A

TECHNICAL REPORT

ON

STUDENT’S INDUSTRIAL WORK EXPERIENCE SCHEME

(SIWES)

UNDERTAKEN AT

WATER CORPORATION OF OYO STATE

(WCOS)

IBADAN-IFE EXPRESS ROAD, ASEJIRE,

IBADAN, NIGERIA

BY

AGBEYOMI FAVOUR DAMILOLA

1402329

SUBMITTED TO

THE DEPARTMENT OF SCIENCE LABORATORY AND TECHNOLOGY,

EKITI STATE UNIVERSITY, ADO-EKITI,

EKITI STATE, NIGERIA

JANUARY 2019

ii
 CERTIFICATION
This is to certify that this report is a given account of Student Industrial Work

Experience Scheme (SIWES) undertaken by AGBEYOMI FAVOUR DAMILOLA of

Matriculation number 1402329 at WATER CORPORATION OF OYO STATE (WCOS)

ASEJIRE IBADAN for a period of six months and has been prepared in accordance to

regulations guiding the preparation of reports in the Department of Science Laboratory and

Technology Ekiti State University, Ado-Ekiti.

SUPERVISOR’S SIGNATURE AND DATE STUDENT’S SIGNATUREAND DATE

ii
 ACKNOWLDGEMENT
Truly, it takes a community to train a child. I would like to first acknowledge

Almighty God for seeing me through and giving me the wisdom to write this report. I would

like to acknowledge the HOD of this prestigious department, Dr. Ademiluyi and all my

lecturers who stand as the shepherd on the road to my success. My sincere acknowledgement

also goes to Mr. Toromade, the Scheme manager of WCOS Asejire water supply scheme and

Mrs. J. A Aiyelabola, the Head of Quality control department for opening the line for

students like myself to learn from this great corporation. I can’t forget the help of the

members of staff who were always ready to answer my incessant questions.

My list would be incomplete without acknowledging my parents, Mr. and Mrs. Agbeyomi

who made my SIWES an enjoyable. I would like to acknowledge other IT students who made

W.C.O.S Asejire a wonderful place of internship. I pray God blesses them all. Amen.

iii
 ABSTRACT
The Industrial training program was designed to enable the 400 level students to

acquire practical skills in their field of study and give account and details of their training

experience during the period of six months. It was on this note that I gave the account of my

industrial experience at Water Corporation of Oyo state, Asejire supply scheme. The report

gives organized detailed information on the various processes of water treatment at Asejire

Water Treatment Plant, especially at the Quality Control Unit.

The 28m deep dam supplies water through a low lift pump (weir pump at the rate of

2,180m³/hr or dresser pump at the rate of 4500m³/hr) to the treatment plant. The aerator

receives the raw water and mixes with alum water to coagulate it leading to the flocculation

process; the flocculated water is hereby transferred to the sedimentation tank for easy

separation of the flocs from the water. The decanting trough aids the movement of water from

the sedimentation tank into the filter bed for filtration, leading to the clear well where

addition of lime and chlorine is effected to ensure the boosting of the water pH and

disinfection respectively.

Thus, the final water certified for consumption is hereby transported to Ibadan

Booster Station through the high lift pump for unit distribution.

iv
 Table of Contents
CERTIFICATION ...................................................................................................................ii
ACKNOWLDGEMENT ........................................................................................................iii
ABSTRACT ............................................................................................................................. iv
LIST OF FIGURES ...............................................................................................................vii
LIST OF TABLES ................................................................................................................viii
CHAPTER ONE ...................................................................................................................... 1
1.0 INTRODUCTION ............................................................................................................................. 1
1.1 Students’ Industrial Work Experience Scheme (SIWES) ............................................................... 1
1.1.1 Aims and Objectives of the Students’ Industrial Work Experience Scheme (SIWES) ..... 2
1.1.2 Objectives of the Report ........................................................................................................ 2
1.1.3 Scope of the Report ............................................................................................................... 3
1.2 Brief History of Water Corporation of Oyo State.......................................................................... 3
1.2.1 Aims And Objectives Of Water Corporation Of Oyo State .................................................... 5
1.2.2 Various directorates in WCOS ................................................................................................ 5
CHAPTER TWO ..................................................................................................................... 8
2.0 WATER TREATMENT...................................................................................................................... 8
2.1 Introduction to water treatment .................................................................................................. 8
2.2 Stages involved in water treatment process ................................................................................ 8
2.2.1 Screening................................................................................................................................ 8
2.2.2 Aeration ................................................................................................................................. 9
2.2.3 Coagulation and Flocculation............................................................................................... 11
2.2.4 Sedimentation .......................................................................................................................... 15
2.2.5 Filtration ............................................................................................................................... 17
2.2.6 Liming ................................................................................................................................... 19
2.2.7 Disinfection / Post Chlorination ........................................................................................... 19
2.3 Chemical Dosing .......................................................................................................................... 20
2.3.1 Aluminium Sulphate Dosing ................................................................................................. 20
2.3.2 Lime Dosing .......................................................................................................................... 22
2.3.3 Chlorine Dosing .................................................................................................................... 22
CHAPTER THREE ............................................................................................................... 23
3.0 WATER QUALITY CONTROL UNIT ................................................................................................ 23
3.1 Quality Assurance and Quality Control ....................................................................................... 23
3.2 Quality Control Laboratory ......................................................................................................... 23

v
 3.2.1 Physical Test ......................................................................................................................... 23
3.2.2 Physico-Chemical Tests ........................................................................................................ 23
3.2.3 Chemical Tests ..................................................................................................................... 24
3.2.4 Bacteriological Tests ............................................................................................................ 24
3.2.1 Physical Tests ....................................................................................................................... 24
3.2.2 Physicochemical Tests.......................................................................................................... 25
3.2.3 Chemical Tests ..................................................................................................................... 27
3.2.4 Bacteriological Analysis ........................................................................................................ 34
3.3 Atomic Absorption Spectrophotometer (AAS) ........................................................................... 39
3.3.1 Sample Preparation.............................................................................................................. 39
3.3.2 Components of the Spectrophotometer ............................................................................. 40
3.4 Preparation of some Reagents used in the Laboratory .............................................................. 42
3.4.1 Preparation of Ammonia Buffer........................................................................................... 42
3.4.2 Preparation of Erichrome Black-T Indicator......................................................................... 42
3.4.3 Preparation of Murexide Indicator ...................................................................................... 43
3.4.4 Preparation Of 1% Aluminium Sulphate (Alum) Solution .................................................... 43
3.4.5 Preparation of Bromothymol Blue Indicator ....................................................................... 43
3.4.6 Preparation of Phenol Red Indicator ................................................................................... 44
3.4.7 Preparation of Methyl Orange Indicator ............................................................................. 44
3.4.8 Preparation and Potency Test of High Test Hypochlorite (HTH) ......................................... 45
3.4.9 Preparation of Agno3 for Argentiometric Titration ............................................................. 45
3.5 Lime Analysis ............................................................................................................................... 46
3.6 Alum Analysis .............................................................................................................................. 46
3.6.1 Title: Insoluble matter .......................................................................................................... 46
3.6.2 Title: Soluble iron compound ............................................................................................... 47
3.6.3 Title: Content of alumina ..................................................................................................... 48
3.7 WHO Standard for potable water ............................................................................................... 49
CHAPTER FOUR.................................................................................................................. 53
4.0 RECOMMENDATION AND CONCLUSION..................................................................................... 53
4.1 Recommendation........................................................................................................................ 53
4.2 Conclusion ................................................................................................................................... 53
REFERENCES....................................................................................................................... 54

vi
 LIST OF FIGURES
Figure 1.1 low lift pump station 4
Figure 1.2 A cross section of dam gate 4
Figure 2.1 screen bar 10
Figure 2.2 spray-like aerator 10
Figure 2.3 cascade aerator 11
Figure 2.4 destabilized colloids 12
Figure 2.5 formation of flocs 12
Figure 2.6 sedimentation tank 16
Figure 2.7 sedimentation tank after complete de-sludge 17
Figure 2.8 filter bed during backwashing 18
Figure 2.9 filter bed without backwashing 18
Figure 2.10 flocculating machine 21
Figure 3.1 prepared standard for silica test 34
Figure 3.2 sterilized nutrient agar 37
Figure 3.3 prepared media set for incubation 38
Figure 3.4 bucket autoclave for moist-heat sterilization 38
Figure 3.5 atomic absorption spectrophotometer 41

vii
 LIST OF TABLES

Table 2.1 Alum Dosage 21

Table 3.1 Physiochemical Properties of Potable Water 49

Table 3.2 Bacteriological Properties of Potable Water 52

viii
 CHAPTER ONE

1.0 INTRODUCTION

1.1 Students’ Industrial Work Experience Scheme (SIWES)

The student industrial work experience scheme (SIWES) was introduced in Nigeria

by the decree No. 46 of 1971 for students in higher institution and was designed to enable

students have practical industrial knowledge in their various discipline. More so, this

programme designed by the Federal Government of Nigeria via the Industrial Training Fund

(ITF) as the supervisor in collaboration with the tertiary institution to train students

professionally in their respective fields of learning hence providing each student an

opportunity for practical exposure outside the institution through attachment to industrial

establishments, companies, research stations etc.

SIWES is more or less skill training programme, which forms part of the approved

minimum academic requirement in the various degree programs for all Universities in

Nigeria. It is an effort to bridge the gap existing between theory and practice of Engineering

and Technology, Science, Agriculture, Medicine, Management and other professional

Education programme in Nigeria tertiary institutions.

It is aimed at exposing students to the operation of machine and equipment,

professional work methods and industrial safety of works in industries and other

organizations. The scheme is tripartite programme involving the students, the university and

the industries (employers of labour). (Onwuji, 2004)

Participation in SIWES has become a necessary pre-condition for the award of

Diploma and Degree certificates in specific disciplines in all institutions of higher learning in

the country, in accordance with the education policy of government.

1
1.1.1 Aims and Objectives of the Students’ Industrial Work Experience Scheme
(SIWES)

The aims and objectives of the students’ industrial work experience scheme are

among others:

(1) To provide an avenue for the students in institution of higher learning to bridge the

gap between theoretical knowledge in their chosen course of study

(2) To prepare students for the work situation they are likely to meet after graduation

(3) To promote technological advancement and enhance students’ contribution to the

economic development of the nation.

(4) To acquire professional ethics and etiquettes

(5) To develop good working relationship between superior and subordinates

(6) To expose students to work methods and techniques in handling equipment and

machineries that they may not have opportunity to work with within educational

institutions.

(7) Witnessing of large scale practical which may be different from small scale practical

obtainable in the school laboratory though both may be based on the same principle.

1.1.2 Objectives of the Report

The following are the objective of the report.

(1) To present a detailed review of the operation at Water Coporation of Oyo State,

Asejire.

(2) To present the details of the training undergone and the skilled acquired

2
1.1.3 Scope of the Report
This report covers the extent of training undergone by the trainee while on attachment

with the Water Corporation of Oyo State, Asejire. With a thorough explanation of the work

carried out during the period of the training.

1.2 Brief History of Water Corporation of Oyo State

The Water Corporation of Oyo State (WCOS) is a public corporation carved out of

the Western Nigeria Water Corporation. It has seven Directorates and four Units which

reports the general manager for the day-to-day activities. In addition, the Corporation has its

headquarter at secretariat, Ibadan with district offices located at Agodi, Bodija, Egbeda,

Jericho, Oke-Ado, Ogbomoso, Oyo and Saki. The water supply system includes raw water

storage, raw water pipework, water treatment (comprising of flocculation, coagulation,

sedimentation/clarification and disinfection), treated water storage (Clear well) and treated

water distribution.

Surface water source for Asejire water treatment plant is a man-made Dam,

established on 1st February, 1966 and was commissioned by General Yakubu Gowon on 17th

November, 1972. The cost of the project was about ₦22 million. Asejire dam has its length

and depth as 63.4m and 26.4m respectively, and a capacity of 32,580million litres. The plant

has daily production of 81million litres. Asejire Water Treatment Scheme is located between

two states; Osun and Oyo State. Asejire dam is named after a nearby village in the Old Ife,

taking its source from Osun-Osogbo River in Osun State.

Along the dam, is a confluence formed from three rivers namely: Agbora from Ikire,

Odo Oba from Iwo and Osun-Osogbo from Osogbo.

Nigeria Breweries and Nigeria Bottling Company also have their flow station on the

dam to source for raw water for their production.

There are altogether nine (9) functioning water supply schemes in Oyo State located

in the strategic places of the State: Asejire, Eleyele, Ogbomosho, Oyo, Eruwa, Saki, Iseyin,

3
Kisi and Igbeti, among which Asejire and Eleyele schemes are found in Ibadan.

Figure 1.1: Low Lift Pump Station

Figure 1.2: A Cross Section of the Dam Gate

4
1.2.1 Aims And Objectives Of Water Corporation Of Oyo State
The main objectives of Water Corporation of Oyo state are as follows:

(1) To control and manage all water works vested under the Edict establishing the

corporation.

(2) To establish, control, manage, extend and develop such new waterworks and to

extend and develop such existing ones as the corporation may consider necessary for

the purpose of water supply in order to meet the requirement of the general public,

agriculture, trade and industry in various parts of the state.

(3) To ensure that water is supplied to the consumer thereof at reasonable charges and in

potable quality and adequate quantity.

(4) To organize the conduct of comprehensive research for the purpose of the Corporation

from time to time on matters relating to its functions under the Edict. This helps to

submit on request, the result of such research to the executive council for utilization

of the same, by it in the formulation of policy relating to the supply and usage of

water in the state.

1.2.2 Various directorates in WCOS

There are eight Directorates in the corporation which play specific roles in achieving

WCOS’s mandate. The Directorates are as follows:

1. Administration and Human resources directorate: This directorate handles

staff recruitment/appointment, staff promotion, transfer and posting in the

corporation. It is also involved in the documentation of new staff records,

prepares staff nominal roll and issues identity cards.

2. Finance and Supply directorate: This directorate co-ordinates the general day

to day financial functions of the corporation, disburse funds of the corporation as

approved by the management, pay all staff salaries when due, prepare budget

5
 estimate for the agency. They also keep profit and expenditure account of the

corporation.

3. Directorate of Design, Research, Planning and Construction: This is a service

directorate that is responsible for planning, researching and collection of

statistical data as well as coordinating and documenting the activities of all other

directorates for efficient achievement of goals of the cooperation. They also

coordinate project design and construction of new treatment plant.

4. Mechanical and Electrical: This directorate sees to the repair of mechanical and

electrical faults on machines such as switch boards, pumping machines, air

blower, chlorine injector, dam gate etc. They are also in charge of maintenance of

issues related to power supply. COS and their functions

5. Quality Control: This directorate is tasked with the analysis and pronouncement

of the quality and safety of final water produced. They are also in charge of

maintaining and controlling the activities of the treatment plant.

6. Commercial Services: This directorate is involved in printing of bills and

invoices.

7. Audit, Project Monitoring, Training and Computer units.

8. Operation and Maintenance: This directorate comprises civil engineers,

plumbers and technologists who function in repair and replacement of damaged

pipes and removing blockages from pipes.

In addition, the corporation has district offices located at Agodi, Egbeda, Jericho, Oke-

Ado, Bodija, Oyo, Ogbomosho and Saki, of which each district is divided into sectors where

the public can report problems for rectification. There is also Leak Detection and Emergency

Unit at the Headquarters for the same purpose.

6
 CHAIRMAN OF BOARD OF DIRECTORS

GENERAL
MANAGER

SECRETARY OPERATION QUALITY MECHANICAL COMMERCIAL

AND CONTROL AND SERVICES
MAINTENANCE ELECTRICAL AND FINANCE

DISTRICT SCHEME
MANAGER MANAGER

CIVIL ELECTRICAL QUALITY ADMINIST MECHANICAL

ENG.DEPT ENG. DEPT CONTROL RATION ENG. DEPT
OFFICE

LABORATORY TREATMENT
SECTION PLANT

CHEMIST LABORATORY LABORATORY

ASSISTANT TECHNICIANS

Figure 1.3 Organogram of the Organization

7
 CHAPTER TWO

2.0 WATER TREATMENT

2.1 Introduction to water treatment

Water treatment is any process that makes water more acceptable for a desired end-

use. The end use may be drinking, industrial water supply, irrigation or many other uses.

Andriamirando et al (2007). The goal of all water treatment process is to remove the existing

contaminants in the water, or reduce the concentration of such contaminants so the water

becomes fit for its desired end-use. The process involved in treating water for drinking

purposes may be solids separation using physical processes such as settling and filtration, and

chemical processes such as coagulation and disinfection. Similarly, biological processes such

as activated sludge or slow sand filtration.

Measures taken to ensure water quality do not only relate to the treatment of the

water, but to its conveyance and distribution after treatment. It is therefore common practice

to keep residual disinfectants in the treated water to kill bacteriological and chemical

contaminants during distribution. (Eaton and Franson, 2005)

2.2 Stages involved in water treatment process

2.2.1 Screening
This process involves the blockage of large particles such as log of woods, leaves,

debris and large aquatic animals being washed down into the dam from entering the pipe to

prevent blockage of the water channels and ease purification. This is done with the aid of a

device called Screen bar, which is placed at a junction just before the low lift pump. The low

lift pump is used to move surface water or raw water from the dam to the aerator.

8
2.2.2 Aeration
The water from the dam through a machine called Low lift pump enters the aerator

where aeration takes place. Aeration is the process of exposing the raw water to the

atmosphere so as to facilitate the removal of odour and the exposure of harmful micro-

organisms to the sunlight rays (UV rays).

What happens at the aerator?

The aerator exposes water from the dam to air in order to:

1. Remove odour

2. Absorb more oxygen into the water

3. Convert soluble particles to insoluble particles to aid flocculation i.e. soluble metals in

form of oxides will be converted to insoluble metals or chemical matters.

Note: As a result of penetration of oxygen when the water is exposed, redox reaction occurs.

About 88% of soluble metals would be converted to insoluble matter as a result of redox

reaction. Soluble Iron (II) would be oxidized to insoluble Iron (III) which forms insoluble

precipitates in water i.e. flocs on reaction with aluminum sulphate solution. Also, a magnet is

present in the aerator which separates any metallic object that comes with water from the

dam.

Aeration is the first stage in water treatment process. There are two types of aerator

used at ASEJIRE water supply scheme:

a. Spray-like aerator

b. Cascade aerator

9
Figure 2.1: Screen Bar

Figure 2.2: spray-like aerator

10
Figure 2.3: Cascade Aerator

2.2.3 Coagulation and Flocculation

Coagulation and flocculation occur in successive steps intended to overcome the

forces stabilizing the suspended particles, allowing particle collision and growth of flocs. If

step one is incomplete, the following step will be unsuccessful.

Coagulation

Coagulation is a process used to neutralize charges by addition of coagulants with

charges opposite to those of the suspended solids in water to form a gelatinous mass to trap

(or bridge) particles thus forming a mass large enough to settle or be trapped in the filter.

Mechanism behind coagulation

A coagulant (typically a metallic salt) e.g. alum with the opposite charge is added to

the water to overcome the repulsive charge and destabilize the suspension. The colloidal

particles are negatively charged and alum is added as a coagulant to create positively charged

ions. Once the repulsive charges have been neutralized (since opposite charges attract) the

van der waal’s force.

11
 Figure 2.4: Destabilized Colloids

Figure 2.5: Formation of Flocs

Flocculation

Flocculation is gentle stirring or agitation to encourage the particles thus formed to

agglomerate into masses large enough to settle or be filtered from solution. Flocculation, a

gentle mixing stage, increases the particle size from submicroscopic microflocs to visible

suspended particles. The microflocs are brought into contact with each other through the

12
process of slow mixing. Collisions of the microflocs particles cause them to bond to produce

larger, visible flocs called pinflocs. The flocs size continues to build through additional

collisions and interaction with inorganic polymers formed by the coagulant or with organic

polymers added which result in formation of macroflocs. Once the flocs have reached its

optimum size and strength, the water is ready for sedimentation. The collision is effected by

Van der Waal’s forces and Brownian motion.

Surface forces and Brownian’s motion is mainly sufficient effective for micro

particles and for larger particles energy input is demanded. For this, a gentle mixing (sheer

power by flash mixer) is used. The flocs formation is limited by the sheer power of the mixer,

insufficient sheer power shall not create enough collision energy, too much sheer power

likely to break the flocs apart again. Therefore, the energy input and the flocs’ size must be

carefully balanced. Flocculation therefore increases the size of flocs due to mechanical

mixing.

The aerated water mixes with alum at the flash mixing point which is also called the

flocculating chamber.

Coagulants

The choice of coagulant depends on the nature of the suspended solid to be removed,

the raw water conditions, the facility design, and the cost of the amount of chemical

necessary to produce the desired result. Final selection of the coagulant (or coagulants)

should be made following thorough jar testing and plant scale evaluation. Consideration must

be given to the required raw water quality, effect upon downstream treatment process

performance, cost, method and cost of sludge handling and disposal, and net overall cost at

the dose required for effective treatment.

Types of coagulants

Generally, coagulants are classified as:

13
 1. Inorganic coagulants Operators

2. Organic coagulants

Inorganic Coagulants

Inorganic coagulants include salts of aluminum and iron in form of their sulphates or

chlorides. They are both cost-effective and applicable for a broad variety of water and waste

water. Inorganic coagulants are particularly effective on raw water with low turbidity (TSS

concentration). Examples include aluminum sulphate Al2 (SO4)3.18H2O and ferric chloride

FeCl3.

When an inorganic coagulant is added to water containing a colloidal suspension, the

cationic metal ion from the coagulant neutralizes the negatively charged electric double layer

of the colloid. Much the same occurs with an organic coagulant, except the positive charge

most commonly comes from an amine (NH4+) group attached to the coagulant molecule.

Aluminum sulphate is used if the release of chloride ions by use of ferric chloride is

unwanted. It is in general much less corrosive in handling compared to ferric chloride, but

create less heavy flocs.

Ferric Chloride creates in general a more heavy flocs which allows larger velocity of

the process. It is used if the addition of sulphate ions, released to the water by use of

Aluminum sulphate is unwanted, as sulphates in high concentration may create a slightly

bitter taste to potable water.

The equation for the reaction of each coagulant in raw water is represented below

Alum:

Al2(SO4)3 + 3Ca(HCO3)2 ( 2Al(OH)3 + 3CaSO4 + 6CO2

Aluminium Calcium
bicarbonate Aluminium Calcium Carbon
sulphate
(already in the hydroxide sulphate dioxide
water)

Coagulant raw water flocs

14
Ferric Chloride:

2FeCl3 + 3Ca(HCO3)2 2Fe(OH)3 + 3CaCl2 + 6CO2

Ferric Calcium Ferric Calcium Carbon

Chloride bicarbonate Hydroxide Chloride Dioxide
Coagulant raw water flocs

Organic coagulants

Generally, organic coagulants are used when sludge generation is desired. The most

widely used class of organic coagulants is the Polyamine and PolyDADMAC. This coagulant

functions by charge neutralization alone so there is no advantage of the “sweep-floc”

mechanism. Polyamines will generally treat higher turbidity raw water (> 20 NTU)

effectively. PolyDADMACs are a specific class of polyamines that fit in this category.

Melamine Formaldehydes and Tannins are also all-organic polymers that act similarly to

inorganic coagulants in that they do not only coagulate the colloidal material in the water, but

also contribute their own precipitated floc as well.

2.2.4 Sedimentation
This is the second stage at the treatment plant where aggregate or coagulated particles

(flocs) settle due to gravity. This is the process of letting the flocs (suspended material) in the

flocculated water settle by gravity. Sedimentation is accomplished by decreasing the velocity

of the flocculated water as its flows into the sedimentation tank (clarifier) to a point below

which the particles will no longer remain in suspension. When the velocity no longer

supports the transport of the particles (flocs), gravity will remove them from the flow.

Coarse sludge particles get settled at the bottom with finer particles rising directly to the

surface where they have time to agglomerate and becoming larger; finally they settle at the

bottom part too. A set of channels (launders) is provided at the top of the

clarifiers/sedimentation tanks to collect the clarified (settled) water evenly and to prevent any

velocity irregularity in the various part of the sedimentation. The blanket gradually increases

15
in volume because of the impurities present in the water. The level of the blanket therefore

rises regularly and sludge must be extracted from the bottom part, which must be extracted at

the rate such that the quantity of suspended solids extracted corresponds to the quantity

entering the clarifier.

The unclean part of the water that contains the sediments is de-sludged periodically to

prevent eruption. Eruption is the movement of water from underneath to the surface of the

water which occurs when dislodging is not carried out and can result in waking the entire

water body unclean. De-sludging is a process which involves opening of the dislodging valve

through wheel and excavator to allow the sediments underneath the tank to escape through

holes.

The first step in the sedimentation tank is settlement by gravity to form sediments, while

decanting is the second step where the clean water (upper layer) passes through the minor

trough to the major trough and the major trough conveys it to from the clarifier to the next

stage of the treatment plant called filtration stage.

Figure 2.6: Sedimentation Tank

16
Figure 2.7: Sedimentation Tank After Complete De - Sludge

2.2.5 Filtration
After leaving the sedimentation tank (clarifier) via the clarified (settle) water launder

or decanting trough, the water flows by gravity to the filter beds. Here, the remaining very

fine particles are filtered by a sand medium which is generally referred to as a Slow Sand

Filter. Underneath the filter bed are nuzzled pipes which convey the final water by gravity

into the clear well. The filter bed is maintained by the act of backwashing. This is done when

the rate of filtration reduce due to the blockage of the sand media in the filter bed.

Backwashing is the back supply of air and clean water aimed at unclogging the sand pores in

the filter bed. It is done to remove the fine particles blocking the filtration of the settled

water. The compressor absorbs air from the atmosphere which then mixes with water from

the upwash or clarifier which moves and agitates the sand in the filter bed when released. The

agitation causes the sand particles to rub each other and this improves the pore spaces which

enables efficient filtration at production stage.

17
Figure 2.8: Filter bed during backwashing

Figure 2.9. Filter bed without backwashing

18
2.2.6 Liming
Liming is the addition of hydrated lime Ca(OH)2 to neutralize the effect of alum in

water thus raising the pH. It is done after the water leaves the filter bed and before it gets to

the clear well tank. Since alum is known to be a little bit acidic in nature, therefore addition

of alum lowers the pH of water. In order to normalize the pH, liming has to be done.

As slaked lime is added to a water, it will react with any carbon dioxide present as follows:

Ca(OH)2 + CO2 ( CaCO3 + H2O (Eq. 1)

Chemistry behind liming:

As lime in the form of lime water is added to raw water, the pH is raised and the

equilibrium of the carbonate species in the water is shifted. Dissolved carbon dioxide is

changed into bicarbonate ion (HCO3-) and then carbonate (CO32-). This action causes calcium

carbonate to precipitate due to exceeding the solubility product. In the process, both the

calcium in the raw water as well as the calcium added with the lime are precipitated. In lime

softening, there is a substantial reduction in total dissolved solids (TDS).

2.2.7 Disinfection / Post Chlorination

Disinfection takes place in the clear well where the final water is stored. The

importance of this is to:

a. Destroy any bacteria (germs) that may be present in the treated water, thereby

preventing their growth. The disinfectant used is chlorine. However, fluorine can

also be used but it should be properly controlled because it is highly hazardous.

Two reactions take place during chlorination;

(i) Hydrolysis: When chlorine is dissolved in water, chlorine converts to an

equilibrium mixture of chlorine, hypochlorous acid (HOCL) and

hydrochloric acid.

1. Cl2 + H2O HOCl + HCl

(ii) Ionization

19
 2. HOCl H+ + OCl- (Hypochlorite ion)

3. OCl- is the active ingredient for disinfection.

b. Prevent the reduction of sulphate in hard water to sulphide which produces taste

and odour.

2.3 Chemical Dosing

Prior to the production, flocculation test, a physical water analysis is always carried

out in the Quality control Laboratory to determine the quantity of chemicals that will be

sufficient to clarify a certain volume of water. The outcome or result of this test is used to

determine the dosage of the chemicals.

The chemicals involved are:

a. Aluminum sulphate Al2(SO4)3.18H2O (Alum) as coagulant

b. Slaked lime for pH correction.

c. Chlorine for disinfection

2.3.1 Aluminium Sulphate Dosing

Aluminum sulphate Al2(SO4)3.18H2O is a white crystal salt (hydrated salt) with

molecular weight of 666g/mol, meaning that the pure Alum content is 8.1% only. It is

delivered in bags weighing 50kg.

Theoretically, the amount of Alum solution required for coagulation depends on the

turbidity and colour of the treated water. Temperature below about 350F or above 700F may

increase the coagulant demand slightly because of a slower reaction or from re-absorption of

the flocs. The experimental work (called Flocculation analysis) from the quality control

laboratory always gives an indication of the approximate dosage required.

The Aluminum sulphate dosing reduces the pH of water.

The achieved flocs size is a function of the Alum dosing rate and the mixing power input. If

the dosage is too low, the created flocs will be too small and hard to settle, while too high

20
dosage creates too large flocs which likes break apart or if they settle creating a bottom heavy

sludge and will be very hard to remove from the sedimentation basin.

The dosage is expected to be between 25 – 30mg/L when the turbidity of raw water is low but

if higher the dosage must be altered accordingly as presented in table 2.1.

Figure 2.10: Flocculating Machine

Table 2.1: Alum Dosage

Raw water turbidity (NTU) Alum dosage (mg/l)

<50 25 - 30

<100 30 - 35

<150 35-40

<300 40 - 45

<400 45 - 50

<500 50 - 55

21
2.3.2 Lime Dosing
Hydrated lime Ca(OH)2 is a white-grey powdered substance with molecular weight of

74g/mol, meaning that the pure calcium content is 54% only. It is delivered in 50kg bags.

NB: Asejire Water Supply Scheme was designed for powdered hydrated lime Ca(OH)2 and

not for Kilned Lime CaO.

Lime dosing point is located at the inlet of the clear well for final pH correction. Lime

increases the pH due to the release of hydroxide group (OH-) during chemical dissociation as

shown in the chemical reaction below:

Ca(OH)2 Ca2+ + 2OH-

Normally, a lime dosage of up to 10mg/L is sufficient but depends on the Alum

dosage and the raw water chemical characteristics. The dosing pump is meant to be adjusted

manually till the desired pH is reached. The effect of the dosing is to be verified after 1 – 2

hours of production by checking the pH of clarified water.

The greater the dosage of Alum, the lower the pH and the higher the quantity of lime required

for pH correction. In a nut shell, the dosage is controlled by the pH range of the water.

2.3.3 Chlorine Dosing

The Scheme makes use of Chlorine gas as disinfectant. Chlorine is a greenish-yellow

gas with higher specific density compared to air. Chlorine is used to disinfect water due to its

high oxidizing potential, by oxidizing volatile organic matter, algae, bacteria, germs as well

as Ferric and Manganese (II) ions and ammonia.

22
 CHAPTER THREE

3.0 WATER QUALITY CONTROL UNIT

This chapter deals with the work done during my six months industrial work training

at WCOS. During my stay, I was attached to the quality control laboratory which I have

explained below giving detailed account of the work done in the laboratory.

3.1 Quality Assurance and Quality Control

Quality Assurance is the system that sets the policies, standard, methods and

specification for monitoring the quality of production, products and services.

Quality control (QC) which is a subset of QA is the day to day monitoring of production for

conformance to the standard and specification set under QA programme. In order to meet to

up to the standard set aside by Quality Assurance, some Standard Operating Procedure (SOP)

and Good Manufacturing Practice (GMP) must be strictly adhere to, however the standard is

called quality assurance standards.

3.2 Quality Control Laboratory

Quality control laboratory is the lab that handles the analysis of packaged water

samples. The tests that are carried out in the lab can be divided into four summarized below.

3.2.1 Physical Test

1. Odour

2. Taste

3. Appearance

4. Colour

3.2.2 Physico-Chemical Tests

1. Electrical Conductivity

2. Total dissolved solids

3. pH

23
 4. Total solids

5. Salinity

3.2.3 Chemical Tests

1. Total alkalinity

2. Chloride

3. Total hardness

4. Chlorine demand

5. Dissolved oxygen

6. Calcium Hardness

7. Magnesium Hardness

8. Iron

9. Silica

10. Calcium ion

11. Magnesium ion

12. Sulphate

3.2.4 Bacteriological Tests

1. Coliform organisms

2. Total colony count

3. E. coli

3.2.1 Physical Tests

Physical parameters are determined in water samples and they include clarity, taste,

odour, appearance and colour. Clarity test is done to ensure that the water does not have

particles. Taste, odour and appearance are to ensure that the water is colourless, odourless

and tasteless.

24
Colour Test

The colour of water depends on the dissolved particles in it. A colourless appearance

is one of the properties of potable water. The value ranges from 5 to 100. This test is always

carried out on raw water, during flocculation analysis and at every 30 minutes interval on

final water to ensure potable water supply.

Equipment: Lovibond Nessleriser, two test tubes and distilled water.

Procedure

Fill one of the test tube with distilled water and the other with the water sample. Insert the

two test tubes into the lovibond Nessleriser and view vertically through the hole on it and

compare the colour until the corresponding colour is achieved.

Read and record the corresponding value on the disc as the result.

Note: During comparison one might not find the colour that matches, in such cases, one need

to dilute the sample (this is called serial dilution), as thus;

Take one-tenth of the water sample and dissolve it in 100 mL of distilled water.

Repeat steps 1 and 2 respectively.

3.2.2 Physicochemical Tests

These are tests that are carried out with the use of equipment. pH meter or lovibond

comparator is used to determine the pH of the water sample. This is to have a range of 6.5-8.5

to be accepted as safe for consumption. TDS/Conductivity/Salinity meter is used to determine

the total dissolved solid, conductivity and salinity of the water sample.

Determination of the Turbidity of Water Sample

Turbidity is an expression of optical property wherein light is scattered by suspended

particles present in the water sample (Tyndall effect) and is measured using a nephelometer

or a turbidimeter. It is measure in NTU: Nephelometric Turbidity unit. Suspended solids such

as clay, silt, finely divided organic and inorganic matter and other microscopic organisms

25
cause turbidity in water. Turbidity affects light scattering, absorption properties and aesthetic

appearance in a water body. Increase in intensity of scattered light results in higher values of

turbidity. It is the amount of light transmittable suspended solids present in the water.

Turbidity for potable water is supposed to be greater than or equal to 0.1.

Aim: to determine the turbidity of a water sample

Principle: Nephelometric measurement is based on the comparison of the intensity of

scattered light of the sample with the intensity of light scattered by a standard reference

suspension (formazin polymer) under similar conditions.

Apparatus/Reagents: Nephelometer, sample cells, distilled water, stock primary formazin

suspension.

Procedure:

Switch on the turbidimeter (at least 30 minutes before the test)

Calibrate the turbidimeter using formazin suspension of 400NTU

Calibrate the turbidimeter to 0 NTU using distilled water.

Shake the sample cell thoroughly and insert into the turbidimeter.

Record the value on displayed by the turbidimeter.

Determination of the pH of Water Sample

This is a measure of alkalinity or acidity of water. It ranges from 0 to 14. The pH

scales measures the logarithmic concentration of hydrogen (H+) and hydroxide (OH-) ions

present in water. If a pH less than 6.5 is confirmed in the water, the water may be corrosive.

If a pH greater than 8.5 is confirmed in the well water, it may pose serious health problems

like eye and mucous irritation. Although a pH less than 6.5 does not pose serious health risks,

it may contribute to the corrosion of plumbing materials and the release of metals into the

water, such as lead, cadmium, zinc, or copper. The presence of such metals in drinking water

26
may pose health risks which are linked to a number of neurological and reproductive

problems.

This test is carried daily; once on raw water, during flocculation analysis and every 30

minutes interval on final water during production.

Aim: To determine the pH of a water sample.

Apparatus/Reagents

Lovibond comparator, phenol red solution/bromothymol blue solution, lovibond disk,

dropper, cuvette.

Procedure

Measure 10 mL of water sample into the cuvette.

Add 10 drops of bromothymol blue or phenol red as indicator and invert to mix.

Erect the cuvette containing the solution into the right hand side of the Lovibond comparator

Place the cuvette containing sample water on the right hand side of the lovibond.

Compare the colour of the solution with the standards on the lovibond disc by rotating the

disc until the colour matches. The value on the lovibond disc when the colour matches is the

pH of the sample.

3.2.3 Chemical Tests

All of these tests are carried out using titration method. These tests are:

Determination of Total Hardness in Water

Hardness is caused by compounds of calcium and magnesium, and by a variety of

other metals. Hardness is expressed in terms of calcium carbonate (CaC03). Water within 0–

60 mg/L is considered soft, 60-120 mg/l moderately hard, 60-120mg/l is moderately hard and

above 180mg/L is very hard water. The total hardness is defined as the sum of calcium and

magnesium concentrations both expressed as CaCO3 in mg/L. Carbonates and bicarbonates

27
of calcium and magnesium cause temporary hardness. Sulphates and chlorides cause

permanent hardness.

Aim: To determine the total hardness of drinking water samples

Procedure:

Measure 50ml of the water sample into a 100ml conical flask

Add 2ml of ammonia buffer

Add a pinch of Erichrome Black T indicator. A purple colour develops in the presence of Ca+

and Mg+.

Titrate with 0.02N EDTA till last tinge of purple colour disappears to give the end point, that

is, a light blue colour.

Record titre value as TV

Calculation: Amount of acid used x (Normality of acid used (eq/L) x 50,000 (Mg

CaCO3/eq) / Volume of water sample taken). This is simplified to give: Volume of acid used

x 20

EQUATION OF REACTION

Ca2+ + EDTA4 CaEDTA2-

Mg2+ + EDTA4 MgEDTA2-

Limit: The hardness of good quality drinking water should be between the ranges of 50-

150mg/L measured as calcium carbonate.

Determination of Calcium Hardness

The presence of calcium (fifth most abundant element) in water results from the passage of

water through or over deposits of limestone, dolomite, Gypsum and such other calcium

bearing rocks. It is measured by EDTA titrimetric method. Small concentration of calcium

prevents corrosion of metal pipes by laying down a protective coating. But increased amount

of calcium precipitates on heating to form harmful scales in boilers, pipes and utensils.

28
Aim: To determine the calcium hardness of drinking water samples

Apparatus/Reagents: 50ml burette, 100ml measuring cylinder, conical flask, beakers,

droppers, NaOH solution, murexide indicator (ammonium purpurate), standard EDTA titrant

0.02N.

Procedure:

Measure 50ml of water sample into a conical flask

Add 2ml of NaOH solution to standardize and regulate the pH of the water sample.

Add a pinch of murexide as indicator.

Titrate with 0.02N EDTA until the pink colour changes from pink to purple.

Record titre value as TV

Calculation: Volume of EDTA used x 20 gives the calcium hardness of the water sample.

Determination of Magnesium Hardness

Magnesium is found in all natural water and its source lies in rocks, generally present

in lower concentration than calcium. It is also an important element contributing to hardness

and a necessary constituent of chlorophyll. Its concentration greater than 125mg/L can

influence cathartic and diuretic actions.

Aim: To determine the magnesium hardness of a water sample

Principle: Magnesium hardness can be calculated from the determined total hardness and

calcium hardness.

Determination of Total Alkalinity in Water

Total alkalinity value is obtained by the summation of the methyl orange alkalinity

and the phenolphthalein alkalinity.

Aim: To determine the total alkalinity of a water sample

Apparatus: 50ml burette, 100ml measuring cylinder, conical flask, 0.02N H2SO4 solution,

methyl orange indicator, sodium thiosulphate solution.

29
Procedure:

Measure 50ml of the water sample into a conical flask

Add 2-3 drops of sodium thiosulphate to regulate or isolate the chloride ion in the water.

Add 2 drops of methyl orange as indicator to give the initial colour

Titrate with 0.02N H2SO4 to endpoint when colour changes from yellow to orange

Record the titre value

Calculation: The volume of acid used x 20 gives the total alkalinity of the water sample.

Determination of Chloride

When chloride ions are present in drinking water, that is, in high concentration, they

make the water salty. These chloride ions get into water when salt deposits dissolve.

Aim: To determine the amount of chloride ions present in packaged drinking water samples

Apparatus: 50ml burette, 100ml measuring cylinder, conical flask, 0.1N AgNO3 solution,

0.5N Potassium chromate solution

Procedure:

Measure 100ml of the water sample a conical flask.

Add 2ml of K2Cr2O4 to it

Titrate against 0.1N AgNO3 solution until a perceptible brick red colour appears

Record titre value

Calculation: Volume of AgNO3 used x 5 gives the value of the chloride in mg/L

Limit: 250mg/L maximum

Determination of Dissolved Oxygen in Water

Aim: To determine the amount of dissolved oxygen in sample of water

Principle: Oxygen present in the sample oxidizes the dispersed divalent manganese

hydroxide to the higher valency to precipitate as a brown hydrated oxide after addition of

potassium iodide. Upon acidification, manganese reverts to its divalent state and liberates

30
iodine from potassium iodide, equivalent to the original dissolved oxygen content of the

sample. The liberated iodine is titrated against 0.025N sodium thiosulphate.

Apparatus/Reagents: Vitro bottles, measuring cylinder, conical flask, beaker, dropper,

manganese sulphate, alkali iodide, concentrated H2SO4, standard sodium thiosulphate

(0.025N)

Procedure:

Fill the vitro bottle to the brim with the sample water. Ensure there is no bubble in the vitro

bottle.

Add 2ml of manganese sulphate, cork and shake.

Add 2ml of alkali iodide, cork and shake,

Add 2ml of concentrated H2SO4 solution, cork and shake again

Measure 200ml out of the solution into a conical flask.

Titrate against 0.025N sodium thiosulphate from brown to colourless.

Calculation: The volume of the sodium thiosulphate used gives the amount of dissolved

oxygen in mg/L

Determination of Chlorine Demand of Water Sample

Chlorine demand is the difference between total chlorine added in the water and

residual chlorine after a given contact time. It is the amount which reacts with the substances

in water, leaving behind an inactive form of chlorine. Chlorine demand may change with

dosage, time, temperature, pH and nature and amount of impurities in the water. Chlorine

demand is caused by a complex set of reactions. Chlorine reacts with dissolved or suspended

organic materials in the water to form stable chlorinated organic compounds (e.g.

trihalomethanes, halo acetic acids or other chlorinated organic compounds). Some of these

compounds (trihalomethanes) are referred to as disinfection by-product (DBPs). Other

chlorinated organics contribute to taste and odour problems. As a rule, the lower the chlorine

31
demand, the lower the amount of DBPs formed and less taste and odour problem occurs.

Chlorine is also reduced by inorganic reductants contained in the water e.g. ferrous,

manganous, nitrite and sulfite ions. The ammonia present in the water consumes chlorine to

form chloramines.

Aim: To determine the chlorine demand of a water sample.

Apparatus/Reagents: 3 amber bottles, pipette, measuring cylinder, Milton solution.

Procedure

Measure 200 mL of the sample water into three amber bottles.

Pipette 1.2, 1.4 or 0.6 of Milton solution into each amber bottle and shake. Note the dosing

might differs if the sample water contains many bacteria.

Leave the solution to stand for about 30 minute. This is the contact time required.

Check the residual after the 30 minutes.

Fill the lovibond comparator cuvette to the mark with the water sample.

Add 8 drops of orthotoludene as indicator into the water sample.

The residual value of chlorine on the lovibond disk is used to calculate the chlorine demand.

Calculation

Chlorine demand = (A x B) – C

A= Value of the Milton solution dispensed

B= Concentration of the Milton solution

C= Value of the chlorine residual

Determination of Sulphate in Water

Sulphate is found appreciably in all natural waters, particularly those with high salt

content. Besides industrial pollution and domestic sewage, biological oxidation of reduced

sulphur species also adds to sulphate content. Soluble in water, it imparts hardness with other

32
cations. Sulphate causes scaling in industrial water supply, and odour and corrosion problems

due to its reaction with hydrogen sulphide.

Aim: To determine the amount of sulphate in water sample

Apparatus/Reagent: Sulphate test kit

Procedure:

Measure 20ml of the water sample into the sulphate tube (engraved with a line underneath)

Add 8 drops of sulfat 1 to the sample water.

Add a level filled sulfat 2 using micro spatula

Presence of sulphate turns the solution milky.

Visibility of the line underneath from top view indicates that sulphate is less than 35.

Determination of Silica in Water

Aim: To determine the amount of silica in water

Apparatus/Reagent: beaker, measuring cylinder, (1+1) HCl solution, Ammonium

molybdate (NH4)2MoO4, Oxalic acid (C2H2O4)

Procedure:

Measure 50ml of the sample water into the beaker.

Add 1ml of (1+1) HCl and shake slightly.

Add 1.5ml of ammonium molybdate

Add 2ml of oxalic acid. A colour change is observed.

Compare the colour with series of prepared Silica standards in different mg/L

The value is recorded in mg/L

33
Figure 3.1: Prepared Standards For Silica Test

3.2.4 Bacteriological Analysis

Pathogenic microorganisms likely to cause waterborne diseases are mainly

categorized as bacteria, viruses and protozoa and those most commonly concerning water

supplies have been listed by the World Health Organization.

Microbiological examination of potable water requires the isolation and enumeration of

organisms that indicate the presence of faecal Contamination. In some circumstances, the

same indicator organisms may also be used to assess the efficiency of potable water treatment

plants, which is an important element of Water Quality Control. Other Microbiological

indicators, not necessarily associated with faecal contamination/pollution, are also used for

this purpose.

Bacteria that are typically transmitted by the faecal-oral route include pathogenic

Esherichia coli, Campylobacter sp, Salmonella sp, Shigella sp, Vibrio cholerae and Yersinia

enterocolitica.
34
 Escherichia coli are abundant in human and animal faeces; in fresh faeces it may

attain concentrations of 109 per gram. It is found in sewage, treated effluents, and in all

natural waters and soils subject to recent faecal contamination, whether from humans, wild

animals, or agricultural activity. Recently, it has been suggested that E. coli may be present or

even multiply in tropical waters not subject to human faecal pollution.

Thermotolerant coliform bacteria are the coliform organisms that are able to ferment

lactose at 44–45°C; the group includes the genus Escherichia and some species of Klebsiella,

Enterobacter, and Citrobacter. Thermotolerant coliforms other than E. coli may also originate

from organically enriched water such as industrial effluents or from decaying plant materials

and soils. For this reason, the term “faecal” coliforms (although frequently employed) is not

correct, and its use should be stopped.

Note: Because thermotolerant coliform organisms are readily detected, they have an

important secondary role as indicators of the efficiency of water-treatment processes in

removing faecal bacteria. They may therefore be used in assessing the degree of treatment

necessary for waters of different quality and for defining performance targets for removal of

bacteria.

Coliform Organisms and Total Colony Count

Coliforms are rod-shaped. Gram-negative non-spore forming and motile or non-

motile bacteria which can ferment lactose with the production of acid and gas when incubated

at 35-370C in a lactose broth for 24-48 hours.

They have long been recognized as a suitable microbial indicator of drinking-water

quality. They are easy to culture, and their presence is used to indicate that other pathogenic

organisms of faecal origin may be present. Coliform procedures are performed in aerobic or

anaerobic conditions.

Enumeration of Faecal Coliform/Enteric Bacteria in Treated Water to ensure its quality

35
Aim: To enumerate the faecal coliform/enteric bacteria in treated water.

Apparatus/Reagents: Bucket autoclave, hot-air oven, pipette, Bunsen burner, methylated

spirit, cotton wool, aluminum foil, sodium thiosulphate, petri dishes, conical flasks, test

tubes, test tube rack, Durham’s tubes, MacConkey Broth, Nutrient agar, incubator, fume

cupboard, colony counter.

Procedure:

Label three conical flasks as raw, settled and final.

Sterilize adopting the moist-heat method at 1100C for 15 minutes in a bucket autoclave.

Wash and sterilize the workbench and incubator using detergent and methylated spirit

respectively.

Add 1 ml of sodium thiosulphate to the 3 sample flasks before collecting the water samples to

neutralize the effect of chlorine on the microorganisms and also to prevent growth of fungi so

that the enteric bacteria are easily observed.

Wrap the pipettes with foil paper and sterilize adopting the dry-heat method at 1210C for 1hr

30mins in a hot air oven.

Measure the culture media, Nutrient Agar and MacConkey broth in the conical flasks and

label the petridishes according to their source. (e.g. raw, settled and final)

Sterilize the already prepared media and petridishes adopting the moist-heat method in a

bucket autoclave at 1100C for 15 minutes.

Measure 8ml of MacConkey broth into well stoppered test tubes with inverted Durham tubes

aseptically before re-sterilization which would last for 20 minutes.

Inoculation is done in aseptic condition using the pour-plate method by inoculating 1ml of

water sample into the re-sterilized test tubes with the Durham tubes vertically inverted.

Measure 1ml of the sample water into three sterilized petridishes and pour the nutrient agar

aseptically into the plates and swirl gently until it is uniformly mixed with water samples.

36
Pipette 1ml of the medium into petridish containing 10 ml of distilled water and allow to

serve as control experiment.

Allow the nutrient to solidify in the petridish and seal the test tubes with aluminum foil and

carefully arrange in the test tube rack.

Transfer the test tube rack and invert the petridishes into the incubator set at 370C and leave

for 24 to 48 hours to observe microbial growth.

Observation: growth in the medium is confirmed by visible turbidity, and/or a colour

change, in the case of MacConkey Broth, the colour changes from red into yellow. And gas

production is detected in the inverted Durham tubes. The colonies observed on the plates are

counted using the membrane colony counter.

Conclusion: Plates and test tubes were observed after 48 hours of incubation. T.V.C (Total

Viable Count) was within permissible limit 0-10 CFU (Colony Forming Units) and there was

no presence of coliform. Asejire water supply is potable and safe for consumption.

Note: TVC represents the number of colony forming units per gram (or per ml) of the sample.

A high TVC is usually attributable to poor quality.

Figure 3.2: Sterilized Nutrient Agar And Macconkey Broth

37
Figure 3.3: Prepared Media Set For Incubation

Figure 3.4: Bucket Autoclave for Moist-Heat Sterilization

38
3.3 Atomic Absorption Spectrophotometer (AAS)
Metals that can be detected by the AAS:

Aluminum (Al), Lithium (Li), Antimony (Sb), Magnesium (Mg), Arsenic (As), Manganese

(Mn), Beryllium (Be) Mercury (Hg), Barium (Ba), Molybdenum (Mo), Calcium (Ca), Nickel

(Ni), Chromium (Cr), Niobium (Nb), Cadmium (Cd), Ruthenium (Ru), Cobalt (Co), Tin

(Sn),Copper (Co), Tungsten (W), Gallium (Ga), Vanadium (V), Hafnium (Hf), Zinc

(Zn),Indium (In), Zirconium (Zr), Iron (Fe) Lead (Pb)

3.3.1 Sample Preparation

Before a sample can be analyzed by the AAS, there are some steps to make it

analyzable by the instrument. There are three main steps involved in the preparation of

samples:

1. Weighing

The sample is first homogenized to get a representative of the bulk sample. About 2-

5g of the sample is taken into a labelled and tarred crucible. The weight is taken by an

analytical balance

2. Ashing

involves burning the organic component of the sample to leave only the inorganic

part which contains the metals which need to be analysed. Ashing is also done to break open

the matrix of the complicated structure of the sample, thereby, releasing the metals for

analysis.

The ashing of samples is done in two stages. Before the sample is placed in the

furnace to completely ash, pre-ashing is done. Pre-ashing is done before the main ashing in

the furnace. It is done to prevent excessive smoking in the furnace, prevent self-

contamination of samples and reduce the time it takes for the sample to completely ash. The

crucible containing the weighed sample is placed on a hot plate or a heating mantle. The hot

plate should be placed in a fume cupboard so as to trap the fumes emitted. The sample is pre-

39
ashed at a temperature of 100-2300C. When the samples stop fuming, they are transferred

using the desiccator to the furnace. The furnace used for complete ashing of samples is the

Carbolite furnace which operates at a temperature of 500-5500C. The samples are left in the

furnace for a minimum of 24hrs. For samples that are not yet ashed after 24hrs, few drops of

HNO3 are added to hasten ashing.

Liquid samples are treated a bit different. Before (pre-) ashing is done, the liquid part of the

sample is allowed to evaporate by placing the weighed sample on the water bath so it remains

only the solid part.

3. Making Up

The solvent used to make up samples is 1% HNO3. It is prepared by adding 1% of

concentrated HNO3 to 99% of deionized water. For example, in a 2000mL volumetric flask,

20mL of concentrated HNO3 is added to 1980mL of deionized water. The water used is

deionized to prevent interference and wrong results.

When the samples have completely ashed in their labelled crucible, they are made up into

100mL volumetric flask with the 1% HNO3. This is done by soaking the remaining residue

left after ashing with the solvent and pouring it into the standard flask.

HNO3 is used as a solvent because it helps to ionize the atoms readily in the solution and also

has a wide range of solubility.

The sample solution is then filtered into sample bottles so as to remove the particles which

could block the aspirator of the AAS.

The sample solutions are transferred into vials on the auto sampler for analysis.

3.3.2 Components of the Spectrophotometer

The most important components of the AAS instrument are listed below:

AUTO SAMPLER: This is the part of the instrument where the prepared samples are

introduced manually.

40
NEBULIZER: The nebulizer sucks the sample via the aspirator from the auto sampler. It

converts it to an aerosol by mixing it with gas and then pumps it to the flame to be ionised.

HOLLOW CATHODE LAMP: This is a cylindrical metal cathode, filled with argon or neon

gas at low pressure, containing the specific element to be analysed and an anode. This emits

the radiation of the element of interest when a high voltage is applied across the anode and

the cathode.

DEUTERIUM LAMP: It works with the Hollowed cathode lamp to help correct background

errors and bring out the wavelength of the analyte.

ATOMIZER: This atomizes the sample in solution. Here the flame atomizers uses two

different type of flames which are the Air-Acetylene flame with temperature about 2300⁰C

and Nitrous oxide-Acetylene flame with temperature of about 2700⁰C.

DETECTOR: It detects the analyte. The Photo multiplier tubes (PMT) are the most

frequently used detectors in AAS. This decodes the information from the Hollowed cathode

lamp and converts it to its absorbance and concentration.

Figure 3.5: Atomic Absorption Spectrophotometer

41
3.4 Preparation of some Reagents used in the Laboratory

3.4.1 Preparation of Ammonia Buffer

Ammonia buffer used in the laboratory to regulate the pH of the water sample during

the test for hardness is as thus:

 15.9g of NH4Cl is dissolved in 143ml of NH3 solution to make solution A.

 1.79g of sodium EDTA salt (Na2C10O8N2H14.2H2O) mixed with 0.78g of MgSO4

is dissolved in 100ml of distilled water to make solution B.

 Solution A and B is placed in 250ml volumetric flask and filled to the mark with

distilled water.

 The 250ml solution is then placed in reagent bottle and used as buffer for pH

regulation.

3.4.2 Preparation of Erichrome Black-T Indicator

Erichrome black T is used as indicator during titration when carrying out total

hardness test.

Reagents and Apparatus

Electronic weighing balance, weighing pan, spatula, mortar and pestle, NaCl salt, conc.

Erichrome black T

Procedure:

 Switch on the weighing balance, keep the weighing pan (Petri dish) on it and set the

reading to zero

 Weigh 50g of NaCl into a crucible (A)

 Weigh 0.5g of conc. Erichrome black T (B)

 Crush A and B together thoroughly and transfer it into a clean reagent bottle for use.

42
3.4.3 Preparation of Murexide Indicator
Murexide is an indicator used during titration when carrying out calcium hardness

test. It is a solid mixture of conc. murexide and NaCl in ratio 0.1 to 50

Apparatus and Reagents

Weighing balance, mortar and pestle, murexide, NaCl

Procedure:

 Switch the electrical weighing balance on.

 Weigh 0.1 g of conc. murexide (reddish-brown) into a clean crucible

 Weigh 50 g of NaCl salt and add to the murexide in the crucible

 Grind with pestle till it turns powdery (yellowish-brown) then transfer the content into

a bottle for use.

3.4.4 Preparation Of 1% Aluminium Sulphate (Alum) Solution

This reagent is use as a coagulant during flocculation analysis.

Apparatus and Reagents

Weighing balance, weighing pan (Petri dish), mortar and pestle, distilled water and

Aluminum sulphate crystal

Procedure:

 Grind the Alum crystal into powder using mortar and pestle

 Switch on the weighing balance keeping the petridish on it and calibrate it to zero

 Measure 10 g of Alum powder into a beaker and carefully transfer into a 1000ml

standard flask.

 Add 1000 mL of distilled water to the alum powder to make up to mark.

NB. This simply means the ratio of alum to distilled water is 1:100

3.4.5 Preparation of Bromothymol Blue Indicator

Bromothymol blue is an indicator used in the checking the pH of sample water.

43
Apparatus and reagent used: Weighing balance, Petri dish, mortar and pestle, 0.05 N NaOH,

bromothymol blue, pipette and 500ml standard flask.

Procedure:

 Weigh 0.2g of bromothymol blue powder using the electrical weighing balance.

 Prepare 0.05N solution of Sodium hydroxide (NaOH)

 Pipette 6.4ml of 0.05N NaOH into the petridish containing the measured

bromothymol blue powder.

 Transfer the content and the washings into a 500ml standard flask,

 Make it up to mark in the standard flask using distilled water.

3.4.6 Preparation of Phenol Red Indicator

Phenol red is an indicator used in the checking the pH of sample water.

Apparatus and Reagents Used

Electrical weighing balance, Petri dish, 0.05 N NaOH, phenol red, beaker, distilled water,

pipette, and 500ml standard flask.

Procedure:

 Measure 0.1g of phenol red powder using the electrical weighing balance.

 Dissolve the phenol red powder with 5.7ml of 0.05N NaOH.

 Transfer the washings and content into the standard flask and make it up to 500ml

using distilled water.

3.4.7 Preparation of Methyl Orange Indicator

Methyl orange is an indicator used during titration when carrying out test for total

alkalinity

Apparatus and Reagents

Weighing balance, Petri dish, distilled water, methyl orange, 1000ml standard flask.

Procedure:

44
  Measure 0.5g of methyl orange into a petridish using the electrical weighing balance.

 Dissolve 0.5g of methyl orange with distilled water.

 Transfer the contents and the washings into a 1000ml standard flask and make up to

mark.

3.4.8 Preparation and Potency Test of High Test Hypochlorite (HTH)

HTH is used in the laboratory for disinfection of water sample. The potency i.e. the

Normality and Molarity must be known after preparation for calculation purposes.

Preparation and potency test of HTH goes thus:

 3.5g of powdered chlorine [Ca(OCl)2] was dissolved in 500ml of distilled water with

thorough mixing to ensure homogenous solution. The homogenous solution achieved

is HTH.

 A pinch of potassium iodide (KI) was added to 25ml of the HTH solution.

 2ml of glacial acetic acid was then added to give yellowish brown colouration.

 It was then titrated with 0.025N sodiumthiosulphate to colourless.

 The molarity and normality (i.e. potency) of the HTH was then determined using

formula.

 Calculate using normality of the solution x titre value x mass of chlorine.

3.4.9 Preparation of Agno3 for Argentiometric Titration

The silver nitrate solution used as the titrant in argentiometric titration geared towards

the determination of Chloride in sample water is prepared as thus:

 2.396g of AgNO3 salt is accurately weighed and placed in 1000ml volumetric flask.

 The content is made to the mark with distilled water.

 The solution is mixed well to get homogenous solution.

 The solution is then stored or kept in amber bottle to avoid decomposition by sunlight.

45
3.5 Lime Analysis
This analysis is carried out to check how efficient the lime used in boosting the pH of

the water is.

Procedure:

 Measure 0.5g of lime sample into a petridish using electrical weighing balance.

 Measure 17g of sugar granules on a petridish.

 Prepare 0.1782N solution of HCl from stock solution.

 Dissolve 0.5 g of lime in 20 mL of carbon dioxide free water and transfer the

washings into a corked conical flask.

 Boil the solution on the hot plate for 5 minutes

 To the solution add 17 g of sugar granules and 150ml of carbon dioxide free water.

 Mix the solution for 5minutes to ensure homogeneity.

 Leave the solution for 30 minutes

 Add 3 drops of phenolphthalein indicator.

 Titrate the solution with 0.178N HCl until the solution turns to colourless.

 The titre value equals the percentage of the CaO present in the lime.

NB. 1 mL of titrant =1% of CaO.

The addition of the sugar removes the water molecule. The expected value is from 74% -

75%. Also CaO quickly absorb the CO2, therefore during production proper storage must be

ensured. The reduction in the percentage of CaO is always as a result of long storage.

3.6 Alum Analysis

3.6.1 Title: Insoluble matter

Aim: To determine the percentage soluble and insoluble content of the alum

Procedure:

 Measure 10g of grounded alum

46
  Mix with 10ml of 1N H2SO4

 Add 100ml of water and stir and warm slightly

 Filter through filter paper or glass wool

 Wash residue once with hot water which is slightly acidulated with 1N H2SO4 then

with hot water until it is free from soluble compounds air dry to contact mass inside

oven at 1050c

Calculation

Insoluble matter =100 × m1/m

M1 – mass of residual after drying

M – mass of alum taken (10g)

3.6.2 Title: Soluble iron compound

Aim: To determine the soluble iron compound percentage by mass

Procedure:

 Measure 10g of grounded alum and add 50ml of distilled water

 Filter the solution

 Add 20ml of concentrated Hcl into the filtrate and heat to boiling

 Add stannous Cl solution until yellow colour disappear

 Cool the solution

 Add rapidly 10ml of mercuric chloride solution and stir until white precipitate of

mercurious chlorine is formed slowly

 Allow to stand for 5 minute

 Add 5ml of concentrated H2PO4

 Dilute to 250ml with distil water

 Add 5 drops of diphenylamine indicator and titrate with standard potassium chromate

solution till colour changes to deep blue

47
Calculation

Soluble Fe compound percentage by mass = 5.584 × VN/M

V – titre value

N – normalty of K2Cr2O7

M – mass of sample alum weighed

3.6.3 Title: Content of alumina

Aim: To determine the percentage of the active ingredient which is alumina

Procedure:

 Weigh 1.0g of alum sample into 400ml capacity beaker and dilute with 100ml distil

water

 Filter to remove undissolved matter and wash filter properly

 Add 5g of NH4Cl and stir to dissolve

 Add 2ml of concentrated HCl and 4 drops of nitric acud and boil gently for few

minutes in order to oxidize Fe

 Add dilute NH4OH/ 1+1 NH3 drop by drop until it smells faintly of ammonia and

yellow appearance on addition of 2 drops of methyl red indicator

 Filter immediately through filter paper, use hot washing solution NH4Cl to wash all

the residue to the top or apex of the filter paper

 Dry the residue which is the ammonia galantine form in a furnace or oven in a

platinium crucible at 10000c – 12000c (if in furnace)

 Cool the crucible together with the content in the desiccator

 Weigh and record it W1

 De-content the crucible and weigh again as W2

Calculations

 Weight of alumina = W1- W2

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  Percentage of alumina = 100 × M1/M – 1.4297A

M1 – mass of residue ignited

M – mass of sample taken

A – percentage of mass by soluble Fe compounds as Fe already determined

 Percentage aluminium to alumina (Al2O3) =soluble Fe compounds as Fe × 0.5291

3.7 WHO Standard for potable water

The WHO standard for physiochemical properties of potable water is presented on table 3.1

Table 3.1: physiochemical properties of potable water

Parameters WHO Technique used Source of Potential health effect

guideline occurrence

value

Colour (Hu) 5 - 20 Visual/ colour kit Due to presence

of dissolved salt

Turbidity (NTU) 5 Soil runoff High level of turbidity

is associated with

diseases causing

bacteria

Taste and odour inoffensive Psychological sense Due to

biological

degradation

49
Appearance Clear

without

particle

Potential 6.5 -8.5 pH meter /lovibond pH is changed Affects mucous

hydrogen comparator due to different membrane; bitter

dissolved gases taste; corrosion

and solids

Total alkalinity 50 – 150 Titrimetric Due to dissolved Embrittlement of

mg/l gases CO2 boiler steel. Boiled

rice turns yellow

Total hardness 50 - 150 Complexometric Presence of Poor lathering with

mg/l as CaCO3 titration calcium and soap; deterioration of

magnesium ion the quality of clothes;

scale forming

Total solids 2000

mg/l

Total dissolved 500 Presence of all Undesirable taste;

solids mg/l dissolved salts gastrointestinal

irritation; corrosion or

incrustation

Total suspended 500

solids mg/l

Nitrate as NO3 50 UV-visible Runoff from Shortness of breathe

mg/l spectrophotometer fertilizers used; and blue – baby

leakage from syndrome in infacts

50
 septic tanks; below the age of six

sewage months

Dissolved 4 - 19 Due to presence Dissolved oxygen

oxygen mg/l of dissolved corrodes water line,

oxygen boilers and heat

exchangers. At low

level marine animals

cannot survive

Conductivity 1000 High conductivity

Ns/cm increases the corrosive

nature of water

Chloride as Cl- 250 Argentiometric Eye/ nose irritation;

mg/l titration stomach discomfort

BOD mg/l <50 Incubation followed Organic material High BOD decreases

by titration contamination in level of dissolved

water oxygen

COD mg/l <250 COD digester

51
The WHO standard for bacteriological properties of potable water is presented on table 3.2

Table 3.2: bacteriological properties of potable water

Parameters WHO guideline value

Total colony count (MPN/100ml) 10

Coliform organism (MPN/100ml) 0

E-coli organism (MPN/100ml) 0

52
 CHAPTER FOUR

4.0 RECOMMENDATION AND CONCLUSION

4.1 Recommendation
The SIWES unit together with the relevant departments should make tangible efforts

to liaise with relevant industries, companies, and organisations to alleviate the difficulties

often faced by the students in securing a placement for the industrial training

Employers should also be encouraged to pay stipends to I.T students to increase their

enthusiasm and motivation for work.

The university officials should visit students often in order to know their challenges

and success

4.2 Conclusion
The Students Industrial Work Experience scheme (SIWES) has bridged the gap

between academic theory and practical and has built a good degree of confidence especially

in me. It has also given me a first-hand experience of the quality control analysis of water, the

privilege to build interpersonal relationship with staffs and colleagues, ability to work as a

team, ability to work both under and under no supervision. Similarly, it has been an eye

opener to the importance of Chemistry nationwide and its status in the society. I can

confidently say that the experience gained from this training is worthwhile.

53
 REFERENCES
Andriamirando, L., Asensi, D., Ballard, T., Bele, P., Bernard, M., Brunet, J., and

Cachot,L., (2007).water treatment handbook 1 (7th ed.).

Rueil-Malmaison, France: Deremont. Pg 120.

Eaton,D., Franson, H., (2005). Standard methods for the examination of water

and wastewater (21 ed). American Public Health association

ISBN 978-0-87553-00047-5. Pp. 45, 56.

Judith, N., (2014). - Evaluation of Student Industrial Work Experience Scheme

(SIWES) in Library School: The Federal Polytechnic

Nekede Experience

Onwuji, J. (2004). The Role of Industrial Placement Centre (IPC)

in the training of our Graduands.

Fedponek News, 1(4):30-31.

WHO (2004) Guidelines for drinking water quality,

3rd ed., WHO, Geneva.

www.gov.ns.ca/nse/water/

www.oyostate.gov.ng/ministries_departments_and_agencies/department_and_agencies/the_

water_corporation_of_oyo_state

www.who.int/water_sanitation_health/hygiene/emergencies/fs2_13.pdf

54