Experiment 2

Solid-Liquid Separation: Batch Sedimentation

I. Introduction

Solid-liquid separation involves the separation of two phases namely, solid and liquid, from
a suspension. An example of solid-liquid separation process is sedimentation. The process of
sedimentation involves the separation of a dilute slurry or a suspension by gravity settling into a
clear fluid and a slurry of higher solids concentration. The materials to be settled are usually solid
particles such as silts or clay present in water systems (Geankoplis, 2003).

Sedimentation can be accomplished by decreasing the medium fluid velocity to almost zero
so the particles would no longer remain in suspension due to fluid dynamics, thereby promoting
settling (Soediono, 1989). During batch sedimentation, suspension of particles are allowed to stand
in a settling tank or column (Latsa et al., 2005). Figure 1 below illustrates the basic stages in the
sedimentation process.

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Figure 1. Progress in Batch Sedimentation (left) and settling zones(right) (McCabe et al., 1993)

At time equal to zero, the total height of the suspension is labeled ZO where the
concentration of the suspended particles are the same at any point. As time progresses, there is a
formation of zones. Zone A is called the clear layer where particle concentration is almost zero,
Zone B is called the sedimentation zone and the concentration is uniform and equal to the original
suspension, the interface at which zone A and B coincides is called the sedimentation interface.
The interface height is the measurement from the bottom of the settling chamber to the
sedimentation interface. The settled solids are located in Zone D (sediment layer) and above Zone
D is called the transition layer or a densely-packed Zone C (McCabe et al., 1993).

As the sedimentation process continues, the depths of zones A and D increase (Figures 1b
to e) while the depth of zone B decreases. The depth of zone C almost remains constant (Figures
1b to c). Eventually, zone B disappears and the solids are deposited at zone D and C (Figures 1d
to e) (McCabe et al., 1993). The settling of particles is generally affected by the container size and
its interaction with other particles. If its distance from the wall is sufficient enough or if the ratio
of the particle diameter to the diameter of the container is less than 1:200 or if the particle
concentration is less than 0.2 volume percent, the interference will be less than 1%. In this case
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the particle is said to be free settling, otherwise the term hindered settling is applied since the
particles become too crowded and settling rate proceeds at a lower rate (Geankoplis, 2003).

The reasons for modification of the settling rate of particles in a concentrated suspension
include: (a) when a wide range of particle sizes are present in the feed, differential settling rates
between large and small particles lead to modification of the effective density of the suspension,
(b) the upward velocity of the fluid is greater at higher concentrations, (c) the velocity gradients in
the fluid surrounding the particles are greater due to the closer proximity of the particles and (d)
the ability of particles to aggregate is enhanced at higher concentrations (Latsa et al., 2005). Other
less apparent factors affect the sedimentation rate aside from the particle size, density and
concentration, and fluid viscosity. These include particle shape and orientation, convection
currents in the surrounding fluid, and chemical pretreatment of the feed suspension (Foust et al.,
2008).

Sedimentation of a suspension is generally assessed by a jar test, usually using a graduated

cylinder, during which a suspension is allowed to settle and the height of the clear liquid -
suspension interface is measured as a function of the settling time. The expected raw data to be
gathered are height of interface zones in terms of volume markings and the corresponding time.
The cross-sectional area of the graduated cylinder will be determined by measuring its inside
diameter. To obtain the actual interface height, the recorded volumes are divided by the cross-
sectional area of the cylinder. Figure 2 below shows how the interface height can be determined
in a jar or cylinder test.

Figure 2. Zones of settling after a given time and determination of the interface height (Tarleton
& Wakeman, 2007)

The recorded volume markings are divided by the cross-sectional area of the cylinder to obtain the
actual interface height (z) (Tarleton & Wakeman, 2007):

𝑣𝑜𝑣𝑙𝑢𝑚𝑒𝑙𝑒𝑣𝑒𝑙
z = 𝑐𝑦𝑙𝑖𝑛𝑑𝑒𝑟𝑎𝑟𝑒𝑎(1)

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 The interface height (z) is plotted against time in Figure 2. It can be observed that the slope
of the plot, which is the velocity of settling, is constant before reaching the critical point C. With
the limitations to the number of data which can be gathered, the velocity can be estimated by
finding the slopes between adjacent points using equation 1 (Geankoplis, 2003).

Figure 3. Height of Interface vs Time curve (Foust, 1980)

The settling rate or settling velocity can be obtained from the plot shown above. The
instantaneous settling velocity is the slope of the line tangent to the curve -dz/dt = v or given by
the equation:

(2)
where v is the settling rate and z is the interface heights with respect to time interval t.

One of the simplest methods to determine the critical point of a settling curve is to draw
two tangent lines, one in the free settling portion, the other at the final compression at the near end
of settling in which interface height becomes almost constant as seen in Figure 2. In the same
figure, an angle bisector of the two tangent lines, which vertex is the intersection point, is drawn.
The intersection of the angle bisector and the settling curve is an estimate of the critical point
(Foust et al., 1980).
Solid-liquid separation is applied in industrial processes which include recovery and
processing of solids or purification of liquids (Svarovsky, 2000). Sedimentation is often utilized
in the food industry such as “separating dirt and debris from the raw material, crystals from their
mother liquor and dust or product particles from air streams” (Earle, 2004). It is also one of the
most widely used unit operations in wastewater treatment systems in removing grit and particulate
matter, sludge from the bioreactor, chemical flocs in a chemical process (Carlsson, 1998).
This experiment highlighted the effects of varying slurry concentration to the
sedimentation characteristics of flour and the construction of the settling curve of the flour slurry.

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II. Objectives

This experiment aimed to determine the effect of varying slurry concentration to the
sedimentation process. Specifically, it aimed to:

a. Determine the relationship between time and interface height at different slurry
concentrations; and
b. Determine the relationship between time and settling rate at different the slurry
concentrations.

III. Scope and Limitations

The experiment was focused on determining the effect of varying solids concentration to
the settling rate of the flour particles. Four varying flour concentrations namely 20 g/L, 40 g/L and
60 g/L were used. The effect of varying fluid height, temperature, and varying particle sizes were
beyond the scope of the experiment and were assumed constant all throughout. The experiment
was only applicable to batch still fluid processes and the effects of fluid dynamics on the settling
of the particle was not considered. Gravity was the sole force acting on the particles. These
limitations implied that any irrelevant results to the experiment were accounted to those factors
that weren't considered. Moreover, the investigation of the effect of different flour concentrations
implied that only the rate at which the solids settled were expected in the results.

The experiment was conducted at the School of Technology’s Unit Operations Laboratory
at standard temperature and pressure. The experiment approximately lasted for 16 hours until all
the solids have completely settled. Necessary data were gathered after the experiment which were
used to plot the relationship between time and settling rate at varying slurry concentrations as well
as between time and interface height at varying slurry concentrations

IV. Methodology

A. Materials
 Vernier caliper  Ruler
 1000-mL graduated cylinder  Stopwatch
 Stirring rod  500 ml Beaker
 Baking soda sample  Analytical balance
 Distilled water  PPE (e.g. mask, gloves)
 Aluminum foil

A. Methods
The Material Safety Data Sheet of flour was reviewed prior to the experiment
proper and proper personal protective equipment attire was observed. Furthermore,

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laboratory materials such as 1000-mL graduated cylinders and 500-mL beakers were
borrowed from the lab technician. The apparatuses were further clean and freed from
contaminants.
The inner diameter of the 1000-mL graduated cylinder was measured using the
Vernier caliper. Simultaneously, 20 g, 40 g, and 60 g of flour were weighed on a 500-mL
beaker. A significant amount of distilled water was poured into the 500-mL beaker and was
slowly mixed with the previously weighed 20 g of flour using stirring rod. Subsequently,
the mixed solution was poured into the 1-L graduated cylinder and was diluted into the
1000 mL mark. The contents were then stirred again using stirring rod for 30 seconds to
ensure uniform particle concentration distribution.
After stirring, the height of the mixture was recorded. The mixture was allowed to
settle and the volume reading of the interface height was then noted for every 2 minutes
interval. The particles were found to fully settled the next day of the experiment. The same
steps were repeated for the two other concentrations namely 40 g/L and 60 g/L.
After the experiment, the workplace was clean as well as the laboratory apparatus
and were returned to the lab technician. The gathered data were then subjected for further
analysis.

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V. Results and Discussion

Table 1. Calculated Height of Interface and Settling Rate

Time Interval Height of Interface (cm) Settling rate (cm/min)
(mins) 20 g/L 40 g/L 60 g/L 20 g/L 40 g/L 60 g/L
0 36.45 35.90 36.45 0.0000 0.0000 0.0000
2 36.38 35.55 36.27 0.03645 0.00036 0.00018
4 36.31 35.19 36.27 0.01823 0.00036 0.00000
6 35.72 35.01 36.09 0.09721 0.00018 0.00019
8 35.72 35.01 36.09 0.00000 0.00000 0.00000
10 35.54 34.83 36.09 0.01823 0.00018 0.00000
12 35.36 34.65 36.09 0.01519 0.00019 0.00000
14 35.36 34.65 36.09 0.00000 0.00000 0.00000
16 35.36 34.65 36.09 0.00000 0.00000 0.00000
18 35.18 34.65 36.09 0.01013 0.00000 0.00000
20 34.99 34.65 36.09 0.00911 0.00000 0.00000
22 34.63 34.65 36.09 0.01657 0.00000 0.00000
24 34.27 34.65 36.09 0.01519 0.00000 0.00000
26 34.27 34.65 36.09 0.00000 0.00000 0.00000
28 34.27 34.47 36.09 0.00000 0.00019 0.00000
30 34.27 34.47 36.09 0.00000 0.00000 0.00000
40 34.27 34.47 35.91 0.00000 0.00000 0.00019
50 34.27 34.29 35.72 0.00000 0.00019 0.00019
60 34.08 34.11 35.72 0.00304 0.00019 0.00000
70 34.08 33.93 35.54 0.00000 0.00019 0.00019
80 34.08 33.93 35.54 0.00000 0.00000 0.00000
90 33.90 33.93 35.36 0.00203 0.00000 0.00019
100 33.90 33.75 35.36 0.00000 0.00019 0.00000
110 33.90 33.75 35.18 0.00000 0.00000 0.00019
120 33.35 33.75 35.18 0.00456 0.00000 0.00000
1170 2.19 3.41 4.92 0.02664 0.50565 0.31849

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 37

36.5

36
interface heihgt (cm)

35.5
20g/ml
y = -0.0095x + 36.272
35 R² = 0.959 40g/ml

34.5 y = -0.0133x + 35.051 60g/ml

R² = 0.7862 Linear (20g/ml)
34
Linear (40g/ml)
33.5
y = -0.0201x + 35.567 Linear (60g/ml)
33 R² = 0.6836

32.5
0 20 40 60 80 100 120 140
time (min)

Figure 2. Plot of Interface Height vs. time for the three flour concentrations

The interface height was determined by dividing the measured volume from the graduated
cylinder by the area of the cylinder. Figure 1 shows the relative slopes of the three concentrations
and it can be noted that the 20g/ml flour concentration has the largest slope (-0.0201) for the
observation time of 120 minutes. This observation is supported by the fact that lower
concentrations of suspended solid, the farther it is from hindered settling. As time progressed, the
difference in interface height readings between successive time intervals slowly decreased due to
the resistance caused by other solid particles coming in contact with the settling particle.
The plot shown in Figure 1 did not account for the total time it took for the solids to fully
settle. Figure 2 includes this data. It is noted that no data were obtained from 120 minutes to the
time it took to fully settle, therefore, no inference regarding the critical point of the settling point
can be acknowledged. The critical point is supposedly the point in time where the settling rate
decreases appreciably. However, the relative settling rate for each concentration can be illustrated.
Shown in Figure 3, it is observed that the settling rates provided a fluctuating value. This
irregularity can be accounted by the experimental errors that occurred during measurement for the
interface line is not inherently apparent.
As time progressed, the settling rate can be observed to decrease. This phenomenon was
due to the crowding of solid particles causing resistance to their downward motion. Another
perspective can be taken that as solids accumulate in region C, it becomes more difficult for the
solids to push out the water below the interface height since the path in which water can pass
through becomes narrower.

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 40
35

interface heihgt (cm)

30
20g/ml
25
y (60 g/ml) = -0.0269x + 36.921 40g/ml
20 R² = 0.9892
y (40g/ml) = -0.0272x + 35.567 60g/ml
15
y (20 g/ml) = -0.0286x + 35.885 R² = 0.9917 Linear (20g/ml)
10 R² = 0.9921
Linear (40g/ml)
5
0 Linear (60g/ml)
0 500 1000 1500
time (min)

Figure 3. Plot of Interface Height vs. time (fully settled)

0.35

0.3
settling rate (cm/min)

0.25

0.2 20g/ml
40g/ml
0.15
60g/ml
0.1

0.05

0
0 20 40 60 80 100 120 140
-0.05
time (min)

Figure 4. Settling Rate vs. Time

VI. Conclusion

The concentration of the solid greatly affects the settling of solids particles in suspension
in water or any fluid. The interface height decreases slower in higher solids concentration (40 and
60 g/ml) than for the lower solids concentration (20 g/ml). The settling rate of solid particles
decreases as time progresses and as the interface height decreases due to the crowding of solid
particles, thus, causing hindered settling.

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VII. Recommendation

Better relationship between settling rate and time ca be observed if data was gathered at
constant time intervals from first settling to full settling in order to establish a reliable curve that
closely resembles that of the theoretical settling curve. Furthermore, the choice of sample should
be carefully chosen so as to establish an apparent interface height for ease of measurement reading

VIII. Appendices

A. Raw Data
Time Interval Volume Readings (mL)
(mins) 20 g/L 40 g/L 60 g/L
0 1000 1000 1000
2 998 990 995
4 996 980 995
6 980 975 990
8 980 975 990
10 975 970 990
12 970 965 990
14 970 965 990
16 970 965 990
18 965 965 990
20 960 965 990
22 950 965 990
24 940 965 990
26 940 965 990
28 940 960 990
30 940 960 990
40 940 960 985
50 940 955 980
60 935 950 980
70 935 945 975
80 935 945 975

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 90 930 945 970
100 930 940 970
110 930 940 965
120 915 940 965
1170 60 95 135

B. Sample Calculation

All data calculated are based on 20 g/L concentration

For the area,

𝜋 2
𝐴𝑟𝑒𝑎 = 𝐷 ; 𝐷 = 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟
4
𝜋
= (5.88 𝑐𝑚)2
4
𝐴𝑟𝑒𝑎 = 27.43 𝑐𝑚2
For the interface height,
𝑚𝑒𝑎𝑠𝑢𝑟𝑒𝑑 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑐𝑦𝑙𝑖𝑛𝑑𝑒𝑟
𝐼𝑛𝑡𝑒𝑟𝑓𝑎𝑐𝑒 ℎ𝑒𝑖𝑔ℎ𝑡 =
𝐴𝑟𝑒𝑎
1000 𝑐𝑚3
=
27.43𝑐𝑚2

𝐼𝑛𝑡𝑒𝑟𝑓𝑎𝑐𝑒 ℎ𝑒𝑖𝑔ℎ𝑡 = 36.45 𝑐𝑚

For the settling rate,
ℎ𝑒𝑖𝑔ℎ𝑡 1 − ℎ𝑒𝑖𝑔ℎ𝑡 2
𝑉𝑒𝑙𝑜𝑐𝑖𝑡𝑦 =
𝑡𝑖𝑚𝑒 𝑒𝑙𝑎𝑝𝑠𝑒𝑑
36.45 𝑐𝑚 − 36.38 𝑐𝑚
=
2 𝑚𝑖𝑛
= 0.03645 𝑐𝑚/𝑚𝑖𝑛

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 C. Photos

Figure 5. Measuring the inside diameter

of cylinder
Figure 6. Covering the
cylinder with aluminum

Figure 7. Taking the Figure 8. 20 g/L, 40 g/L, and 60 g/L

volume reading samples of flour

XI. References

Carlsson, B. (1998). An introduction to sedimentation theory in wastewater. Systems and

Control, 1-7. Retrieved February 11, 2017 from
http://www.it.uu.se/research/project/jass/material/sett98.pdf
Earle, R. L. (2004). Unit Operations in Food Processing. The New Zealand Institute of Food
Science & Technology (Inc.). Retrieved February 11, 2017 from
http://www.nzifst.org.nz/unitoperations/mechseparation3.htm
Foust, A. (1980). Principles of unit operations. John Wiley & Sons (Asia) Pte Ltd.
Foust, A. S., Wenzel, L. A., Clump, C. W., Maus, L., & Andersen, L. B. (2008). Principles of
Unit Operations, 2nd Edition. John Wiley & Sons, Singapore.

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Geankoplis, J. C. (2003). Transport processes and separation process principles (4th Ed). New
Jersey: Pearson Education, Inc.
Latsa, M., Assimacopoulos, D., Stamou, A., & Markatos, N. (2005). Batch Sedimentation.
Applied Mathematical Modeling. Elsevier B.V.
McCabe, Warren L., Smith, J., & Harriot, P. (1993). Unit operations of chemical engineering.
Chemical Engineering Science (5th ed., Vol. 6). New York: McGraw Hill, Inc.
http://doi.org/10.1016/0009-2509(57)85034-9
Soediono, B. (1989). Sedimentation. Journal of Chemical Information and Modeling, 53, 160.
http://doi.org/10.1017/CBO9781107415324.004
Svarovsky, L. (200). Solid-liquid Separation (4th Ed) . Butterworth-Heinemann.
http://dx.doi.org/10.1016/B978-075064568-3/50023
Tarleton, E. S. & Wakeman, R. J. (2007). “Solid/Liquid Separation: Equipment Selection and
Process Desig”. Elsevier Ltd.

Team Members:
Camarote, Bryle Kristiann C.
Romelo, Nimrod B.
Valdon, Sarah Jane I.

Date Performed:
February 13, 2017

Date Submitted:
February 27, 2017

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