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

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Nanopartikel Größenmessung

leicht gemacht!

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

Nanoparticles

gold nanoparticle in water

size: 5 – 10 nm

Bulkphase of gold

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

Colloids

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)

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

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

Signal at the detector

Log intensity

time Noise

homodyne

heterodyne

180° heterodyne back scattering (DLS)

• 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

Applications

Different ways of measurement

drop in nearly every vessel online with Stabino®

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

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

Application: high resolution and differentiation

100 nm

200 nm

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

Application: different concentrations in a mix

Application: ink

white ink

cyan ink

white and cyan ink in original concentrations

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

Application: Filtration control

Application: Gushing inducing particles

Haffmans ISD INPACK 200

SAMPLING DEVICE

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

Application: chitosan

Application: ONLINE in-situ size measurement

Time / min

Application: size & concentration

Application: molecular weight measurement

NANO-flex® Online

Variable probe length

Up to 3.5m flexible tube

Pressure measurement

cell

Remote control of

Software

Combination of Stabino® & NANO-flex®

Combination of Stabino® & NANO-flex®

Remote controlled form

Stabino® Software

Application (pH): Al2O3 with size measurement

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

Summary

MANY THANKS

FOR

YOUR ATTENTION