Department of Chemical Engineering and Energy Sustainability

Faculty of Engineering

KNC 3221 Laboratory 4

Laboratory Report
for
Experiment 7: Sedimentation

By

Group 04

Name Matric No
Amni Syazwani Azman 58456
Muhammad Nur Adib Bin Ramli 58837
Rereina Anak Dovid@David 59140

Course Coordinator: Mohd Farid Atan

BACHELOR OF CHEMICAL ENGINEERING WITH HONOURS

ACADEMIC SESSION 2018/2019

 ABSTRACT

The environment on Earth becomes more polluted nowadays especially to one of

the most important sources, which is water source. Wastewater contains both dissolved
and suspended particles. Wastewater treatment which involves coagulation, flocculation
and sedimentation. Coagulant is added to water in order to gather any waste in the water
such as dust, earth particles, fish eggs, etc., into flocs. Wastewater treatment is also use
widely domestically and industrially. It is a common process in treating wastewater so
that the water that is treated can be used by human safely.

Keywords: Wastewater, Treatment

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 LIST OF TABLES

TABLE 4. 1: EFFECT OF DIFFERENT DOSAGE OF COAGULANT ON THE COLOR OF THE WASTEWATER

(SOLUTION) 8
TABLE 4. 2: REMOVAL PERCENTAGE OF TURBIDITY ON DIFFERENT ALUM DOSAGES 9

LIST OF FIGURES

FIGURE 4. 1: TURBIDITY OF EACH SAMPLE AT DIFFERENT DOSAGE OF ALUMINIUM SULPHATE 9

FIGURE 4. 2: REMOVAL PERCENTAGE OF TURBIDITY VERSUS DOSAGE OF ALUMINIUM SULPHATE 11
FIGURE 4. 3: PH OF WASTEWATER (ADJUSTED AND POST-TREATED) AT DIFFERENT DOSES 13

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 Table of Contents

ABSTRACT 1
LIST OF TABLES 2
LIST OF FIGURES 2
1.0 INTRODUCTION 4
1.1 AIM AND OBJECTIVES 4
1.2 PROBLEM STATEMENT 4
2.0 LITERATURE REVIEW 5
3.0 PROCEDURES 5
3.1 START-UP PROCEDURES 5
3.2 OPERATING PROCEDURES 6
3.3 SHUT-DOWN PROCEDURES 7
4.0 RESULT AND DISCUSSION 7
4.1 INFLUENCE ON DIFFERENT DOSAGE OF COAGULANT ON THE TURBIDITY OF THE
WASTEWATER 9
4.2 INFLUENCE OF DIFFERENT DOSAGE OF COAGULANT ON THE PH OF THE
WASTEWATER 11
5.0 CONCLUSION 13
6.0 REFERENCES 15

3
1.0 INTRODUCTION

Wastewater refers to all the effluents that comes from household, commercial
establishments and institutions, hospitals, industries and many more. These effluents
refer to the sewage or liquid waste that is discharged into water bodies either from direct
sources or treatment plants. Wastewater contains both dissolved and suspended particles.
To remove undesired materials in the solution, the wastewater is treated by the
wastewater treatment which involves coagulation, flocculation and sedimentation.
Coagulation destabilises particles through chemical reaction between coagulant and
colloids, and flocculation transports the destabilised particles that causes collisions with
flocs. Essentially, a coagulant is added to water in order to gather any waste in the water
such as dust, earth particles, fish eggs, etc., into flocs. As these flocs are heavier than
water they settle at the bottom of the sedimentation tank resulting in the removal of 90%
of the suspended matter (Veolia Water Technologies, 2017).

1.1 AIM AND OBJECTIVES

The aim of this experiment is to study the effect of coagulant dosage on the
sedimentation process. The objectives of this experiment are as follows:
1. To conduct the wastewater treatment process which are coagulation,
flocculation and sedimentation.
2. To compare the effect of different dosages of coagulant on the pH, colour and
turbidity of water.

1.2 PROBLEM STATEMENT

The water treatment process conducted is at the laboratory scale which

involve flocculation unit and the usage of coagulant salt that may affect the pH,
the colour and the turbidity of the wastewater solution. Since the scale is different
than the actual water treatment plant, an experiment of sedimentation unit is
conducted.

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2.0 LITERATURE REVIEW

Wastewater treatment comprises applying known innovation to improve or

upgrade the quality of wastewater. Wastewater treatment includes collecting the
wastewater in a central, isolated area and subjecting the wastewater to different
treatment forms (Zăbavă, et al., 2016).

The principal objective of wastewater treatment is mostly to permit human and

industrial effluents to be disposed of while no danger to human health or unacceptable
damage to the natural environment. With the current issues on environmental health and
pollution problems, there is an increasing awareness of the requirement to get rid of these
wastewaters safely and beneficially.

According to Ahamad et al. (2014), coagulation taken after by flocculation as an

aid to sedimentation and filtration has been practiced for centuries.
To upgrade the expulsion of solids in exceedingly concentrated common waters that
contain significant amounts of settleable solids, Coagulation–flocculation can be applied.
The prevail chemical operator for clarification of water is alum, Al2(SO4)3 which is the
best effective in removing the suspension of solid (Bourke et al., 2002).

Based on the experiment conducted by Nunez et al. (1999), the use of the
coagulation-flocculation process in the treatment of slaughterhouse wastewater using
ferric salts and alum reported a removal capacity of 75% of COD. The coagulation-
flocculation handle has been found to be cost effective, simple to function and is an energy-
saving treatment alternative (Amuda & Alade, 2006).

3.0 PROCEDURES

3.1 START-UP PROCEDURES

1. 3 L of waste water sample from UNIMAS lake are collected using 2 bottles of
1.5 L water bottle.

2. 2 L of 2 M H2SO4 solution is prepared by adding 200 mL of 18.0 M H2SO4 into

2 L of distilled water. H2SO4 is poured slowly into the water as it is a strong
acid and have the possibility to explode if the process carried out fast. The
solution is stored in glass bottle and labelled.

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3. 2 L of NaOH solution is also prepared by adding 160 g of NaOH pellet into 2 L
of distilled water. Then, the solution is stored in glass bottle and labelled.

4. Aluminium Sulphate (Alum) is obtained from lab technician.

5. The sedimentation unit equipment is checked for possible leak and

malfunction.

3.2 OPERATING PROCEDURES

1. The Instruction Manual for Standard Operational Procedure (SOP) provided

in the laboratory is read.

2. The wastewater is poured into 450 mL of beaker where the beaker will act as
sedimentation tank.

3. The initial pH and turbidity are measured using Eutech handheld meter kit
pH meter and 2020wi turbidimeter.

4. The waste water pH is adjusted to pH 7 using a few drop of m H 2SO4 solution

and 2M of NaOH solution and the beaker is placed under the stirrer.

• The solution is in neutral that is safe for any consumption.

5. The speed and timer on the control panel is set up and the initial value is 150
RPM for 3 minutes and the stirrer is started.

6. The coagulant (Alum) is added into the sedimentation tank and then stirred
for a minute.

• The solution is stirred for a minute for producing floc particle.

7. Then, the speed of stirrer is decrease to 100 RPM while the time is increase to
15 minutes.

8. The stirrer is stopped and the floc is allowed to settle for 30 minutes.

9. The pH, colour and turbidity of the solution is observed and recorded in Table
5.1, 5.2 and 5.3.

10. Step 4 to 8 is repeated by using different dosage of coagulant

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 3.3 SHUT-DOWN PROCEDURES

1. The chemical waste is disposed properly into chemical waste disposal storage tank
to prevent any contamination issue.
2. The stirrer speed is set back to 0 RPM then switched off. The impellers are also
removed from the stirrers coupling.
3. The main power switch is switched off.
4. The beakers used are removed from the Flocculation Test Unit and cleaned with
provided detergent.

4.0 RESULT AND DISCUSSION

The experiment was conducted to observe the effect of different dosages of

coagulant on the pH, colour and the turbidity of the wastewater which is taken from
UNIMAS Lake. The differences observed were discussed and displayed in Table 4.1.
Coagulant dose is a key of process-control factors because different water quality
conditions can have different effects depending on the doses (Budd et. al., 2004). According
to Benson (2006), implementing a high concentration of coagulant in water treatment
would reduce the time taken needed for the particles to destabilise as it increases the
collision-attachment efficiency.

Coagulation process happens when the dosage of coagulant are varied and added
into all samples, which then undergo flocculation process that clumped the microparticles
into visible particle at various dosages. In water treatment, the addition of coagulant into
wastewater functions in eliminating the turbidity of raw water. Turbidity measures the
cloudiness of water, visibly noted in the colour changes. The addition of sulphuric acid
(𝐻2 𝑆𝑂4 ) and sodium hydroxide(𝑁𝑎𝑂𝐻) would neutralize the wastewater, changing its pH
to 7.0 to optimise the parameter which ensures the effectiveness of the process. Every
operation is handled by ensuring full suspension of solid particles through neutralisation
of ion charge which would form a decent-sized floc to be filtrated out. Hence, turbidity is
reduced resulting in safe pH water level and it emits a pleasant odour. The coagulant
used is aluminium sulphate which is an organic salt used to treat wastewater with pH
ranging from 6.0 to 7.0. In this study, sand is added to acquire high turbidity water as
high initial values were considered, hence sand is synthetically added to form heavier
flocs which can be settled. Furthermore, low turbidity waters are harder to coagulate
because of low concentrations of stable particles (Kalavathy & Giridhar, 2017).

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 Table 4. 1: Effect of different dosage of coagulant on the colour, turbidity and pH of the
wastewater (solution)

Dosage Characteristics of solution

of Turbidity
Sample pH Colour
alum (FNU)
(g) Initial Adjusted Final Before After Before After

A 0.01 6.39 7.10 6.36 1722 137

B 0.02 6.36 7.00 6.52 1078 213

C 0.03 6.32 7.19 6.50 1615 9.74

D 0.04 6.27 7.19 6.53 1239 264

E 0.05 6.22 7.18 5.35 1377 100.1

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 4.1 Influence on different dosage of coagulant on the turbidity of the
wastewater

The influence of aluminium sulphate on raw waste water is visibly noted in the
colour changes. Raw waste water is originally murky, turbid with a decent amount of
suspended particles in it, and it changed upon the addition of coagulant to clear and
transparent. Klimiuk et al. (1999) stated that at neutral condition, an addition in the
quantity of coagulant dosage brings forth an improvement in colour changes or removal,
thus, the treated waste water becomes clearer. The suspended solid particles would
coagulate and left to settle at the bottom, which is called sediment. The density of the
coagulated particles is a lot denser than the treated water, thus it sank, creating 2 layers
consisting of sediment (suspended solid particles) and treated water as pictured in Table
4.1.

Table 4. 2: Removal percentage of turbidity on different aluminium sulphate dosages

Sample A B C D E
Dosage of alum (g) 0.01 0.02 0.03 0.04 0.05
Initial Turbidity (FNU) 1722 1078 1615 1239 1377
Final Turbidity (FNU) 137 213 9.74 264 100.1
Removal Percentage (%) 92.04 80.24 99.40 78.69 92.73

2000
Initial Turbidity Final Turbidity
1800
1600
1400
Turbidity

1200
1000
800
600
400
200
0
0.01 0.02 0.03 0.04 0.05
Dosage of aluminium sulphate (Al2(SO4)3)

Figure 4. 1: Turbidity of each sample at different dosage of aluminium sulphate

According to Leon-Luque et al. (2016), final turbidity is lower than initial turbidity
as turbidity is slowly eliminated by coagulant. The addition of aluminium sulphate

9
(𝐴𝑙2 (𝑆𝑂4 )3 ) into all samples managed to eliminate the turbidity from initially, being at the
range of 1000 -1750 FNU to around 9 – 270 FNU. The differences are significant in
proving that aluminium sulphate is a great substance in treating waste water however,
the amount needed to lower the turbidity till it is safe for consumption has to be further
investigated. At present, there is no reliable formula in determining the most effective
dosage of coagulant to be used in water treatment. However, one of the most reliable
methods in determining the most effective type of coagulant and proper dosage is the jar
test method (Sahu & Chaudhari, 2013). According to Jaeel and Zaalan (2017), optimal
dosage of alum used in treatment plant is 20 mg/L to 30 mg/L. In treatment plant, the
wastewater is treated with coagulant, mainly for it to be disposed safely without affecting
the environment and ecosystem. If the removal percentage is in negative values, this
activity is due to the excess amount of aluminium sulphate used for the treatment. An
excessive amount of aluminium sulphate would result in the solution becoming more
acidic as the flocculation process is disrupted.

Before coagulation and flocculation processes, the turbidity value of each sample
is relatively high and adding aluminium sulphate would reduce the turbidity present.
This happens because the sediment particles in wastewater collided with one another
during the coagulation process due to the stirring action. Precipitation (floc) occurs and it
settles at the bottom. The more active the sediment is in building precipitation, the lower
the turbidity of the treated water. Final turbidity values of Sample B and D are high,
despite both having greater amount of coagulant than the previous samples (A and C).
The increase in final turbidity is due to the hydrolysis products of aluminium in the
system (Packham, 1962). The turbidity of all samples dropped, however, it did not follow
the principle of inverse proportionality, whereby the higher dosages would contribute to
smaller turbidity value. The final turbidity of each sample differed greatly from the
previous sample and it did not line up with the theory in using aluminium sulphate as a
coagulant in waste water treatment.

Turbidity is often caused by the suspended solid particles in it and its removal
percentage is calculated using Equation 4.1.

𝐼𝑛𝑖𝑡𝑖𝑎𝑙 𝑡𝑢𝑟𝑏𝑖𝑑𝑖𝑡𝑦 − 𝑓𝑖𝑛𝑎𝑙 𝑡𝑢𝑟𝑏𝑖𝑑𝑖𝑡𝑦

𝑃𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑜𝑓 𝑟𝑒𝑚𝑜𝑣𝑎𝑙 = × 100% (𝑬𝒒𝒖𝒂𝒕𝒊𝒐𝒏 𝟒. 𝟏)
𝐼𝑛𝑖𝑡𝑖𝑎𝑙 𝑡𝑢𝑟𝑏𝑖𝑑𝑖𝑡𝑦

10
 120.00%

Removal Percentage (%)

100.00%

80.00%

60.00%

40.00%

20.00%

0.00%
0 0.01 0.02 0.03 0.04 0.05 0.06
Dosage of aluminium sulphate (g)

Figure 4. 2: Removal percentage of turbidity versus dosage of aluminium sulphate

In Figure 4.2, Sample C with 0.03 g of aluminium sulphate added in it, has the
most active action on precipitation thus, contributing to lower turbidity of treated water
below 10 FNU. Initially, the turbidity of Sample C is the second highest (1615 FNU) and
it dropped drastically due to higher collision of suspended solid particles during agitation
time. The highest percentage of removal recorded out of all samples is owned by Sample
C at 99.40% while the lowest is at 78.69% (Sample D). Hence, Sample C exhibits the most
optimum behaviour in this study. Lower percentage removal is related to the stirrer speed
which impacts agitation time. According to Pernitsky (2003), higher coagulant doses
would place longer flocculation time and lower filtration rates are much required in high
water turbidity. Thus, optimum turbidity removal and solid-liquid separation mostly
happened in low solubility of coagulant’s pH (Eikebrokk, 1990).

4.2 Influence of different dosage of coagulant on the pH of the

wastewater

The pH value of wastewater was measured and adjusted to pH 7 since the

coagulant (aluminium sulphate) will work effectively in a weak alkaline solution due to
their ability in promoting the neutralisation of non-stable colloidal solids to stick together,
hence forming micro flocs. The addition of sodium hydroxide and hydrochloric acid to the
wastewater solution shall be done carefully as the slightest amount could deter the pH
value. The wastewater with adjusted pH is stirred and coagulant is added on each sample.
The pH value decreased significantly upon the addition of coagulant, shifting the solution
to the acidic range as adding coagulant is like adding a strong acid. Treated water tends
to be more acidic as the addition of aluminium sulphate would incorporate higher amount

11
of high positive charge ions into the wastewater. According to Tang et al. (1998), addition
of 1mg/L of alum might neutralise 0.5 mg/L of hydrogen ions. Equation 4.2 shows the
release of hydrogen ions, sulphate and aluminium ions when it is dissolved in wastewater.

𝐴𝑙2 (𝑆𝑂4 ) ∙ 14𝐻2 𝑂 → 2𝐴𝑙(𝑂𝐻)3 + 6𝐻 + + 3𝑆𝑂42− + 8𝐻2 𝑂 (𝑬𝒒𝒖𝒂𝒕𝒊𝒐𝒏 𝟒. 𝟐)

Aluminium and iron salts hydrolysed in water and become cations which react
with negatively charged particles. According to Camejo et al. (2014), the precipitate is
𝐴𝑙(𝑂𝐻)3 and the ions remained are hydrogen and sulphate ions. The hydrolytic behaviour
of the coagulant affects the contaminants removal, floc ability to settle, sludge properties
and aluminium concentration which remains in the supernatant (Stephenson & Duff,
1996). The ions collided and dissolved along with the sediment. According to Nieto et al.
(2011), particles collided due to their relative motion and the interaction between particles
would subsequently determine the stability against aggregation. Forces such as attractive
and repulsive forces may be operative and is initiated through multiple ways such as pH
and salt concentration. When the solution becomes more acidic, it is due to electrostatic
repulsion between the particles. The increasing dosage of coagulant caused the
electrostatic repulsion to take place whereby the role of positive charged particle becomes
aggressively dominant (Ma et al., 2012).

Adding more aluminium sulphate would reduce the presence of hydroxide ions
(OH-) in the solution. Doses less than 5mg.L is believed to result in charge neutralization
(destabilisation) being the primary mechanism while doses more than 5mg/L, entrapment
mechanism would become pre-dominant (Benson, 2006). To achieve destabilization
through charge neutralisation, distribution of the coagulant plays an active role because
the intermediate products of the reaction are destabilizing agents. The pH value of all
samples except Sample E, dropped gradually upon the addition of coagulant. However,
Sample E showed a steep drop in its pH value due to inadequate amount of alkalinity in
the sample. According to Sahu and Chaudhari (2013), steep drop in pH value could be
avoided by introducing buffer capacity or a sufficient supply of bicarbonate to form metal
hydroxide.

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 8

6
R² = 0.39
5
pH

4 Adjusted pH
3 Final pH
2 Linear (Final pH)

0
0 0.01 0.02 0.03 0.04 0.05 0.06

Dosage of aluminium sulphate (g)

Figure 4. 3: pH of wastewater (adjusted and post-treated) at different doses

In Figure 4.3, the final pH values decreased linearly with the amount of each
dose and the squared correlation, 𝑹𝟐 is far from 1. The value of correlation must be
between 0.8 and above, to be considered valid and acceptable. Since the squared
correlation is less than 1, not even amounting to half, thus the result is considered invalid
and acceptable. These failures might somehow be contributed by random or human error,
such as, method of transferring the coagulant to wastewater is impractical. The coagulant
particles are small and easy to be carried away by air, thus, the value that was originally
weighed might differ. Overdosing the amount of coagulant is harmful to the environment
as the pH value becomes overly acidic, thus it is recommended that accurate amount of
coagulant is added or opting for an organic coagulant instead of chemical-based coagulant
to maintain the pH value during treatment process. High concentration of sulphate ions
which will remain in the solution possessed downstream treatment difficulties and will
lead to increase total dissolved solids levels (Stephenson & Duff, 1996). To maintain an
optimum pH value, artificial buffer is required as pH is a critical condition for coagulation
(Peavey et al., 1985).

5.0 CONCLUSION

In conclusion, wastewater treatment processes such as coagulation, flocculation

and sedimentation are able to be performed using aluminium sulphate and has shown
that final turbidity is lower than initial turbidity, whereby the values of each sample are,

13
137, 213, 9.74, 264 and 100.1 FNU. The coagulant added to the wastewater changed the
turbidity and is further concluded that the relationship between dosage of aluminium
sulphate and turbidity is inversely proportional. Furthermore, visible changes such as the
colour of wastewater turned clearer are noted upon adding the coagulant. It is
recommended that the experiment is done with different wastewater taken from various
sources to thoroughly investigate and provide valid comparison with different doses of
coagulant. Lastly, higher amount of coagulant contributed higher pH value (acidic) with
low turbidity.

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6.0 REFERENCES

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