Batch Sedimentation

Post-laboratory Experiment 4
Dean Joyce B. Alboroto | Ma. Kathleen Pearl F. Grande | John Salvador Y. Ricacho

I. INTRODUCTION
Mechanical-physical separation processes are processes that use mechanical-physical
forces, such as gravitational and centrifugal, actual mechanical and kinetic forces, rather than
molecular or chemical forces and diffusion (Geankoplis, 2015). These processes are done for
the removal of particles from the streams, eliminating contaminants from fluid or recovering
the particles (McCabe, Smith, & Harriot, 2005). Settling and sedimentation are common
types of mechanical-physical separation processes, in which their applications include the
removal of solids from liquid sewage waste, settling of crystals from mother liquor, and
settling of solid food particles from a liquid food (Geankoplis, 2015).

Sedimentation is the separation of dilute slurry into clear fluid and slurry with high
solid content with the use of gravity settling. Its mechanism is best described by batch settling
test in a glass cylinder, found in Figure 1. At first, the solid is uniformly distributed in the
liquid as observed in Figure 1(a). All particles begin to settle at the start of the process,
approaching the terminal velocities under hindered-settling conditions. Several zones of
concentration are established as shown in Figure 1(b). The first one is zone D, where settled
solids of heavier faster-settling particles are found at the bottom part. Zone C is the transition
zone, where solid content varies and fluid rises in this channel. It is known as the zone of
variable size distribution and non-uniform concentration. Zone B is known as the uniform-
concentration zone, where concentration is distributed uniformly. Finally, the top portion,
Zone A, is known as clear liquid. As the sedimentation continues, heights of each zone vary,
where settled materials and the clear liquid grow larger until all solids settle at the bottom,
eliminating the two zones at the middle as shown in Figure 1(c). This is referred to as the
critical settling point (Geankoplis, 2015; Foust, Wenzel, Clump, Maus, & Andersen, 1980).

Figure 1. Mechanism of Batch Sedimentation: (a) original uniform suspension, (b) zones of
settling, and (c) compression of Zone D after Zone B and C disappear (Geankoplis, 2015)

There are two settling processes depending on the interaction of the particles, the
hindered settling and free settling. Hindered settling takes place when there is high
concentration of suspensions having significant interaction between the particles, thus, there
is an increase of force exerted at a given velocity of the particles and particles settle at a
lower rate. Meanwhile, free settling, in a concentrated suspension, obtains a sedimentation
rate less than its terminal falling velocity (Richardson, Harker, & Backhurst, 2002).

In free settling, a particle has sufficient distances with other particles and the walls of
the container, thus, there is no effect on the fall of the particle. The free settling velocity for
laminar flow region (NRe<1) observes Stoke’s Law given in Equation 1 (Perry & Green,
2008).
𝑔𝐷𝑝2 (𝜌𝑝 −𝜌)
𝑣𝑡 = (Equation 1)
18𝜇

where, g is the gravitational constant, Dp is the particle diameter, 𝜌𝑝 is the particle density, 𝜌
is the fluid density, and 𝜇 is the fluid viscosity (Perry & Green, 2008).

Hindered settling flow obtains a settling velocity less than the calculated velocity
from Stoke’s Law due to a greater force in suspension from interference of particles. For
laminar flow region, the equation for settling velocity becomes (Geankoplis, 2015;
Richardson et al., 2002):
𝑔𝐷𝑝2 (𝜌𝑝 −𝜌)
𝑣𝑡 = (𝜀 2 𝜓𝑝 ) (Equation 2)
18𝜇

Where, 𝜀 is the volume fraction of the liquid and 𝜓𝑝 is an empirical correction factor
defined as (Geankoplis, 2015):
1
𝜓𝑝 = 101.82(1−𝜀) (Equation 3)

II. OBJECTIVES:
The main objective of the experiment was to perform and study the mechanism of a
batch sedimentation process. Specifically, it aimed to:

1. observe and determine the characteristics of the process;

2. determine the effect of initial concentration of the sample on the settling rate
of the slurry;
3. generate a plot of interface height vs time;
4. and determine the settling velocity of the slurry for every time interval.

III. SCOPE AND LIMITATIONS

The experiment will be conducted inside the Food Processing Lab of the School of
Technology. The experiment will investigate the theories and information of a batch
sedimentation process specifically for solid particles using chalk. Graduated cylinder will be
used in the experiment that corresponds to the traditional vertical settling tanks used in the
industry. Different concentrations of the solid particles will be varied to determine its effect
to the settling rate. Tap water from the laboratory will be used to clearly see the settling of the
sediments and it is assumed that its density is 1000kg/m3. Chalk will be bought from the
Miagao Public Market.

IV. METHODOLOGY
A. Materials and Apparatus
1. 40 Chalks
2. 3 stirring rod
3. 3 1000mL graduated cylinder
4. 3 500mL beaker
5. 3 200mL beaker
6. 250mL beaker
7. 3 Funnel
8. 3 Tape Measure
9. 3 brush
10. Mortar and pestle
11. Tap water
12. Stopwatch
13. Sieve
14. Analytical balance

B. Experimental Set-up

(a) (b) (c)

Figure 2. Experimental set-up with three different

concentrations of solid particles. (a) 10g, (b) 50g,
and 100g.
C. Procedure
1. In a clean area, prepare all materials and apparatus needed for the experiment.
2. Crush the chalks into powdered form using the mortar and pestle.
3. Sieve the powdered chalk to make finer particles and place it in a 250 mL beaker.
4. Crush again the particles left in the sieve and sieve it again.
5. Repeat the steps 2-4 until about 160 g of fine powdered chalk is obtained.
6. Measure a 10 g, 50 g, and 100 g of fine powdered chalk using the analytical balance
and place it in a 200 mL beaker separately.
7. Fill the three 1000 mL graduated cylinders with water until the 500 mL mark.
8. Transfer the three weighed fine powdered chalk at the same time to the three 1000 mL
graduated cylinders.
9. Fill the three 1000 mL graduated cylinders with water until the 1000 mL mark.
10. Stir each solution simultaneously, until its phase is uniformed.
11. Stop the stirring for the three solutions.
12. Start the stopwatch. Allow the sediments in the solution to settle.
13. Record the changes in height of different settling layers, if there are any, every minute
until all sediments settle at the bottom.
14. Repeat steps 1-13 for the second trial.

V. RESULTS AND DISCUSSION

In line with the objectives, the interface heights were recorded at different slurry
concentrations. The average values for the interface heights for three trials are shown in
Table 1. The calculated instantaneous settling velocities are also shown in the table. The raw
data for the different trials and the sample calculation for the settling velocity are shown in
the Appendices section.

Table 1. Values for interface heights and settling velocities

Time (min) Interface height (cm) Settling velocity (cm/min)

30g/L 50g/L 30 g/L 50g/L
1 14.2 16.4 0 0
2 11.5667 15.93333 2.63333 0.466666667
3 8.96667 15.33333 2.6 0.6
4 6.83333 14.53333 2.13333 0.8
5 6.36667 13.86667 0.46667 0.666666667
6 5.96667 13.16667 0.4 0.7
7 5.8 12.16667 0.16667 1
8 5.4 11.6 0.4 0.566666667
9 5.23333 11 0.16667 0.6
10 4.9 10.5 0.33333 0.5
11 4.9 10.33333 0 0.166666667
12 4.9 10.33333 0 0
 A plot for the values of interface height versus time is shown in Figure 1. As
observed, as time increases, the interface height decreases. This decrease in interface height
indicates the settling of the particles at the bottom of the graduated cylinder. The interface
heights continue to decrease until such time that a constant interface height is achieved. The
plateauing of the curves in Figure 1, which corresponds to constant interface heights,
indicates that all the solids in the slurry have fully settled. The settling time for the 30 g/L
chalk concentration is around 10 minutes, while the settling time for 50g/L is around 11
minutes. This implies that the lower the concentration of the slurry, the lower the settling
time.

Comparing the plots for 30g/L and 50g/L concentrations, the decrease in interface
height for the 30g/L is larger in magnitude compared to that of the decrease in interface
height for 50g/L. The values of the slopes for the two best-fit lines also confirm that the
smaller concentration has a steeper decrease in interface height. These results show that at
higher concentrations, the particles experience hindered settling due to significant
interactions between particles. Meanwhile, at a lower concentration, free settling is
experienced due to sufficient particle distances (Perry & Green, 2008).

18
16
14
Interface height (cm)

12
10 y = -0.6169x + 16.94
8
6
4
y = -0.7057x + 11.673
2
0
0 2 4 6 8 10 12 14
Time (min)

30g/L 50g/L Linear (30g/L) Linear (50g/L)

Figure 1. Interface height vs. time

Another plot, which shows the relationship of settling rate and time for different
slurry concentrations, is shown if Figure 2. In general, as time progresses, the settling
velocity decreases. This decrease in velocity is attributed to the crowding of the particles,
causing shorter interparticle distance and inducing hindered settling. However, there are
observed fluctuations in the settling rates at specific time intervals which may be caused by
errors during the experiment. Possible sources of error are measurement reading errors and
the decrease in slurry concentration due to some particles sticking on the stirrer after stirring.
 Comparing the two concentrations, the 30 g/L slurry initially has higher settling
velocity compared to the settling velocity of the 50 g/L slurry. However, after several
minutes, the settling velocity of the 30 g/L velocity significantly decreased and became lower
in comparison to the settling velocity of the 50 g/L slurry. This is because at the point where
there is significant decrease in settling velocity for the 30 g/L, it is already close to
completing full settling of particles. This point is called the critical point, defined as the point
where there is a significant decrease in settling velocity (Foust et al., 1980). From visual
inspection of Figure 2, the critical point for the 30 g/L slurry is subjectively at 4 minutes,
while the critical point for the 50 g/L slurry is subjectively at 10 minutes.

2.5
Settling velocity (cm/min)

1.5

0.5

0
0 2 4 6 8 10 12 14
-0.5
Time (min)

30g/L 50g/L

Figure 2. Settling velocity vs. time

VI. CONLUSION AND RECOMMENDATIONS

The experiment for batch sedimentation of chalk was successfully conducted. The
results gathered show that the time consumed for the completion of a sedimentation process
is dependent on the slurry concentration. It was found that the higher the slurry concentration,
the higher the settling time, therefore, the lower the slurry concentration, the faster the
sedimentation process. Plotting a graph of interface height vs. time confirms the direct
proportionality of increasing settling time and increasing slurry concentration, which is
caused by hindered settling at increasing concentrations. Meanwhile, the settling rates for
each time interval were observed to decrease due to decreased interparticle distance.

It is highly recommended that for future experiments, three or more concentrations of

slurry are used in order to fully confirm the validity of the relationship of the different
sedimentation parameters. Moreover, different materials in addition to chalk can be used to
compare their effects on settling parameters. Lastly, to increase the precision and accuracy of
the experiment, errors during stirring and measurement readings should be minimized.
VII. REFERENCES
Foust, A. S., Wenzel, L. A., Clump, C. W., Maus, L., & Andersen, L. B. (1980). Particulate
Solids Flow and Separation through Fluid Mechanics. In Principles Of Unit
Operations(2nd ed., pp. 629-630). Hoboken, NJ: John Wiley & Sons.
Geankoplis, C. J. (2015). Mechanical-Physical Separation Processes. In Transport Processes
and Separation Process Principles (includes Unit Operations) (3rd ed., pp. 800-820).
USA, NJ: Prentice-Hall International, Inc.
McCabe, W. L., Smith, J., & Harriott, P. (2005). Mechanical Separations. In Unit
Operations of Chemical Engineering (5th ed., pp. 1047-1053). NY: McGraw-Hill
Professional.
Perry, R., & Green, D. (2008). Fluid and Particle Dynamics. In Perry's Chemical Engineers'
Handbook, Eighth Edition (8th ed., pp. 6-52). NY: McGraw-Hill Professional Pub.
Richardson, J. F., Harker, J. H., & Backhurst, J. R. (2018). Sedimentation. In Coulson and
Richardson's Chemical Engineering: Volume 2: Particulate Systems and Particle
Technology (5th ed., pp. 237-240). Oxford, England: Butterworth-Heinemann.

VIII. APPENDICES
 A. Raw Data
Table A.1. Raw data for batch sedimentation

Time (min) Interface Height (cm)

30 g/L 50 g/L

Trial 1 Trial 2 Trial 3 Trial 1 Trial 2 Trial 3

1 14.2 13.9 14.5 1 16.5 16.2
2 12 11.5 11.2 2 16 15.8
3 9.2 8.6 9.1 3 15.7 15.3
4 7 7.5 6 4 14 14.8
5 6.8 6.8 5.5 5 14 13.8
6 6.5 6.3 5.1 6 13.5 13
7 6.3 6.1 5 7 12.5 12
8 6.3 5 4.9 8 11.8 11.5
9 5.3 5.2 5.2 9 11 11
10 5 4.8 4.9 10 10.5 10.5
11 5 4.8 4.9 11 10.5 10
12 5 4.8 4.9 12 10.5 10

B. Sample calculations
 Calculation for the instantaneous settling velocity (2 mins, 50 g/L)
∆ 𝑖𝑛𝑡𝑒𝑟𝑓𝑎𝑐𝑒 ℎ𝑒𝑖𝑔ℎ𝑡 15.9333 𝑐𝑚 − 16.4 𝑐𝑚
𝑣= = = 0.4666667 𝑐𝑚/𝑚𝑖𝑛
∆ 𝑡𝑖𝑚𝑒 2 min − 1 𝑚𝑖𝑛