Experiment No: 6

Experiment Name: Particle size analysis using Laser Particle size analyzer

I. Aim: To determine the average particle size and particle size distribution of (sample name) by wet
dispersion method

II. Procedure:
Steps for Analysis:

Step 1: Switch ON sequence

• Power ON the Hydro 2000 MU along with optical unit(at least 30 min before starting the analysis
for Laser stabilization)
• Power ON the PC

Step 2: Cleaning the Optical unit

• Ensure that the arm of the Hydro is lowered and rinsing or cleaning fluid is filled in the sample
beaker before starting the analysis (at least 650 ml of dispersant)
• Set the pump speed at 4000 rpm and ultrasonic displacement as required
• Press Pump ON on the keypad to start the pump for cleaning the Flow cell
• Clean the Flow cell (optical device) with the dispersant for about three times
• Fill the beaker with clear dispersant, set the pump speed at 2000 rpm and ultrasonic displacement
as required

Step 3: Steps for handling the software to run the analysis

• Open the Mastersizer 2000 software
• Select Measurement and choose Manual option
• Now analysis window will be displayed and at the bottom of the window “When the sample is
clean and ready for measurement, click start” message will appear
• Don’t click “Start” right now

• Go to Options Material enter Sample material name and Dispersant name (for
others select from the list) and click ok
• Select Documentation enter sample name and source name (user name), click ok
• Now click START to start the analysis, wait for background and laser obscuration.

Step 3: Loading of sample

• Add the sample slowly into the beaker containing dispersant until the “LASER
OBSCURATION IS BETWEEN 10 TO 20 %” (~12% — indicated by blue bar rising into the
green area from the red on the window)
• When the obscuration level being achieved click START again
• The detector array will start to take over 2000 snap shots (1ms for each snap shot) of the
scattering patterns for the measurement and averages the results.

Step 4: For collection of results

• Right click the files of interest result analysis Batch print save
III. Results and analysis:

1. Instrument name (make and model) :

2. Measurement:
3. Size range of the instrument:
4. Laser beam source:
5. Sample details:
6. Sonication time:
7. Method:

Observations:
(i) Volume mean diameter (VMD) : µm
(ii) Surface mean diameter (SMD) : µm
(iii) d(0.5) (Mass Mean Diameter) :
(iv) d(0.9) : µm
(v) d(0.1) : µm
(vi) Particle size distribution range: µm

Calculate :

(vii) Average particle size: µm

(viii) Geometric mean : µm

IV. Precautions to be taken :

1. Lifting and lowering the Hydro pump arm needs utmost care while cleaning
2. Set the required pump speed for cleaning and while analyzing the samples
3. Make sure that you drained all the water from the flow cell during the cleaning step
4. Wait for light obscuration and background measurements before starting the experiments
5. Should not operate the motor of Hydro MU for a long time (i.e., more than one hour)
6. Don’t shift/shake/vibrate the instrument. Otherwise it will spoil the alignment.
7. Don’t analyze “OIL SAMPLE”.

V. Example analysis

Aim : Determination of the average particle size and particle size distribution of TiO2 by wet dispersion
method
Results and analysis:
1. Measurement: Mie scattering
2. Size range of the instrument: 0.02 to 2000 Micron
3. Laser beam source: Helium-Neon laser source
4. Sample details: 0.2 g of TiO2 dispersed in 50 ml of dispersant
5. Sonication time: 15 min
6. Method: Wet dispersion method
Observations:
From the particle size analysis, various particle size values were computed :
1. Volume mean diameter (VMD) : 1.166 µm
2. Surface mean diameter (SMD) : 0.566 µm
3. d(0.5) (Mass Mean Diameter) : 0.622 µm.
4. d(0.9) : 1.251 µm
5. d(0.1) : 0.332 µm
6. Particle size distribution range: 0.138 and 69.183µm
7. Average particle size: 11.41
8. Geometric mean :3.1 µm

Note: d (0.5) is the size in microns at which 50% of the sample has particles with a larger
diameter and 50% of the sample has particles with a smaller diameter than this size

d (0.9) is the size of the particles below which 90% of the sample lies

d (0.1) gives a size of particles below which 10% of the sample lies