CL-610 Experimental Lab

Exp. No. 16
​

​DYNAMIC LIGHT SCATTERING

​Experiment performed on : 19th, February,2019

Submitted by batch T2

Prachee Prabhutendolkar (183020047)

Taufique Akbar (183020052)

Instructors
Prof. Jyoti Seth
Prof. Y S Mayya
Prof. Rajdeep Bandopadhya

Department of Chemical Engineering,Indian Institute of Technology, Bombay.

Table of Content

Aim: 2

Introduction: 2

Theory: 3

Experimental Setup : 4

Procedure : 4

Results: 5

Table of Figures

Fig 1: Light Scattering due to particles.

Fig 2: Correlation Factor

Fig 3: Experimental Setup

Aim:
To determine the particle size distribution of a given sample by Dynamic Light Scattering (DLS) method
using Malvern zetasizer.

Introduction:
Particle size which is a valuable indicator of quality and performance and influences many properties of
particulate materials. This is true for powders, suspensions, emulsions, and aerosols. The PSD of a
material can be important in understanding in physical and chemical properties. The strength and
load-bearing properties of rocks and soils can be affected. It affects the reactivity of solids participating
in chemical reactions and the performance of a catalyst for a solid catalyzed reaction.

The size and shape of powders influences flow and compaction properties. Larger, more
spherical particles will typically flow more easily than smaller or high aspect ratio particles. Smaller
particles dissolve more quickly and lead to higher suspension viscosities than larger ones. Smaller
droplet sizes and higher surface charge (zeta potential) will typically improve suspension and emulsion
stability. The better aerosol can be prepared in the range of droplets of 2-5µm and will penetrate into
lungs deeper than larger sizes. For these and many other reasons it is important to measure and control
the particle size distribution of many products. The most important methods for the characterization of
particles in the nanometer and micrometer range are dynamic and static laser light scattering (laser
diffraction).

Theory:
Dynamic Light Scattering (DLS) a technique in physics that can be used to determine the size distribution
profile of small particles in suspension or polymers in solution. In the scope of DLS, temporal
fluctuations are usually analyzed by means of the intensity or photon auto-correlation function (also
known as photon correlation spectroscopy or quasi-elastic light scattering).The amount of light
scattered depends upon the particle size of the sample i.e. more amount of light is scattered for smaller
particles and less amount of light is scattered for larger particles. This scattered light interfere
constructively and destructively which leads to the formation of dark and bright areas on the detector
also known as speckle patterns.
 Fig 1: Light Scattering due to particles.

Due to Brownian motion movement of particles due to the random collision with themolecules of the
liquid that surrounds the particle the corresponding speckle patterns of changes and the change in
speckle pattern is analyzed by an auto correlator that compares the intensity of light at each spot over
time. If there is no change in the speckle patterns or speckle patterns are similar than correlation factor
is close to one and if two speckle patterns are very different than correlation factor is zero. Since smaller
particles have higher brownian motion the correlation factor decays faster over consecutive readings
vice versa for larger particles. The relationship between the size of a particle and its speed due to
Brownian motion is defined in the Stokes-Einstein equation.

Fig 2: Correlation Factor

Experimental Setup :
A monochromatic light source, usually a laser, is shot through a polarizer and into a sample. The
scattered light then goes through a second polarizer where it is collected by a photomultiplier and the
resulting image is projected onto a screen. This is known as a speckle pattern. All of the molecules in the
solution are being hit with the light and all of the molecules diffract the light in all directions. The
diffracted light from all of the molecules can either interfere constructively (light regions) or
destructively (dark regions). This process is repeated at short time intervals and the resulting set of
speckle patterns are analyzed by an auto correlator that compares the intensity of light at each spot
over time. The polarizers can be set up in two geometrical configurations. One is a vertical/vertical (VV)
geometry, where the second polarizer allows light through that is in the same direction as the primary
polarizer. In vertical/horizontal (VH) geometry the second polarizer allows light not in same direction as
the incident light.

Fig 3: Experimental Setup

Procedure :
1. Create a diluted sample of required concentration using deionized water according to particle size
distribution. Here we used silica in double distilled water (LUDOX).

2. Wash the vile/cuvette with distilled water and then rinse using the solution and fill half vile/cuvette
with the solution.

3. Put the vile inside the equipment with transparent side of the vile facing towards the laser.

4. Open the software (Zetasizer) and create a new measurement file.

5. Open Measure tab and set the required fields such as Sample name, Refractive Index as 1.475 and
temperature as 25°C.

6. Click on the dispersant tab and set it as water and set the equilibration time as 60 sec.

7. Select wide angle measurement of 173° and the cell type as Quartz.

8. Specify the number of measurements and start the experiment.

9. Finally export the results through data processing.

Results:
The results of the experiments are as follows:

SAMPLE PARTICLE SIZE

(nm)
1 30.67
2 30.92
3 31.19
Mean 30.92