Overview of HORIBA Particle Technologies Final.ppt · 2012-04-13 · Microsoft PowerPoint -...

© 2012 HORIBA, Ltd. All rights reserved.

Overview of HORIBA Particle TechnologiesSize, Shape, Zeta Potential, and Surface Area

Mark Bumiller &

Ian Treviranuswww.horiba.com/particle


Who are HORIBA?

I admit I had no ideaOmoshiro Okashiku

Headquartered in Kyoto, JapanFounded in 1945

We’ve come a long way


Scientific• Synergy of HORIBA and

HORIBA Jobin Yvon’s Technologies • Raman, Grating, and Fluorescence

Business SegmentsAutomotive Test Systems• Emission Measurement Systems (EMS)• Mechatronics Devices (MCT) • Test Automation Systems (TAS)

Process & Environmental• Environmental Systems• Environmental Regulation & Process Business

Semiconductor• Mass Flow Controller• In-situ Analysis• Synergy among HORIBA HQ, HORIBA STEC and

HORIBA Jobin Yvon’s Technologies

Medical• In-Vitro Diagnostic (IVD) Systems• Integration of HORIBA ABX’s

Technology & Marketing Know-How


Numbers at a glance

5,000+ employees worldwideFamily-operated Offices in Japan, France,

Germany, Austria, UK, Korea, China, India, Thailand, Singapore, Canada, Brazil, and USAFive business segments PSA is part of Scientific

$1.5B annual sales, growing


What we’ll talk about

LA-950Laser Diffraction

SZ-100Dynamic Light Scattering & Zeta Potential

CAMSIZER & CAMSIZER XTDynamic Image Analysis

PSA300Static Image Analysis

SA-9600Flowing Gas BET Surface Area


LA-950: Laser Diffraction

Particle size performance leaderNinth generationUltra durableLowest total cost of ownershipSuspension, emulsion, powder,

paste, gel10 nanometer – 3 mm


Dynamic Range 0.01 – 3000 µmWidest wet measurement rangeOnly system to measure 30 nm!

30 nm silica 40 nm latex


Low End Sensitivity

30, 40, 50, 70 nm latex standards overlay of individual runs

Shorter wavelength = better pattern


Large Particle Detection

q(

%)

Diameter(µm)

0

14

2

4

6

8

10

12

10.00 3000100.0 10000

100

10

20

30

40

50

60

70

80

90Coffee Results

Need exceptionally stable optical benchVertical design means no density limit

for dry


Smaller Sample Volume

5 ml 35 ml 100 ml

•Wide range of sample cells depending on application•High sensitivity keeps sample requirements at minimum•Powerful dispersion with 130W 20kHz ultrasonic probe

• High power, low freq. = faster deagglomeration


MiniFlow Accessory

Auto fill pump Circulation pump 30W ultrasonic40 mL volume Max. chemical resistance Auto rinse

Application Note 176: Minimizing Sample Quantity


Superior Dry Powder Feeder

Direct flow ofpowder down tocell rather thanturn 90o, thenaround plastic tube, no densityrestriction likehorizontal units, zero impact surfaces meansgood dispersionw/o comminution

Webinar TE016: Optimizing Dry Powder Measurements


Superior Dry Powder Feeder

Automatic control of sample feed rateLA-950 monitors amount of sample

supplied by the vibratory feeder. Automatic feed back control keeps constant mass flow rate of powder during measurementThis is CRITICAL

– More reproducible, robust– No ghost peaks– No cutting off results– Fewer headaches!

Unique to HORIBA


Software Automation


LA-950 Method Expert

Unique guided method developmentOptimize parameters Choose the best refractive index Create “one button” SOPs


SZ-100: Nanoparticle Analyzer Size: .3 nm - 8 µm

90° and 173° Zeta potential: -200 - +200 mV

Patented carbon coated electrodes

Molecular weight: 1x103 - 2x107 g/mol Optional titrator

•Nanoparticles•Colloids•Proteins•Emulsions•Disperison stability


-60

-50

-40

-30

-20

-10

0

10

20

30

40

50

60

2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0

pH

Zeta potential/mV

Measures particle surface chargeHigh zeta potential = stableLow zeta = unstable, aggregate

Zeta Potential: Dispersion Stability, IEP


Zeta Potential Cells

-10

-5

0

5

10

15

20

0 2 4 6 8 10 12 14

pH

zeta

pot

entia

l

Gold coated electrodes (ruined) Carbon coated electrodes

IEP 3.4 nm protein 800 measurements with one cell


Two Approaches

Dynamic:particles flow past camera

Static:particles fixed on slide,stage moves slide


CAMSIZER: Image Analysis

High resolution size & shape Intelligent sieve correlationPatented dual capture30 micron – 30 millimeter


CAMSIZER XT: Fine Image Analysis

High resolution size & shapeExtends lower detection rangeCohesive & free-flowing powders,

suspensions1 micron – 3 millimeter


X-Jet Dry Powder Dispersion

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

Cum

ulat

ive

Dis

trib

utio

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


Advantage of Image Analysis

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


Shape Analysis

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

Equivalent spherical diameter

Perimeter

Longest diameter

Shortest daimeter

Area


CAMSIZER Comparison

CAMSIZER CAMSIZER XTSize range 30 µm – 30mm 1 µm -3 mmShape analysis yes yesDetection of oversized particles yes yesImages / second 60 277Resolution CCD-Cameras 790,000 1,300,000

Comparison with sieving identical results possible identical resultspossible

Handling fast fast

Representative Sample Amounts yes, small and large amounts

yes, small and large amounts


Two Approaches

Dynamic:particles flow past camera

Static:particles fixed on slide,stage moves slide


Image Acquisition and enhancement

Thresholding

Image Processing

Measurements

Objective &camera

Subjective orautomatic

Decisions orblack box

Advantages:Quick size + shape infoStatistically validHigh resolutionParticle images

Disadvantages:ExpenseKnowing which numbers are important

Automated Microscopy


Case Study: Effect of Number Counted

0

5

10

15

20

25

0 200 400 600 800 1000 1200 1400 1600

d10 d50 d90

Number of particles required n*, = 0.05, p = 0.95 GSD n*(MMD) n*(Sauter) n*(MVD)

0.05 1.1 585 389 1311.15 1460 934 2941.2 2939 1808 528

1.25 5223 3103 8431.3 8526 4920 1247

1.35 13059 7355 17501.4 19026 10504 2363

1.45 26617 14457 30931.5 36007 19295 3956

1.55 47358 25093 49521.6 60811 31919 6092


Acilcular Separation:

Fiber Separation


SA-9600: BET Surface Area

Surface area affects:Dissolution, reaction, combustion, hydration

Fastest measurement timeDynamic (flowing gas) vs. static (volumetric)

QC: easy to use, high throughputLowest total cost of ownershipFull software controlTSA: 0.1 – 50 meter squared


Method Comparison

Dynamic (Flowing-Gas)

Faster Easy to use Increased sensitivity

to low SSA materials Higher throughput Lower operating costs Lower service costs

Static(Volumetric)

Slower Easy to use Low SSA longer

measurement times Lower throughput Higher operating costs Higher service costs


The SA-9600 Surface Area Analyzer

Out-gassing station

Analysis station

Liquid N2 bath


SA-9600 Surface Area Analyzer

0.1 - >2000 m2/gSingle or multi-point analysisOne or three station systemsSingle point: up to 30 analyses

per hourHigh value route to quick and

easy surface area analysis


To Learn More: www.horiba.com/particle

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View application/technical notes (>130), webinars (>40), white papers.

Talk to us, ask questions


Danke

Gracias

Большое спасибо

GrazieاُشْكرΣας ευχαριστούμε

감사합니다 Obrigado

Tacka dig

谢谢ขอบคุณครบั

ありがとうございました

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Overview of HORIBA Particle Technologies Final.ppt · 2012-04-13 · Microsoft PowerPoint -...

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