Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm ....

33
Nanopartikel Größenmessung leicht gemacht!

Transcript of Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm ....

Page 1: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Nanopartikel Größenmessung

leicht gemacht!

Page 2: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Content • Basics

– General basics

– Measurement basics

• Applications

– Strengths and limits off DLS

– Measurement examples

– Online measurement

– Concentration and molecular weight measurement

• Different setups of the systems

– Online, Cuvettes

• Combination with Stabino®

• Summary

Page 3: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Nanoparticles

gold nanoparticle in water

size: 5 – 10 nm

Bulkphase of gold

Page 4: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

What are Colloids?

• Macromolecules in solution

– < 1nm – 10 nm

• Particles dispersed in liquids

– < 1 nm – 10 µm

• > 20 nm turbid

clear

turbid > 20 nm

1 nm

100 nm

Page 5: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Colloids

Page 6: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Methods of Light Scattering (LS)

Q

I

t

I

%

size/µm

Static LS Dynamic LS

10nm – 2mm 0.8nm – 6,5µm

FFT Mie

Q

Static LS (SLS):

The information on

size is in the angle

function

Dynamic LS (DLS)

The information on

size is in the

fluctuation of the

scattering signal

(Brownian motion)

Page 7: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

DLS - Stokes-Einstein-relation

• To calculate particle size:

• 𝑟 =R·𝑇

𝑫·6π·𝜂·NA

• r = particle radius; D = diffusion coefficient; R = gas constant; NA =

Avogadro‘s constant; = viscosity of continuous phase and T =

temperature

Page 8: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Laser

Scattered light

from particles

Detector

Laser in &

reflected laser

Scattered &

reflected

light

Size & concentration

0.01 – 40 vol%

Homodyne Heterodyne

K: colloid D: detector O: imaging optics R: partial reflecting surface

180° heterodyne back scattering (DLS)

highest possible concentration

from transparent to carbon black

No multiple scattering

Page 9: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Signal at the detector

Log intensity

time Noise

homodyne

heterodyne

Page 10: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

180° heterodyne back scattering (DLS)

Page 11: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

• size 0.8 nm (0,3 nm) – 6.5 µm (10 µm)

• Concentration up to 40 vol.%

• Minimum sample volume 10 µL

• Molecular weight by Debye Plot dn/dc

• Online or inline Measurements are possible

• Cuvettes

• Zeta potential option with Stabino® / ZETA-

Check

Specifications

Page 12: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Applications

Page 13: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Different ways of measurement

drop in nearly every vessel online with Stabino®

Page 14: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

NANO-flex® Applications

• protein

• drinks

• lysozyme

• liposome

• humic acid

• fullerene

• diamond

• CNTs

• quantum Dots

• emulsion

• metal oxide

• polymer dispersions

• printing ink

• coatings

• and much more

Page 15: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

3790 nm

711 nm

83.9 nm

Dia / nm

measured

Vol %

measured

Dia /nm

theoretical

Vol %

theoretical

83.9 11.7 % 95.6 33.74 %

711 76.8 % 746 63.22 %

3790 11.5 % 4760 3.04 %

Application: three modal latex beads mixture

Page 16: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Application: high resolution and differentiation

100 nm

200 nm

Page 17: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

5 drops 20 nm PS in 1 mL water 5 drops 20 nm PS in 1 mL water + 1 drop 100 nm PS

20 drops 20 nm PS in 1 mL water + 1 drop 100 nm PS

Application: different concentrations in a mix

25 drops 20 nm PS in 1 mL water + 1 drop 100 nm PS

Page 18: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Application: different concentrations in a mix

Page 19: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Application: ink

white ink

cyan ink

white and cyan ink in original concentrations

Page 20: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Application: ceramics

50 w% ceramic slurry with a liquid agent at pH 9

50 w% ceramic slurry with a liquid agent at pH 1

D 50 = 462 nm

D 50 = 299 nm

Page 21: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Application: Filtration control

Page 22: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Application: Gushing inducing particles

Haffmans ISD INPACK 200

SAMPLING DEVICE

red: gushing; green: tendency to gushing; blue: no gushing

Page 23: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Application: chitosan

Page 24: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Application: ONLINE in-situ size measurement

Time / min

Page 25: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Application: size & concentration

Page 26: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Application: molecular weight measurement

Page 27: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

NANO-flex® Online

Variable probe length

Up to 3.5m flexible tube

Pressure measurement

cell

Remote control of

Software

Page 28: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Combination of Stabino® & NANO-flex®

Page 29: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Combination of Stabino® & NANO-flex®

Remote controlled form

Stabino® Software

Page 30: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Application (pH): Al2O3 with size measurement

Page 31: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Summary

High concentration

High dynamic range AND high resolution

Organic and aqueous solutions

Online Measurement

Remote Control

Presentation of sample in any vessel including cuvettes and drops

Combination with Stabino® for particle charge measurement and

titrations

Page 32: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

Summary

Page 33: Nanopartikel Größenmessung leicht gemacht! - Colloid Metrix€¦ · D 50 = 462 nm D 50 = 299 nm . Application: Filtration control . Application: Gushing inducing particles Haffmans

MANY THANKS

FOR

YOUR ATTENTION