CDB 3082

Chemical Engineering Laboratory IV

Long Report
MAY 2016

EXPERIMENT : COAGULATION AND WATER HARDNESS

GROUP : A8
GROUP MEMBERS : KOI ZI KANG 18868
MASRIHAN BIN ABU HASAN 19454
NOOR HAFIZAINIE BINTI MOHD ZOHAN 19323
SITI NUR AISYAH BINTI AHMAD 19353
LAB INSTRUCTOR : MISS NURAIN
DATE OF EXPERIMENT : 28 JUNE 2016
Table of Contents

Chapter 1: Introduction
Summary ........................................................................................................................ 1
Problem Statement ......................................................................................................... 1
Objectives ...................................................................................................................... 1

Chapter 2: Literature Review ..................................................................................................... 1

Chapter 3: Methodology ............................................................................................................ 3

Chapter 4: Results and Discussions

Results ............................................................................................................................ 5
Discussions .................................................................................................................. 11
Error and Recommendation ......................................................................................... 11

Chapter 5: Conclusion ............................................................................................................. 12

References ................................................................................................................................ 12

Appendix .................................................................................................................................. 13

Questions and Answers ........................................................................................................... 14

1.0 INTRODUCTION

1.1 Summary

A common wastewater monitoring test is coagulation, flocculation and water hardness. The
purpose of this experiment is to determine the optimum coagulant dosage by varying the
concentration. Also, we aimed to compare the effectiveness of two different coagulants which
are alum solution and ferric sulfate. Effect of increasing concentration onto turbidity and pH
value of the sample water is to be discussed as well. . Based on the result, the more effective
coagulant is alum solution which can reduce turbidity and did not cause the sample turn into
acidic solution immediately. For ferric sulphate, it causes the pH value to increase as the
concentration of ferric sulphate increase. Both optimum dosage of alum solution and ferric
sulphate was found to be 20ppm, which is 20ml from 1g/1L of each respective solution.

1.2 Problem Statement

- What is the optimum coagulant dosage using different types of coagulants by varying their
concentration as well as their effectiveness?

1.3 Objectives

i. To become familiar with wastewater treatment plant tests.

ii. To illustrate some difficulties in performing these tests.

iii. To illustrate the principles of coagulation and water hardness.

2.0 LITERATURE REVIEW (THEORIES)

i) Water Hardness
Hard water is water that has high mineral content (in contrast with "soft water"). Hard water
is formed when water percolates through deposits of limestone and chalk which are largely
made up of calcium and magnesium carbonates. The simple definition of water hardness is
the amount of dissolved calcium and magnesium in the water. Hard water is high in dissolved
minerals, both calcium and magnesium. (USGS, n.d.)

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According to Fairfax Water (n.d.), many industrial and domestic water users are concerned
about the hardness of their water. Hard water requires more soap and synthetic detergents for
home laundry and washing, and contributes to scaling in boilers and industrial equipment.
Hardness is caused by compounds of calcium and magnesium, and by a variety of other
metals. Water is an excellent solvent and readily dissolves minerals it comes in contact with.
As water moves through soil and rock, it dissolves very small amounts of minerals and holds
them in solution. Calcium and magnesium dissolved in water are the two most common
minerals that make water "hard."

The hardness of water is referred to by three types of measurements: grains per gallon,
milligrams per liter (mg/L), or parts per million (ppm). Typically, the water produced by
Fairfax Water is considered "moderately hard" to "hard." The table below is provided as a
reference.

Water Hardness Scale

Grains Per Gallon Milligrams Per Liter (mg/L) or Classification
Parts Per Million (ppm)
less than 1.0 less than 17.1 Soft
1.0 - 3.5 17.1 - 60 Slightly Hard
3.5 - 7.0 60 - 120 Moderately Hard
7.0 - 10.5 120 - 180 Hard
over 10.5 over 180 Very Hard
Table 2.1: Water Hardness Scale

ii) Coagulation
Solids are removed by sedimentation or settling followed by filtration. Small particles are not
removed efficiently by sedimentation because they settle too slowly; they may also pass
through filters. They would be easier to remove if they clumped together (coagulated) to form
larger particles, but they don't because they have a negative charge and repel each other (like
two north poles of a magnet). In coagulation, we add a chemical such as alum which
produces positive charges to neutralize the negative charges on the particles. Then the
particles can stick together, forming larger particles which are more easily removed. The
coagulation process involves the addition of the chemical (e.g. alum) and then a rapid mixing
to dissolve the chemical and distribute it evenly throughout the water. (Michigan

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Environmental Education Curriculum, n.d.)

iii) Turbidity and pH Value

Turbidity is the cloudiness or haziness of a fluid caused by large numbers of individual
particles that are generally invisible to the naked eye, similar to smoke in air. The
measurement of turbidity is a key test of water quality. Fluids can contain suspended solid
matter consisting of particles of many different sizes. While some suspended material will be
large enough and heavy enough to settle rapidly to the bottom of the container if a liquid
sample is left to stand (the settable solids), very small particles will settle only very slowly or
not at all if the sample is regularly agitated or the particles are colloidal. These small solid
particles cause the liquid to appear turbid.

pH is a numeric scale used to specify the acidity or basicity of an aqueous solution. It is

approximately the negative of the logarithm to base 10 of the molar concentration, measured
in units of moles per liter, of hydrogen ions. More precisely it is the negative of the logarithm
to base 10 of the activity of the hydrogen ion. Solutions with a pH less than 7 are acidic and
solutions with a pH greater than 7 are basic. Pure water is neutral, being neither an acid nor a
base. Contrary to popular belief, the pH value can be less than 0 or greater than 14 for very
strong acids and bases respectively.

3.0 METHODOLOGY

Experiment A: Determination of Optimum Coagulant Dosage

1. The coagulant is prepared.

2. The water sample is analysed to determine its pH and turbidity.
3. Prepare 6 beakers and pour 1 liter of the waste water into each beaker. Different portions
of coagulants of 0, 10, 20, 30, 40 and 50 mg/L are prepared.
4. The water is mixed at 50 rpm to ensure complete mixing.
5. Mixing speed is increased to 250 rpm. The chemicals are added to each reactor near the
vortex. Make sure that the reactor is dosed at the same time.
6. The water is mixed rapidly at 250 rpm. The mixing is then reduced to 60 rpm for 9 min.
Mixing is reduced to 25 rpm for 4 min. Lastly, mixing is reduced to 10 rpm for 2 min. All
the reactors are observed to detect the formation of flocs and the time of floc appearance is
recorded.

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7. Mixers are turned off and the relative floc size is recorded.
8. The particles is allowed to settle down for 20 min. The clarity of supernatant liquid and
settling characteristics of the floc is noted.
9. The turbidity and pH of sample water is measured by sampling at the top without disturbing
the sediment in the sampling.
10. The depth of sludge in the beaker is measured.
11. The graph of turbidity against alum dosage is plotted.

Experiment B: Determination of Optimum pH

1. The jar test is repeated using observed optimum dosage of aluminium by adjusting the pH
of water sample in each jar to 3, 5, 7, 9, and 11 with NaOH or H2SO4 prior adding coagulant.
2. The turbidity and pH of liquid in each jar is measured by sampling at the top without
disturbing the sediment in the sampling.
3. The depth of sludge in the beaker is measured.
4. The graph of turbidity against pH is plotted.

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4.0 RESULTS AND DISCUSSIONS

4.1 Results

Coagulant: Alum solution Coagulant: Ferric Sulfate

0 ml

Both seemed to be turbid. There were some sediments being settled at the bottom of both
beaker. The sediments are deduced to be the muds collected along with the sample.
20 ml

- The solution was colorless - The solution was almost colorless.

- Small size particles or sediments were - Small size particles or sediments were
found at the bottom of the beaker found at the bottom of the beaker
- The sediments did not clump with each - The sediments did not clump with each
other. other.

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 40 ml

- The solution was colorless. - The solution was yellowish.

- There were medium sized particles being - There were medium sized particles being
settled at the bottom of the beaker. settled at the bottom of the beaker.
- Some of the particles clumped together. - Some of the particles clumped together.
60 ml

- The solution was colorless. - The solution was more yellowish.

- There were medium particles being - There were medium particles being
settled at the bottom of the beaker. settled at the bottom of the beaker.
- More particles clumped together - More particles clumped together.
80 ml

- The solution was colorless. - The solution was more yellowish.

- There were large particles being settled - There were large particles being settled at
at the bottom of the beaker. the bottom of the beaker.
- A lot more particles clumped together. - A lot more particles clumped together.

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 100 ml

- The solution was colorless. - The solution was more yellowish.

- There were large particles being settled at - There were large particles being settled at
the bottom of the beaker. the bottom of the beaker.
- Almost all particles clumped together. - Almost all particles clumped together.

Table 4.1: The end results of the experiment and observation of the sediment produced

Alum solution

Before After
Coagulant (ml)
Turbidity (NTU) pH Turbidity (NTU) pH
0 109 6.80 89.2 6.80
20 123 6.85 2.65 5.41
40 118 6.93 2.9 4.66
60 114 6.91 2.86 4.54
80 118 6.81 4.67 4.44
100 139 6.86 8.33 4.37
Table 4.2: The data of the sample before and after addition of Alum solution as coagulant

Ferric Sulfate

Before After
Coagulant (ml)
Turbidity (NTU) pH Turbidity (NTU) pH
0 153 6.98 127 6.98
20 143 6.99 7.43 4.68
40 156 6.98 17.1 3.33
60 158 6.96 17.6 3.06
80 154 6.93 21.8 2.89
100 210 6.96 28 2.78
Table 4.3: The data of the sample before and after addition of Ferric Sulfate as coagulant

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 Turbidity vs. Alum solution concentration
160

140

120
Turbidity, NTU

100

80
Before
60 After

40

20

0
0 20 40 60 80 100
Coagulant, ml

Graph 4.1: The Bar chart of Turbidity vs. Volume of Alum solution as coagulant

pH vs. Alum solution volume

8

5
pH

4
Before
3 After

0
0 20 40 60 80 100
Coagulant, ml

Figure 4.2: The Bar chart of pH value vs. Volume of Alum solution as coagulant

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 Turbidity vs. Ferric Sulfate volume
250

200
Turbidity, NTU

150

Before
100 After

50

0
0 20 40 60 80 100
Coagulant, ml

Graph 4.3: The Bar chart of turbidity vs. Volume of Ferric Sulfate as coagulant

pH vs Ferric Sulfate volume

8

5
pH

4
Before
3 After

0
0 20 40 60 80 100
Coagulant, ml

Graph 4.4: The Bar chart of pH value vs. Volume of Ferric Sulfate as coagulant

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 Turbidity vs. Coagulant Volume
140

120

100
Turbidity, NTU

80

Ferric Sulfate
60
Alum solution

40

20

0
0 20 40 60 80 100
Flocculant, ml

Graph 4.5: The Bar chart of Turbidity vs. Volume of different coagulant

pH vs. Coagulant Volume

8

5
pH

4
Ferric Sulfate
3 Alum solution

0
0 20 40 60 80 100
Flocculant, ml

Graph 4.6: The Bar chart of pH value vs. Volume of different coagulant

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4.2 Discussion

From the experiment conducted, we can identify that coagulation can be used to purify
water with high turbidity. There are many factors affecting the coagulation rate, for instance
temperature, concentration of coagulant and also type of coagulation. Many types of coagulants
had been introduced to treat contaminated water however the type of coagulant we should use
depends on the type of treatment that is to be carried out. Based on the figures above, we can
clearly see that the coagulant cleaned the water by aggregating the impurities in the water into
floc and then it settled at the bottom of the beaker. In this experiment, we differed the type of
the coagulant (Alum solution and Ferric Sulfate) and varied concentration of the coagulants
respectively. We measured the turbidity and also the pH value of the sample water before and
after the addition of coagulant to identify the changes and thus determine the optimum dose.
From graph, we can see that the more effective coagulant for this experiment is Alum solution
as it managed to reduce turbidity of the sample water to the least amount which is 2.65 NTU.
Also, alum solution did not cause its pH value to drop drastically to form acidic solution.
Instead, addition of ferric sulfate decreases the pH value of the sample in a drastic trend when
its concentration increases. We can also see that the optimum dose of alum solution is 20 ml
from 1g/1L solution which is 20ppm. This is because this amount reduces turbidity of the
sample water to the least amount and the pH value was maintained near to neutral pH value.
For ferric sulfate, the optimum dose is also 20 ml from 1g/1L solution which is 20ppm. This is
because this amount reduces turbidity of the sample water to the least amount and the pH value
was maintained near to neutral pH value.

4.3 Errors and Recommendations

i. Error: Systematic error when using the pH meter and spectrophotometer.

Recommendation: The equipment should be calibrated well before starting the
experiment and make sure to rinse the equipment to remove impurities so that more
accurate reading will be obtained.

ii. Error: Parallax error when measuring the volume of water sample and the depth of
sludge.
Recommendation: Make sure the eyes level is perpendicular to the reading scale
to avoid the error.

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 iii. Error: Human error might occur when the addition of coagulant did not happen at
the same time due to different location of beakers.
Recommendation: One person should observe the overall situation and remind the
others to add the coagulant at the exact time.

5.0 CONCLUSION

Coagulation is a process of destabilization of colloids by addition of chemical that can

neutralize the negative charges which is known as coagulants. In this experiment we also deal
with water hardness. Basically, water hardness is cause by dissolved magnesium ions and
calcium ions. There are two coagulants used in the experiment; alum solution and ferric
sulphate. By using different type of coagulant at different concentration, we study the optimum
coagulant dosage. Based on the result, the more effective coagulant is alum solution which can
reduce turbidity and did not cause the sample turn into acidic solution immediately. For ferric
sulphate, it causes the pH value increase as the concentration used increase. Both optimum
dosage of alum solution and ferric sulphate is 40ppm, 20ml from 1g/1L solution.

REFERENCES

Fairfax Water. (n.d.). Explanation of Water Hardness. Retrieved 16 July 2016, from
https://www.fcwa.org/water/hardness.htm

Hard water. (n.d.). Retrieved 15 July 2016, from https://en.wikipedia.org/wiki/Hard_water

Michigan Environmental Education Curriculum. (n.d.). Drinking Water Treatment

Coagulation. Retrieved 15 July 2016, from
http://techalive.mtu.edu/meec/module03/WastewaterRegulations.htm

pH. (n.d.). Retrieved 15 July 2016, from https://en.wikipedia.org/wiki/PH

Turbidity. (n.d.). Retrieved 15 July 2016, from https://en.wikipedia.org/wiki/Turbidity

USGS. (n.d.). Water Hardness. Retrieved 16 July 2016, from

http://water.usgs.gov/edu/hardness.html

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APPENDICES

1) Calculations for concentration of Alum solution and Ferric Sulfate:

Using 1 1 = 2 2

Lets say V1 = 20ml of Alum solution

Given M1 = 1g/L = 1000 mg/L = 1000 ppm and V2 = 1000 ml

1 1 = 2 2

1000ppm (20ml) = M2 (1000ml)

M2 = 20 ppm

2) Pictures

Figure 1: Turbidity Measurement Equipment

Figure 1: pH Value Measurement Equipment

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QUESTIONS AND ANSWERS

1. What is optimum dosage of alum and at what pH?

The optimum dosage of alum is 40ppm at 20ml from 1g/1L of the solution. The pH of
solution at the optimum dosage is 5.41.

2. Did the pH increase or decrease during the coagulation? Why?

The pH is decrease as the amount of coagulant use is increase for both Alum solution
and ferric sulphate. But, the pH decrease in a drastic trend when using ferric sulphate
compare to Alum solution. Adding of alum or ferric sulphate has the same effect as
adding a strong acid. Therefore, the pH and alkalinity of the system is decreasing.

3. Compare the production of sludge from experiment done in A and B. Which has
more sludge generation and why?
Theoretically Experiment A should have generate more sludge compare
Experiment B because alum solution has its own optimum pH, so only one of
the reactor in experiment B that have optimum pH for Alum solution will have more
sludge. While in experiment A, the pH is almost same for all the reactor, only
more coagulant generate more sludge. But, our result during the experiment are
not produce any sludge.

4. What can you conclude from the experiment done on the important factors
affecting coagulation?
In this experiment, we are study the effect of dosage and pH on the coagulation.
Based on part A experiment, at the pH value of 6.8 to 7.0, the optimum dosage of
coagulant is 40ppm from 20 ml of 1g/1L solution. That is the suitable amount or
dosage need to reduce the turbidity and get the desired treated solution. Turbidity
removal efficiency slightly decrease when the concentration of coagulation increase.
5. Explain why trivalent cations are important for an effective coagulation?
In order to neutralize the charges of the colloids, the addition of an ion of opposite
charge to the colloids is needed. Using of trivalent cations can reduced the charges
faster compare to monovalent or divalent ion.

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6. Assuming that a water plant influent is 0.044 m3/s and alum is used to remove
particulate matter, reducing the concentration of organic matter and reduce the
alkalinity of water according to the following equation:

Al2(SO4)3.14H2O + 6HCO3- 2Al(OH)3 (s) +6CO2 + 14H2O + 3SO2 -4

If the organic matter concentration is reduced from 8 mg/L to 3 mg/L, determine the
total mass of alkalinity consumed and the total mass of dry solids removed per day
using the optimum dosage obtained.

Optimum dosage= 40ppm=40mg/L

Molecular weight of alum = 594.35g/mol
40 103
( ) ( ) 6.73 105
= =
594.35/

3
= 6 6.73 105
4.0384
=

4.038 104 3
= 0.044 1000 3 86400

= 1535.09 /

1 mole of alum=2 moles of precipitate

= 2 6.73 105
= 1.346 104 /

1.346 104 3
= 0.044 1000 3 86400

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= 511.70 78


= 39.91

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