

5

6

7

8

9

q3 [%/µm]

Solder-Powder-#8-X-Jet-30kPa_vvv_xc_min_Mv.rdfSolder-Powder-#8-X-Jet-30kPa_TP1_vvv_xc_min_001.rdfSolder-Powder-#8-X-Jet-30kPa_TP2_vvv_xc_min_002.rdfSolder-Powder-#13-X-Jet-30kPa_TP1_vvv_xc_min_001.rdfSolder-Powder-#13-X-Jet-30kPa_TP2_vvv_xc_min_002.rdfSolder-Powder-#13-X-Jet-30kPa_vvv_xc_min_Mv.rdfSolder-Powder-#27-X-Jet-30kPa_TP1_vvv_xc_min_001.rdfSolder-Powder-#27-X-Jet-30kPa_TP2_vvv_xc_min_002.rdfSolder-Powder-#27-X-Jet-30kPa_vvv_xc_min_Mv.rdf

Measurement principle – X-Fall


Measurement range from 10µm to 3mm

For free flowing materials

similar to standard CAMSIZER

Sample recovery after analysis

• Complete sample recovery

• No contamination

Dry Dispersion with X-Fall

Measurement principle – X-Fall


Measurement principle – X-Flow


Measurement range from 1 µm to 600 µm for emulsions and suspensions

stronger dispersion with ultrasonic module

Optional for organic solvents

Wet Dispersion with X-Flow

Measurement principle – X-Flow



Pharmaceuticals using Wet Cell

Cancer Pharmaceuticals



Advanced, patented optics design

Sample flow

Light source 2

Light source 1

Basic Camera

Zoom Camera




Sample flow

Light source 2

Light source 1

Basic Camera

Zoom Camera


Features of the CAMSIZER XT

Calibration Reticule



Calibration Reticule

Physical Dynamic Partical Standards


Whitehouse Glass Bead Standard XX030for X-Dry and X-Fall


Particle size

Results X-Flow

Particle Size Distribution 2.5µm + 5µm, Wet Dispersion

X-Change of wet and dry modules in < 1minute





Highlights of the optics setup design:•More than 275 images per second

•Full frame cameras with > 1.3 Megapixel resolution

•Separate light sources for optimised brightness, homogenity, and contrast

•2 Cameras: High resolution combined with excellent statistic

for a wide dynamic range

•Image processing in real-time: Each particle in each image is analysed

•Hundreds of particles in each image: Excellent statistics in short time

CAMSIZER XT can measure in a wider dynamic range with better statistics and reproducibility than any other image processing system

Advantages

fast repeatable and reproducible

maintenance free and robust

precise


Content


InstrumentInstrument

1.Measurement principle

2.2. ResultsResults

Applications



Results


For agglomerating powders

- Metal powder- Coal dust- Wheat flour

Particle size

Velocity Adaption


When you illuminate the backlight two times within one photo you will see every particle two times on the image


v1

v2

v3

Velocity Adaption

Particles of different size have different speeds


v1s1

v2

v3

s2

s3

Velocity Adaption

Particles of different size move different distances


v1s1

v2

v3

s2

s3

v = s/t

Velocity Adaption


Velocity Adaption

Results with and without velocity adaption

xc_min [µm]100 200 300 400 500 600 700 8000

10

20

30

40

50

60

70

80

Q3 [%]

Pharma-Product-30kPa_xc_min_1.rdfPharma-Product--30kPa_xc_min_2.rdfPharma-Product-30kPa_2_xc_min_4.rdfPharmaProduct-30kPa-VitesseAdaption_xc min_8.rdfPharmaProduct-30kPa-VitesseAdaption_xc min_9.rdfPharma-Product-lot002-tamis-Sieve-Analysis.ref

Glass Recycling


xc_min [µm]20 40 60 80 100 120 140 1600

10

20

30

40

50

60

70

80

90

Q3 [%]

17-12-10_Ausgangsmaterial_kl200µm_30kPa_2mm_F0.3_vvv_x17-12-10_Ausgangsmaterial_kl200µm_30kPa_2mm_F0.3_vvv_x17-12-10_Ausgangsmaterial_kl200µm_30kPa_2mm_F0.3_vvv_x17-12-10_Ausgangsmat_kl200µm_30kPa_2mm_Mahlspalt-100_17-12-10_Ausgangsmat_kl200µm_30kPa_2mm_Mahlspalt-100_17-12-10_Ausgangsmaterial_kl200µm_30kPa_2mm_Mahlspalt-117-12-10_Ausgangsmaterial_kl200µm_30kPa_2mm_Mahlspalt-1

Crushed glass in DM 200 (Retsch Disk Mill)

Different gap settings of the disc mill

Results X-Jet


Sample: PMMA Beads

Detection of oversized particles

8 10 12 140

10

20

30

40

50

60

70

80

90

Q3 [%]

CA10 Feed 450CA10 Feed 450CA10 T18 C 45CA10 T18 C 45CA10 T18F-A 4CA10 T18F-A 4CA10 T18F-B 4CA10 T18F-B 4

Cu

mu

lati

ve D

istr

ibu

tio

n

Particle size [µm]

4 Samples:RedGreenBlueViolet

xc_min [µm]13 14 15 16 17 18

99.0

99.2

99.4

99.6

99.8

100.0

Q3 [%]

CA10 Feed 450kpa_xc_min_av.rdfCA10 T18F-B 450kpa_xc_min_av.rdfCA10 T18 C 450kpa_xc_min_av.rdfCA10 T18F-A 450kpa_xc_min_av.rdf

∆ ~ approx 0.5% Vol.

Red with oversized particlesGreen without oversizeBlue with oversized particlesViolet without oversize

Results X-Jet


Identical results to sieve analysis

Results X-Jet


xMa_min [µm]1 2 4 60

5

10

15

20

q3 [%/µm]

PR6 SIKA 4_xMamin_011.rdfPR6 SIKA 4_xMamin_010.rdf

Sample: SiC At the lower resolution limit ........

Particle Size Distribution 1µm -10µm, Dry Dispersion

Particle size


xc_min [µm]2 4 6 8 10 12 140

5

10

15

20

25

q3 [%/µm]

Duke10um12um_gl0_xc_min_009.rdfDuke10um12um_gl0_xc_min_010.rdfDuke10um12um_gl0_xc_min_011.rdf

Particle Size Distribution 10µm + 12µm, Wet Dispersion

Results X-Flow (Calibration)

xc_min [µm]4 6 8 10 120

5

10

15

20

25

30

35

40

45

50

q3 [%/µm]

Duke10um12um_gl0_xc_min_009.rdfDuke10um12um_gl0_xc_min_010.rdfDuke10um12um_gl0_xc_min_011.rdfDuke10um_xc_min_002.rdfDuke10um_xc_min_003.rdfDuke10um_xc_min_004.rdf


Particle size

Results X-Flow (Calibration)

Particle Size Distribution 10µm + 12µm, Wet Dispersion

Results X-Jet


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

Shape Analysis with CAMSIZER XT


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

Results X-Flow


b/l0.4 0.5 0.6 0.7 0.8 0.90

10

20

30

40

50

60

70

80

90

Q3 [%]

A32L 2__xc_min_001.rdfA32L 2__xc_min_002.rdfA32L 2__xc_min_003.rdfA32L 2__xc_min_004.rdfA32L 2__xc_min_005.rdf

Shape analysis for detection of broken particles:„What you see is what you get“

broken round

Length and shape numbers for single particles, from real pictures

Precise analysis of the amount of broken particles by shape

detection

Sample: Glass beads, multimodal

Results X-Fall


Excellent repeatabilty and detection efficiency for „large particles“ and small sample volumes

• Digital image processing with patented 2-camera system (ISO 13322-2)

• wide dynamic range from 1µm to > 3mm

• newly developed optical system with ultra bright LEDs for sharp contrasts and large depth of focus

• short analysis time 1 – 3 minutes for few million particles

• safe detection of oversized and undersized

• modules for dry and wet dispersion

• analysis results optionally compatible to sieve analysis

Advantages


Content


Instrument


2.Results

ApplicationsApplications

3.3. Markets and applicationsMarkets and applications


• Industrial labs

• Research institutes

• Production control

• Quality control for final products

• Quality control of incoming raw materials

• Immediate control and optimisation of

production processes

Application areas


Application areas


Typical sample materials

• Pharmaceutical powders, granules or

small pellets

• Pulverized and granulated food, spices

• Detergents, enzymes, fillers for washing powders

• Metal or ore powders

• Abrasives (medium and small grit)

• Sand and cement, building materials, limestone

• Fibres

Content


Instrument


2.Results

ApplicationsApplications


4.4. Alternative analysis methodsAlternative analysis methods

Alternative Methods


Sieving CAMSIZER XTSize range 10µm - 63mm 1µm – 3mmShape analysis no yesDetection of oversized particles each particle few big particles

from < 0.1% Vol.Resolution poor high resolution

Multi-modal distributions poor size resolution better resolution

Repeatability and lab-to-lab comparison „difficult“ superior

Comparison with sieving identical results possible

Handling simple, but time consuming easy and fast

Sieving CAMSIZER XT


Results X-Jet


Identical results to sieve analysis

xc_min [mm]0.1 0.2 0.3 0.4 0.5 0.6 0.70

10

20

30

40

50

60

70

80

90

Q3 [%]

Ca-hydrogenphosphate_100kPa-T38567-vvv_xc_min_005.rdfCa-hydrogenphosphate_100kPa-T38567-vvv_xc_min_003.rdfCa-hydrogenphosphate_100kPa-T38567-vvv_xc_min_004.rdfT38567-Sieve-Analysis-Customer-Site.ref


Sieving CAMSIZER XT

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

xc min = = d = Xc min

particle-width


Sieving CAMSIZER XT

Influence of Mesh Width

1400µm 1400µm 1429.5µm

Mesh sizes warpMesh 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 ~1455µm sieve No. 03033531 (nominal 1400µm)

Theory: Reality:


Sieving CAMSIZER XT

Real Mesh Width

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


Sample Reproducibility of CAMSIZER XT measurements of xc min (red, and blue) with Basic + Zoom or Zoom only, Retsch sieve result (real mesh sizes from optical inspection) AS 200 TAB (*black), Customer nominal sieve results (*blue)


xc_min [µm]10 20 30 40 500

10

20

30

40

50

60

70

80

90

Q3 [%]Solder_Sample_G_xc_min_001.rdfSolder_Sample_G_xc_min_002.rdfSolder_Sample_G_xc_min_003.rdfTin-Solder_Sample_G__xc_min_001.rdfTin-Solder_Sample_G__xc_min_002.rdfTin-Solder_Sample_G__xc_min_003.rdfRT1763 Sieve-Analysis G customer-site-nominal.refRT1763 Sieve-Analysis_G_AS200tap_real-sizes.ref


Glass Recycling

Crushed GlassSimilar results to sieve analysis

xc_min [µm]20 40 60 80 100 120 1400

10

20

30

40

50

60

70

80

90

Q3 [%]

17-12-10_smaller 50µm-white_30kPa_2mm_vvv_xc_min_002.rdf15-12-10_smaller 50µm-white-Lab_30kPa_2mm_vvv_xc_min_001.rdfRT1798_Customer-Sieve -Analysis smaller 50µm_white_Ha.ref

Applications: Metal powdersMaterial: Cu


Identical results to the sieve analysis

xc_min [mm]0.04 0.1 0.2 0.4 1 20

10

20

30

40

50

60

70

80

90

Q3 [%]

Automatic reports,many languages

available


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


Glass Recycling

Very Acicular and Angular Particles

without and with Elementary Fitting

xc_min [µm]100 200 300 400 500 6000

10

20

30

40

50

60

70

80

90

Q3 [%]

15-12 50-100µm-gray_30kPa_2mm_vvv_xc_min_001.rdfRT1798_Customer-Sieve-Analysis_50-100µm_gray.ref

xc_min [µm]100 200 300 400 5000

10

20

30

40

50

60

70

80

90

Q3 [%]

15-12 50-100µm-gray_30kPa_2mm_vvv_xc_min_001.rdfRT1798_Customer-Sieve-Analysis_50-100µm_gray.ref

CAMSIZER XT Laser sizer


Laser sizer CAMSIZER XTSize range down to 20nm > 1µmShape analysis no yesDetection of oversized particles percent range few big particles

< 0.1% Vol.

Resolution good for fines better resolution for large particles

Multi-modal distributions more difficult better volume model, better size resolution

Comparison with sieving not possible identical results

Information content black box + mathematics pictures

Results X-Jet


200 400 600 800 1000 1200 14000

10

20

30

40

50

60

70

80

90

Q3 [%]

PR1 10089 Grov_xMamin_001.rdfRT1686_Elkem1_sieb.refRT1686 1089 coarse M2000.ref

Sample: Petrolcoke for Electrodes

Reliable results, closer to sieving

Particle size [µm]

Cum

ulat

ive

Dis

tribu

tion

CAMSIZERSievingLaser diffraction (customer results)

100 200 300 400 500 600 700 8000

10

20

30

40

50

60

70

80

90

Q3 [%]

PR4 10086 Grov Senter_xMamin_0RT1686 10086 coarse ELKEM.refRT1686_Elkem4_sieb.ref

CAMSIZERSieving (Retsch AS200)Sieving (customer results)

Particle size [µm]

Cum

ulat

ive

Dis

tribu

tion

CAMSIZER XT Optical Microscope


Microscope CAMSIZER XTSize range 0.5 – 500 µm 1 µm -3 mm

Shape analysis yessuperior image quality yes

Detection of oversized particles no few big particles

< 0.1% Vol.Resolution better good

Statistics Low,few 1,000 particles million particles/minute

Comparison with sieving not possible identical results possible

Handling time consuming fastRepresentative Sample Amounts

difficult, only narrow distributions

yes, small and large amounts


xc_min [µm]200 400 600 800 10000

10

20

30

40

50

60

70

80

90

Q3 [%]

PPO-646_xc_min_001.rdfRT1766_ppo646_sieve.ref



CAMSIZER XT CAMSIZER

CAMSIZER CAMSIZER XTSize range 30 µm – 30mm 1 µm -3 mmShape analysis yes yesDetection of oversized particles yes yes

Images / second 60 277Resolution CCD-Cameras 790,000 1,300,000

Comparison with sieving identical results possible

identical results possible

Handling fast fastRepresentative Sample Amounts




Comparison of CAMSIZER and CAMSIZER XT

Results of CAMSIZER (black) and CAMSIZER-XT (red) of sample #30

CAMSIZER distribution is wider, the results are not that accurate and repeatable as results from CAMSIZER XT.


xc_min [µm]15 20 25 30 35 40 45 500

10

20

30

40

50

60

70

80

90

Q3 [%]

Solder-XT-with-X-Jet-#30-Einzel-250kPa_xc_min_005.rdfSolder-XT-with-X-Jet-#30-Einzel-250kPa_xc_min_006.rdfSolder-XT-with-X-Jet-#30-Einzel-250kPa_xc_min_007.rdfSolder-XT-with-X-Jet-#30-Einzel-250kPa_xc_min_008.rdf#30-classic-CAMSIZER-Repeatability-xc_min_013.rdf#30-classic-CAMSIZER-Repeatability-xc_min_014.rdf#30-classic-CAMSIZER-Repeatability-xc_min_015.rdf#30-classic-CAMSIZER-Repeatability-xc_min_Mv.rdf

Thank you for your attention!

camsizer xt - horiba · camsizer xt - the latest in dynamic image analysis webinar wednesday, 14th...

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