CL610: EXPERIMENTAL METHODS

EXPERIMENT NO: 12

PARTICLE SIZE ANALYSIS

Date of Experiment Performed: 29-01-2018

Date of Draft Report Submission: 5-02-2018

Date of Final Report Submission: 12-02-2018

BATCH: M10

Rahul C R (183020058)

INSTRUCTORS: PROF. V.A. JUVEKAR

PROF. Y.S. MAYYA

DEPARTMENT OF CHEMICAL ENGINEERING

INDIAN INSTITUTE OF TECHNOLOGY, BOMBAY

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 CONTENTS

1. Objective 4

2. Theory & Principle 4

3. Apparatus and chemicals 5

4. Procedure 5

5. Calculations 6

6. Results and Discussion 7

7. Precautions 11

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 LIST OF FIGURES AND TABLES

Fig 1: Particle size analyzer ( LA-960 ) 5

Fig 2: Histogram Plot of Silica Particles Size Distribution 7

Fig 3: Histogram Plot of CaCO3 Particles Size Distribution 7

Fig 4: Histogram Plot of Silica-CaCO3 75-25%mixture Particles Size Distribution 8

Fig 5: Histogram Plot of Silica-CaCO3 75-25%mixture Particles Size Distribution 8

Fig 6: Histogram Plot of Glass Particles Size Distribution 9

Fig 7: Particle Size distribution of all samples 10

Fig 8: Cumulative Particle Size distribution of all samples 10

Table 1: Distribution Properties of all samples 8

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OBJECTIVE

i) To determine the particle size distribution of Silica, CaCO3, Silica-CaCO3 50-50%,Silica-

CaCO3 75-25% mixture and glass powder sample using Laser Scattering Particle size
Distribution analyzer LA-960.
ii) To find out Mean, Mode, Median, Variance and standard deviation of each sample.

THEORY

Particle size distribution influences rate of reaction, potential to dissolve, packing density,
sedimentation, effectiveness of drug delivery by inhalation, product appearance etc. It is also
important in understanding its physical and chemical properties. Particles in nano-meter and
micro-meter range can be characterized by dynamic and static laser light scattering (laser
diffraction). Analysis of emulsions, suspensions and dry samples can be done using static laser
light scattering. 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. Powder or droplets in the range of 2-5μm aerosolize
better and will penetrate into lungs deeper than larger sizes.

Particle size distribution can greatly affect the efficiency of any collection device. Settling
chambers will normally only collect very large particles, those that can be separated using sieve
trays. Centrifugal collectors will normally collect particles down to about 20 μm. Higher
efficiency models can collect particles down to 10 μm. Fabric filters are one of the most efficient
and cost effective types of dust collectors available and can achieve a collection efficiency of
more than 99% for very fine particles. Wet scrubbers that use liquid are commonly known as
wet scrubbers. In these systems, the scrubbing liquid (usually water) comes into contact with a
gas stream containing dust particles. The greater the contact of the gas and liquid streams, the
higher the dust removal efficiency. . They can be very efficient at the collection of very fine
particles. Filter Press used for filtering liquids by cake filtration mechanism. The PSD plays an
important part in the cake formation, cake resistance, and cake characteristics. The filterability
of the liquid is determined largely by the size of the particles.

PRINCIPLE

The amplitude of scattered light at different angles (the scattering pattern) depends not only on
concentration and particle size, but also on the ratio of the refractive indices of the particles to
the medium in which the particle exists. The more the particles differ from the medium (i.e. the
more their refractive indices differ), the more light will be scattered by the particles. At the other
extreme, if there is no difference in refractive indices, no light will be scattered It shows incident
light beams (assume intensity I and wavelength λ) in close proximity with a spherical particle.
Photons in one ray are sufficiently far away from the particle to have no interaction and are
unaffected by its presence. Another beam comes close enough to be diffracted by interaction

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with the edge of the particle. Another beam intersects the particle. Some photons are reflected;
others penetrate the surface and, in doing so, are refracted. The refracted ray of photons strikes
the far side of the particle.

Laser diffraction measures particle size distributions by measuring the angular variation in
intensity of light scattered as a laser beam passes through a dispersed particulate sample. Large
particles scatter light at small angles relative to the laser beam and small particles scatter light
at large angles. The angular scattering intensity data is then analysed to calculate the size of the
particles responsible for creating the scattering pattern, using the Mie theory of light scattering.
The particle size is reported as a volume equivalent sphere diameter.

Fig 1: Particle Size Analyser

APPARATUS AND CHEMICALS

• Particle size analyzer LA-960 .

• Spatula spoon.
• Silica Powder, Calcium carbonate powder,Silica-CaC03 50-50 %mixture, Silica-CaC03 75-
25 % mixture.

PROCEDURE

1. Start LA-960 electronic display and go to advance then set mode and then choose dry.
2. Feed the Samples on the top of analyser on the given space and adjust the convex
mirror to see sample when operating.

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 3. Set sample, Refractive index of sample etc.
4. Click for measurement screen and set feeder amplitude automatic.
5. First switch vacuum button then air then alignment then blank and then feed.
6. Click on measurement button after which measurement will begin and particle size
distribution will be displayed as a histogram plot.
7. Repeat the same procedure for all the samples taken.

CALCULATIONS

Mean:

Mean Size = ∑ {q(J) *X{J}/ ∑{ q(J)}.

J: Particle Diameter Division Number.

q (J): Frequency Distribution value (%).

X {J}: Jth particle Diameter in micro-meter.

Variance:

Variance = ∑ [(X(J) - Mean)2*q(J)/100] .

Median Size:

Median is the cumulative particle diameters equivalent to 50%.

Mode Size:

Frequency distribution value’s largest values that become particle diameter of the frequency
distribution graph’s peak.

Standard Deviation (SD):

Value taken from arithmetic distribution value’s square root.

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RESULTS AND DISCUSSION

HISTOGRAM PLOTS

Fig 2: Histogram Plot of Silica Particles Size Distribution

Fig 3: Histogram Plot of CaCO3 Particles Size Distribution

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Fig 4: Histogram Plot of Silica-CaCO3 75-25% mixture Particles Size Distribution

Fig 5: Histogram Plot of Silica-CaCO3 50-50% mixture Particles Size Distribution

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 Fig 6: Histogram Plot of Glass Particles Size Distribution

Sample Mean Mean Volumetric Median Mode Variance SD % Error

(µm) cal. (µm) Mean(µm) (µm) (µm) (µm)2 (µm)

Silica 250.98 268.60 383.60 236.144 242.51 7826.94 88.47 7.02

CaCO3 8.119 8.69 29.78 6.965 7.153 26.14 5.1137 7.03

Silica 141.257 151.177 304.12 147.034 187.534 1101.40391 105.3632 7.02

75%
Silica 97.88 104.7636 234.42 12.522 190.79 9639.3134 98.18 7.03
50%
Glass powder
119.93 128.353 167.59 113.07 109.046 1179.92 34.35 7.02

Table 1: Distribution properties of all Samples

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 Fig 7: Particle Size Distribution of all Samples

Fig 8: Cumulative Particle Size Distribution of all Samples

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DISCUSSIONS

 From Fig 6 , we can see that Silica has got the maximum size range among all the
samples with an average of 250 µm, with a considerable amount of around 17% of particles
showing the maximum diameter, means that much fraction deviating at smaller angles to laser
beam.
 While we can see CaCO3 particles shows the minimum diameter range of around 8 µm, with a
fraction of 12.5% showing the same. Even though around 8 % fraction of Silica50% mixture
shows a diameter range of 6 µm, a quite higher fraction of 13% shows its diameter range
around 190 µm, thereby giving an average around 98 µm.
 Among all these samples , glass particles has got more uniform composition as a higher fraction
of around 25% showed the same size distribution of 100-110 µm . Also Silica75% has got the
most non-uniform composition as a very lesser fraction of 3% and 9% particles showed the size
ranges as given in the figure.

PRECAUTIONS

• Diameter larger than 1500 micro-meter can block the pathway. So use smaller size particle.
• Heat the wheat flour before size measurement to vaporize the moisture and avoiding lumping.
• Feeder rate should not be very high otherwise lumped particle will not segregate and also can
block the pathway.
• Do not operate this unit in areas receiving direct sunlight, direct air conditioning or where large
temperature changes can occur.
• Operate the unit where dust levels are low, and no corrosive gases are present.
• Unit should be horizontal, and there should be no vibration.
• Unit should be placed on stable support or table.
• Do not operate this unit near strong magnetic or electric fields, or high- frequency devices.

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