Sub-Sieve Techniques Introduction and Stokes’ Law

Russel M. Culibar
METE 125 – MINERAL PROCESSING I
Sub-Sieve Techniques
• Sieving is rarely carried out on a routine basis below 38 µm; below this size the
operation is referred to as sub-sieving.
• The most widely used methods are sedimentation, elutriation, microscopy, and laser
diffraction, although many other techniques are available.
• Many concepts in use for designating particle size within the sub-sieve range, and is
important to be aware particularly when combining size distributions determined by
different methods.
• For irregularly shaped particles, use combining factor when combining size distributions:
Conversion Multiplying Factor
Sieve size to stokes’ diameter (sedimentation, 0.94
elutriation)
Sieve size to projected area diameter 1.4
(microscopy)
Sieve size to laser diffraction 1.5

Square mesh sieves to roundhole sieves 1.2

Stokes’ Equivalent Diameter

• Based on stokes’ law:
a perfect sphere traveling through a viscous liquid feels a drag force proportional to the
frictional coefficient.
• Assumptions for stokes law:
• Laminar Flow
• Spherical particles
• Homogeneous (uniform in composition) material
• Smooth surfaces
• Particles do not interfere with each other.
• Separation of particles based on the resistance of the particle to motion in a fluid.
• The resistance to motion determines the terminal velocity which the particle attains as
it is allowed to fall in a fluid under the influence of gravity.
𝑑2g(Ds − Df)
v=
18ŋ
v=terminal velocity
d=diameter
g=gravity
Ds=particle density
Df=fluid density
ŋ=fluid viscosity (ŋ=0.001 Nsm-2 for water at 20oC)
 • Because of the assumptions of stokes law, there is an upper size limit determined by the
particles Reynolds number, a dimensionless quantity defined by:
vdDf
R= ŋ
v=terminal velocity
d=diameter
g=gravity
Df=fluid density
ŋ=fluid viscosity (ŋ=0.001 Nsm-2 for water at 20oC)
R=Reynolds number
• Reynolds number should not exceed 0.2 if the error in using stokes’ law is not to exceed
5%.
• In general, Stokes law will hold for all particles below 40 µm dispersed in water; particles
above this size should be removed by sieving beforehand.
• The lower limit being 1 µm below which the settling times are too long, and also the
effects on unintentional disturbances, are far more likely to produce serious errors.

PREPARED BY: Dayle Tranz R. Daño

COURSE: METE 125
PROFESSOR: Dr. Vannie Joy Resabal
TOPIC: Sedimentation Method
GROUP NUMBER: 1

INTRODUCTION
Sub-sieving techniques are used to determine the particle size of materials ranging
below 38μm. The most widely used methods are sedimentation, elutriation, microscopy, and
laser diffraction.

DEFINITION AND PROCESS

Sedimentation Methods are
based on the measurement of the rate
of settling of the particles uniformly
dispersed in a fluid. This is well
illustrated in the common laboratory
experiment “beaker decantation”. The
material being tested is uniformly
distributed in low concentration in
waiter, contained in a beaker or any
similar container. The material
concentration must be low to ensure
that no interaction between materials
will happen upon settling. A wetting
agent may be added to ensure complete

Figure 1. Beaker Decantation

dispersion of the particles. A syphon tube is immersed into the water to a depth of h
below the water level, corresponding to about 90% of the liquid depth L.
The terminal velocity v is calculated from Stokes' law for the various sizes of particle
in the material, say 35, 25, 15, and 10 µ,m. For an ore, it is usual to fix D, for particles
which are most abundant in the sample.

The time required for a 10 urn particle to settle from the water level to the bottom of
the syphon tube, distance h, is calculated as

t = h/v where t = time to settle

h= immersion depth of siphon
v= velocity calculated from Stokes’
law --------- -----stoke
The pulp is gently stirred to disperse the particles through the whole volume of water
and then it is allowed to stand for the calculated time from the equation above. The water
above the end of the tube is syphoned off and all particles in this water are assumed to be
smaller than 10 urn diameter However, a fraction of the -10 urn material, which started
settling from various levels below the water level, will also be present in the material below the
syphon level.
In order to recover these particles, the pulp remaining must be diluted with water to
the original level, and the procedure repeated until the decant liquor is essentially clear. In
theory, this requires an infinite number of decantation, but in practice at least five treatments
are needed, depending on the accuracy required. The settled material can be treated in a
similar manner at larger separating sizes, i.e. at shorter decanting times, until a sufficient
number of fractions is obtained.

ADVANTAGES AND DISADVANTAGES

Sedimentation method has several advantages. Firstly, it is simple and cheap.
Sedimentation method does not require equipment that are hard to look for and does not
require an expert to perform. It also has the advantage over many other sub-sieve techniques
in that it produces a true fractional size analysis, i.e. reasonable quantities of material in
specific size ranges are collected, which can be analyzed chemically and mineralogically.
This method is, however, extremely tedious, as long settling times are required for very
fine parti•cles, and separate tests must be performed for each particle size. For instance,
a 25 um particle of quartz has a settling velocity of 0.056cm per s ,and therefore takes about
3.5 min to settle at 12 cm h, a typical immersion depth for the syphon tube. Five separate tests
to ensure a reasonably clear decant therefore require a total settling time of about
 18 min. A 5 μm particle, however, has a settling velocity of 0.0022cm per s, and therefore
takes about 1.5 hours to settle 12 cm. The total time for evaluation of such material is thus
about 8 h. A complete analysis may therefore take an operator several days.
Another problem is the large quantity of water which dilutes the undersize material,
due to repeated decantation. Theoretically an infinite number of decantations are required
to produce a 100% efficient separation into oversize and undersize fractions, and the number
of practical decantations must be chosen according to the accuracy required and the width of
the size range required in each of the fractions .

EFFICIENCY
In the system, after time t, all particles larger than size d have fallen to a depth below
the level h. All particles of a size d1 , where d1 < d, will have fallen below a level h1 below
the water level, where h1 « h.
The efficiency of removal of particles of size d1 into the decant is thus:

since at time t = 0 the particles were uniformly distributed over the whole volume of liquid,
corresponding to depth L, and the fraction removed into the decant is the volume above the
syphon level, h-h1.
Now, since t= h/v, and v is proportional to d2,

Therefore, by further derivation,

Where a = h/L

If a second decantation step is performed, the amount of -di material in the

dispersed suspension is 1 - E, and the efficiency of removal of -d1 particles after two
decantations is thus
In general, for n decantation steps, the efficiency of removal of particles of size d1 at a
separation size of d, is
The following table shows the number of decantation steps required for different efficiencies
of removal of various sizes of particle expressed relative to d, the separating size, where
the value of a= 0.9.

Table 1. Number of decantations required for required

efficiency of removal of fine particles

It can be shown that the value of a has relatively little effect; therefore there is nothing to
be gained by attempting to remove the suspension adjacent to the settled particles, thus
risking disturbance and re-entrainment.
Table 1 shows that a large number of decantations are necessary for effective removal of
particles close to the separation size, but that relatively small particles are quickly eliminated.
For most purposes, unless very narrow size ranges are required, no more than about twelve
decantations are necessary for the test.

ANDREASEN PIPETTE TECHNIQUE

A much quicker and less-tedious method of sedimentation analysis is the Andreasen
pipette technique The apparatus (Figure 2) consists of a half-litre graduated cylindrical flask
and a pipette connected to a 10 ml reservoir by means of a two-way stop cock. The tip of the
pipette is in the plane of the zero mark when the ground glass stopper is properly seated.
A 3-5% suspension of the sample, dispersed in the sedimentation fluid, usually water, is
added to the flask. The pipette is introduced and the suspension agitated by inversion. The
suspension is then allowed to settle, and at given intervals of time, samples are withdrawn
by applying suction to the top of the reservoir, manipulating the two-way cock so that the
sample is drawn up as far as the calibration mark on the tube above the 10 ml reservoir. The
cock is then reversed, allowing the sample to drain into the collecting dish. After each sample is
taken, the new liquid level is noted.
 The samples are then dried and weighed, and the weights compared with the weight of
material in the same volume of the original suspension. There is a definite particle size, D,
corresponding to each settling distance h and time t, and this represents the size of the
largest particle that can still be present in the sample.
These particle sizes are calculated from Stokes' law for
the various sampling times. The weight of solids
collected, g, compared with the corresponding
original weight, i.e. g/g0 then represents the fraction
of the original material having a particle size smaller
than D, which can be plotted on the size-analysis
graph.
The method is much quicker than beaker
decantation, as samples are taken off successively
throughout the test for increasingly finer particle
sizes. For example, although 5 urn particles of
quartz will take about 2.5 h to settle 20 cm, once
this sample is collected, all the coarser particle-size
samples will have been taken, and so the complete
analysis, in terms of settling times, is only as long as
the settling time for the finest particles.
The disadvantage of the method is that
the samples taken are each representative of the
particles smaller than a particular size, which is not as
valuable, for mineralogical and chemical analysis, as
samples of various size ranges, as are produced by
beaker decantation.
Figure 2. Andreasen
Pipette
Sedimentation techniques tend to be very tedious, due to the long settling times
required for fine particles ( up to 5 h for 3 urn particles) and the time required to dry and
weigh the samples. The main difficulty, however, lies in completely dispersing the material
within the suspending liquid, such that no agglomeration of particles occurs.
Combinations of suitable suspending liquids and dispersing agents for various metals are given
in BS ISO 13317-1.
Although the Andreasen pipette is perhaps the most widely used method of sizing by
sedimentation, various other techniques have been developed, which attempt to speed up
testing. Examples of these methods, which are comprehensively reviewed by Allen ( 1997),
are the photo-sedimentometer, which combines gravitational settling with photo-electric
measurement, and the sedimentation balance, in which the weight of material settling out onto
a balance pan is recorded against time, to produce a cumulative sedimentation size analysis.

REFERENCES
Wills B.A, Napier-Munn T.J (2006). Will’s Mineral Processing Technology. Elsevier Science &
Technology Books
Isabela Psalm C. Torcende (Group 1) MetE 125- Mineral Processing I
2013-0330 Dr. Vannie Joy Resabal

WRITTEN REPORT: ELUTRIATION TECHNIQUES

Elutriation is a process of sizing particles by means of an upward current of fluid, usually

water or air. The process is the reverse of gravity sedimentation and the Stoke’s law applies. In
sedimentation, the material to be sized is dispersed in a fluid and allowed to settle under
carefully controlled conditions. Meanwhile, in elutriation, samples are sized by allowing the
dispersed material to settle against a rising velocity. Both techniques separate the particles on
the basis of resistance to motion in a fluid. Resistance to motion determines the terminal
velocity which the particle attains as it is allowed to fall in a fluid under the influence of gravity.
Classification is a method of separating mixtures of minerals into two or more products on the
basis of the velocity with which the grains fall through a fluid medium. The fluid being either air
or water, usually water in mineral processing. Wet classification is applied to minerals that are
too fine to be sorted efficiently by screening. The velocity of the particles in the fluid medium is
dependent of the size, shape, and specific gravity of the particles.
Principles of classification are important in mineral separation utilizing gravity
concentrators.
When a solid particle falls freely in a vacuum, it is subject to constant acceleration and
its velocity increases indefinitely, being independent of size and density. Hence a lump of lead
and a feather fall together at exactly the same rate.
In a viscous medium, there is resistance to this movement and the value increases with
velocity. When equilibrium is attained between the gravitational and fluid resistance forces, the
body reaches its terminal velocity and thereafter falls at a uniform rate. The nature of
resistance depends on the velocity of the descent. At low velocities motion is smooth because
the layer of fluid in contact with the body moves with it, while the fluid a short distance away is
motionless. Between these two positions is a zone of intense shear in the fluid all around the
descending particle. Effectively all resistance to motions is due to the shear forces or viscosity
of the fluid and is hence called viscous resistance. At high velocities the main resistance is due
to the displacement of fluid by the body, and viscous resistance is relatively small; this is known
as turbulent resistance. Whether viscous or turbulent resistance predominates, the acceleration
of particles in a fluid rapidly decreases and the
terminal velocity is quickly reached.

All elutriators consist of one or more “sorting

columns” (Figure 4.10) in which the fluid is rising at
constant velocity. Feed particles introduced to the
sorting column will be separated into two fractions,
according to their terminal velocities, calculated
from Stoke’s law.
𝑑2 𝑔 (𝐷𝑠 − 𝐷𝑓 )
𝑣=
18ƞ
 Those particles having terminal velocities less than that of the velocity of the fluid will
report to the overflow, while those particles having a greater terminal velocity than the fluid
velocity will sink to the underflow.

Elutriation is carried out until there are no

visible signs of further classification taking place or
the rate of change in the weights of the product
are negligible. This involves the use of much water,
involving dilution of the undersize fraction, but it
can be shown that this is not as serious as in
beaker decantation. Consider a sorting column of
depth h, sorting material at a separating size of d.
If the upward velocity of water flow is v, then by
Stoke’s law, 𝑣 ∝ 𝑑 2 .
Particles smaller than the separating size d
will move upwards in the water flow at a velocity
dependent on their size. Thus, particles of size 𝑑1 ,
where 𝑑1 < 𝑑, will move upwards in the sorting
column at a velocity 𝑣1 , where 𝑣1 ∝ (𝑑 2 − 𝑑12 ).
The time required for a complete volume
ℎ
change in sorting column is 𝑣 , and the time required for particles of size 𝑑1 to move from the
ℎ
bottom to the top of the sorting column is . Therefore the number of volume changes
𝑣1
required to remove all particles of size 𝑑1 from the sorting column
ℎ/𝑣1 𝑑2 1
= = 2 2 =
ℎ/𝑣 𝑑 − 𝑑1 1 − (𝑑1 )2
𝑑

Comparing these figures with those in Table 4.5, it can be seen that the number of
volume changes required is far less with elutriation than it is with decantation. It is also possible
to achieve complete separation by elutriation, whereas this can only be achieved in beaker
decantation by an infinite number of volume changes.
 Elutriation thus appears more attractive than decantation, and has certain practical
advantages in that the volume changes need no operator attention. It suffers from the
disadvantage, however, that the fluid velocity is not constant across the sorting column, being a
minimum at the walls of the column, and a maximum at the centre. The separation size is
calculated from the mean volume flow, so that some coarse particles are misplaced in the
overflow, and some fines are misplaced into the coarse underflow. The fractions thus have
considerable overlap in particle size and are not sharply separated. Although decantation
method never attains 100% efficiency of separation, the lack of sharpness of the division into
fractions is much less than that due to velocity variation in elutritation (Heywood,1953).
Elutriation is limited at the coarsest end by the validity of Stoke’s law, but most
materials in the sub-sieve range exhibit laminar flow.
At the fine end of the scale, separations become impractical below 10µm, as the
material tends to agglomerate, or extremely long separation times are required.
Separating times can be considerably decreased by utilization of centrifugal forces, and one of
the most widely used methods of sub-sieve sizing in modern mineral processing laboratories is
the Warman cyclosizer (Finch and Leroux, 1982), which is extensively used for routine testing
and plant control in the size range 8-50µm for materials of specific gravity similar to quartz
(sp.gr. 2.7), and down to 4µm from particles of high specific gravity, such as galena (sp.gr. 7.5).

Figure 4.1 Warman cyclosizer

The cyclosizer consists of five cyclones, arranged in series such that the overflow of one
unit is fed to the next unit. The individual units are inverted in relation to conventional cyclone
arrangements, and at the apex of each, a chamber of is situated so that the discharge is
effectively closed.
Water is pumped through the units at a controlled rate, and a weighed sample of solids
is introduced ahead of the cyclones. The tangential entry into the cyclones induces the liquid to
spin, resulting in a portion of the liquid, together with the faster-settling particles, reporting to
the apex opening, while the remainder of liquid, together with the slower settling particles, is
discharged through the vortex outlet and into the next cyclone in the series. There is a
successive decrease in the inlet are and vortex outlet diameter of each cyclone in the direction
 of the flow, resulting in a corresponding increase in
inlet velocity and an increase in the centrifugal forces
within the cyclone, resulting in a successive decrease in
the limiting particle-separation size of the cyclones.
The cyclosizer is manufactured to have definite
limiting separation sizes at standard values of the
operating variables, viz. water flow rate, water
temperature, particle density, and elutriation time. To
correct for practical operation at other levels of these
variables, a set of correction graphs is provided.
Complete elutriation normally takes place after
about 20min, after which the sized fractions are
collected by discharging the contents of each apex
chamber into separate beakers.
Reference:
Wills, B.A. & Napier-Munn, T. (2005). Mineral
Processing Technology. Publisher:
Elsevier Science & Technology Books.

Prepared by : Jonel A. Quitiquit

Subject : MET E 125
Professor : Engr. Vannie Joy T. Resabal
Group # :1

Objectives:
- To know what is Micropic Sizing and Image Analysis.
- To know the function and uses in the industry.

I. Introduction

A microscope examination should always be carried out whenever a sample is

prepared for particle size analysis. Such an examination allows an estimate of the
particle size range of the powder under test and its degree of dispersion. If the
dispersion is incomplete it can be determined whether this is due to the presence of
agglomerates or aggregates and, if agglomeration is present, may indicate the need
for an alternative dispersing procedure

Microscopy is often used as an absolute method of particle size analysis since it

is the only method in which the individual particles are observed and measured.
 It is useful not only for particle size measurement but also for particle shape and
texture evaluation, collectively called morphology, with sensitivity far greater than
other techniques.

The images may be viewed directly or by projection. Binocular eyepieces are

preferred for particle examination but monoculars for carrying out a particle size
analysis since, by using a single eyepiece, the tube length can be varied to give
stepwise magnification.

II. Microscopic Sizing

The image of a particle seen in a microscope is two dimensional and from this
image an estimate of particle size must be made. Microscopic sizing involves
comparing the projected area of a particle with the areas of reference circles, or
graticules, of known sizes, and it is essential for meaningful results that the mean
projected areas of the particles are representative of the particle size. This requires a
random orientation in three dimensions of the particle on the microscope slide,
which is unlikely in most cases.

III. Analysis Method

Manual methods of obtaining data from images are slow and tedious and this
can give rise to considerable error. The introduction of fully automated image
analysis systems has virtually eliminated manual methods and also supplanted semi-
automatic systems. All image analysis systems use scanning techniques for
converting images into electrical signals that are processed to yield data on the
images.
IV. How Does it Work?

Image analysers accept samples in a variety of forms - photographs, electron

micrographs, and direct viewing- and are often integrated in system software. Figure
shows the grayscale electron backscatter image of a group of mineral particles
obtained with a scanning electron microscope; grains of chalcopyrite (Ch), quartz
(Qtz), and epidote (Epd) are identified in the image. On the right are plotted the size
distributions of the "grains" of the mineral chalcopyrite (i.e, the pieces of
chalcopyrite identified by the instrument, whether liberated or not) and the
"particles" in which the chalcopyrite is present. The plots are based on the analysis
of several hundred thousand particles in the original sample, and are delivered
automatically by the system software. Image analysis of this kind is available in many
forms for the calculation of many quantities (such as size, surface area, boundary
lengths) for most imaging methods, e.g. optical, electron.

V. Uses in the industries

- Determination of particle size distribution

- Particle shape e.g. aspect ratio (ratio between breadth and length) which gives
valuable extra information -complementary to laser diffraction – about particle
characteristics.
- Overview of particles dispersed in liquid or air.
- Measurement of object sizes e.g. mesh size of sieves.

VI. Advantages and Disadvantages of Microscopic Sizing and Image Analysis

 The advantages of using semi or fully automated methods are the accuracy of the
examined particle. It is also available in many forms for the calculation of many
quantities such as size, surface area, boundary lengths for most imaging methods.

The disadvantages of manual method are that the operator were over
estimating/under estimating and badly biased on the sample. In the semi/fully-
automated machine depends on the input setup by the operator. Errors may be
directly made by erroneous inputs of operator.

VII. References:

Wills, B.A. & Napier-Munn, T. (2005). Mineral Processing Technology. Publisher:

Elsevier Science & Technology Books.

Written Report
Electrical Impedance Method (Coulter)
2014 – 0145
Kristelle Mae P. Sanoy

The Coulter method of sizing and counting particles is based on measurable changes in
electrical impedance produced by nonconductive particles suspended in an electrolyte.
A Coulter counter is a machine used for counting and sizing particles suspended in
electrolytes. A typical Coulter counter has one or more microchannels that separate two
chambers containing electrolyte solutions. As fluid containing particles or cells is passes through
each microchannel, each particle causes a change to the electrical resistance of the liquid. This
machine detects these changes in resistance.
The Coulter principle states that particles pulled through an orifice, simultaneous with
an electric current, produce a change in impedance that is proportional to the volume of the
particle passing through the orifice.
This change in impedance or pulse is caused by the displacement of the electrolyte due
to the particle. The pulses are electronically amplified, scaled and counted. The volume may be
represented as the equivalent spherical diameter. The measured particle sizes can be
channelized using a height analyzer circuit and a particle size distribution is obtained. The
instrument measures particle volume, the equivalent diameter is calculated from that of a
sphere of the same volume.
The instrument is applicable in the range of 0.4 – 1200 µm.
The electrical response of the instrument is essentially independent of the shape of
particles with the same volume, an exception to this may occur with some extreme shapes.
Color or refractive index of the particles does not affect the results.
 Report
On
Laser Diffraction Instruments
By: Advent Fel R. Bañez
Laser Scattering Technology
Low angle light scattering or Laser Diffraction has been known as a laboratory technique
since 1960 specially when wide range of distribution need to be analyzed. With a dynamic
range of 0.1-3000 microns. The Size Analysis is based on the theory of intensity distribution
measurement of coherent laser light scattered by the particles describe by Mie theory. And the
width of the pattern is dependent on size. The process can be described as the laser light meets
a population of particles, volumetric size distribution can be determined from the scattered
light distribution. Based on this observation that large particles scatters light at low angle and
intensity of light scattered is high and small particles scatters light at high angle and the
intensity of light scattered is low. Two important Theory governs the function of laser light
diffraction the Mie Theory and the Franhaufer theory. The Mie theory assumes the particles are
spherical in nature. And Franhaufer theory states that the intensity of light scattered is
proportion to the particle size. Repeatability and precision are the most important feature of
light scattering technology over a wide particle size range. Also the speed, non-contact nature
and robustness of the method to ambient condition make laser diffraction suitable for on line
particle size analysis applications. Which also does not require external calibration.

Instruments
1. Malvern
Specifications:
Particle size range = 0.01 – 3500 microns
Accuracy = Better than 0.6%
Precision = Better than 0.5% variation

2. CILAS 1090
Specifications:
Particle Size range: 0.04 – 500 microns
Multi Laser Design
 2. Microtac S3500
Specifications:
Particle size range = 0.02 – 2800 microns
Precision = 0.6% variation

Loopholes

Although Laser Diffractometry is the most popular particle size analysis used today with
its ease and proven precision. It has also some drawbacks that needs to be address such as
False Assumptions of random particle orientation. And the Distortion measurement in which a
ghost particle caused by sharp edge can be interpreted by the laser diffraction instruments to
be small particles.
Conclusion:
Laser Diffraction Instruments selection based on the above specifications depend on what
size the particle are to be analyzed. and based on the address loopholes the use laser
diffraction instruments is reliable due to its precision and speed.