CEE307

Water Supply Engineering Lab

ISO 9001:2008 CEE208- Rev. # 01 Date: Feb 2021

Department of Civil Engineering

Lab Manual

For

Water Supply Engineering Lab

Name Signature
Muhammad Umar Mahmood
Prepared by:

Reviewed by: Engr. Tauqeer Akhtar

Approved by: Dr. Sadam Hussain

 COURSE NAME: Water Supply Engineering CR: 0-1
COURSE CODE: CEE 307

REFERENCE MATERIAL:

1. Water supply Engineering by S. K. Garg

2. Elements of Water supply and waste water disposal by Fair and Geyer
3. Environmental Engineering by Peavey. H.S. RR & George. T.

PROGRAM LEARNING OUTCOMES:

The course is designed so that students will achieve the following PLOs:
● PLO-07: Environment and Sustainability

COURSE LEARNING OUTCOMES:

● CLO-3: Perform & Demonstrate various parameters to check the water qualities. (P4-
Mechanism) (PLO-07)
● CLO-4: Accumulate lab reports and present them in an effective/organized way. (A3-Valuing)
(PLO-07)

LAB COMMITMENT CHART:

Pre-Lab
Group 30 Minutes 130 Minutes 10 Minutes
(10 Minutes)
Experiment Performance (Demonstration by Lab
Instructor) [10Mins]
Query
+
Attendance, Literature Session (If
Experiment Performance (by G1) [20Mins]
G1-G6 Assigned + any) + next
+
Tasks Instruction lab
In-Lab Evaluation (by Instructor) [20Mins]
discussion
+
Lab Report Preparation (by G2-G6 [80Mins]
LAB PLAN:

Exp # Experiment Name

To measure the Turbidity of Waste Water.

01

02 Determination pH Value of water.

03 To Find out the Suspended Solids.

04 To Find out the Dissolved Solids.

05 To Find out the Total Solids in given Sample Of Water.

To find Out The Concentration of Chloride in water.

06

07 To Find Out The Hardness In given Sample Of Water.

08 Determine The Chemical Oxygen Demand (COD) In Water.

09
Determine The Biochemical Oxygen Demand (BOD) In Water.
10 Determine The Dissolved Oxygen In a Sample.
LAB TARGETS:

Teaching Methodology Assessment PLO’s To

Experiments CLO No.
Methodology Target
Instruction +Discussion Lab Assignment +
01-05 3 +Demonstration + Lab Sessional 1 + PLO-7
Experimental performance Lab Sessional 2
Instruction +Discussion Lab Assignment +
06-10 4 +Demonstration + Lab Sessional 2 + PLO-7
Experimental performance Final

1-10 3,4 Experimental performance Lab Report PLO-07

TEACHING METHODOLOGY:
In order to achieve the course learning objectives, demonstrations, discussions, lab reports, queries and
presentations will be utilized.

STUDENT PARTICIPATION AND ATTENDANCE POLICY:

● Attendance must be at least 80%.

● Students should make every effort to be in class on time

ASSESSMENT
Evaluation will be competency based and student grades will be based on the following factors.
 Sr. Marks Distribution Total CU-Online Entity to
No. Marks Enter Marks
1 0.5*B + 0.5*A (Average Score of Labs before S1) 10 Lab Sessional 01
2 0.5*B + 0.5*A (Average Score of Labs after S1 and before S2) 15 Lab Sessional 02
3 Score of any Lab 25 Lab Assignments
4 0.5*B + 0.5*A (Average score of labs 2-
16) 50 Lab Terminal

Grand Total Lab Marks 100

MARKING SCHEME FOR LAB (1/3)

A) Marks break down for regular labs

B) Marks Breakdown for Lab Sessional 1, 2, and Lab-Terminal
C) tem B at S. No. 4 of last table corresponds to rubric-based evaluation conducted in Lab Terminal slot.

MARKING SCHEME FOR LAB (2/3)

Marks Breakdown for Regular Labs (1-16)

A
Pre-Lab In-Lab Post-Lab Total Marks
(1) (5) (4)
OBE Written Report
Rubric Evaluation
Check In-Lab Tasks
e.g.,

● Setting up the apparatus Written report providing

analysis of the data
Possible range Check Pre-Lab ● Note down required supported by appropriate
of activities for Tasks readings figures and tables (where 10
grading + applicable) and clearly
● Plot graphs
Attendance stated observations and
● Compare experimental calculations
and theoretical values

MARKING SCHEME FOR LAB (3/3)

Marks Break Down for Lab Sessional 1, 2 and Lab Terminal

B
In-Lab evaluation Only (OBE In-Lab Rubrics Based Evaluation) Total marks
 Performance of In-Lab Tasks given by instructor, which are based on
Possible content so far covered in future, for example,
range of
● Calculate thermal conductivity of a given material
activities for
grading
● Viva
LAB RUBRIC FOR ASSESSING IN-LAB PERFORMANCE
P3-PLO7 (Individual & Team Work)
Performanc Exceeds expectation
e (5-4)
Analysis is organized and
well supported by equations,
models etc.
Guided
Response Proper interpretation of
the results along with the
conclusion is made.
Able to explain
fundamental concepts
Q and A
correctly and provide
alternative solutions.
LAB RUBRIC FOR ASSESSING WRITTEN-LAB REPORT
A4-PLO7 (Communication)
Exceeds Expectations
Criteria
(4-5)
Student demonstrates
diligence in creating a
set of visually appealing
Data Presentation
tables and graphs that
effectively present the
experimental data
Data Analysis Student provides a very
accurate and focused
analysis of data. All
observations are stated
well and clearly
supported by the data.
Does not meet
Meets expectation
expectations
(3-2)
(1)
Analysis is
adequate and
the reader is
able to interpret
the results.
Able to explain most of
the relevant fundamental
concepts.
Meets Expectations
(2-3.99)
Experimental data is
presented in appropriate
format with only a few
minor errors or omissions
Student has analyzed the
data, observed trends and
compared experimental
results with theoretical
results.
Any discrepancies are
adequately addressed
10
Score
Analysis is inadequate
and the reader is unable
to interpret the results.
Unable to explain or
answer relevant
fundamental concepts.
Does not meet
expectations Score
(1-1.99)
Experimental data is poorly
presented.
Graphs and tables are poorly
constructed with several of the
following errors: data is missing
or incorrect, units are not
included, axis not labeled or
titles missing
Student has simply restated
what type of data was taken with
no attempt to interpret trends,
explain discrepancies or
evaluate the validity of data in
terms of relevant theory.
Student lacks understanding of
 All expected observations
the importance of the results.
are made.
Lab report has very few Lab report has several spelling
Lab report has no spelling or grammatical or grammatical errors.
spelling or grammatical errors. Student rarely uses technical
errors. The sentence flow is terms or uses them incorrectly
Writing Style
All sections of the report smooth. and too often resorts to jargon or
are well-written and Student uses technical clichés.
technically accurate. terms effectively.

HEALTH & SAFETY REGULATIONS

Users of EFM Laboratory must comply with the following safety instructions. At the beginning of the course the
instructor should brief the students about health and safety. The students should know where the fire exits, fire
extinguisher, fire alarm and the assembly point are in case of emergency such as fire or earthquake etc.

● No experiments should be conducted in the absence of Lab engineer and technician.

● Smoking is strictly prohibited inside the Lab.

● There should be no over-crowding. Only one person should operate one machine. In case, the
experiment needs more than one person for the operation, other group mates would join.

● Before operating any machine, you must be aware of the following:

● Location of fire extinguishers, fire blanket and the outside exits.

● How the machine operates. Read instructions or manual of the machine before operating it.

● How to turn off the machine in case of damages.

● Do not run inside the lab and concentrate on the present task.

● When moving heavy equipment or gas cylinders, use carts.

● Always use the right tools for the given task.

● Handle the tools and equipment with extreme care and return the tools to their proper places.

● Do not leave fuels in open containers.

● Please leave the Lab clean and tidy at end of experiment.
 Introduction of Water Supply Engineering Lab
The course aims at students developing a good working understanding of the basic and fundamental principles
of Water Supply Engineering. The object of this course is to introduce the basic principles and methods of
experimental Engineering to the students majoring in the Civil Engineering Department. The primary emphasis
of the course is on fundamental understanding the underlying principles of the topics that have been discussed
in the lectures using various experimental techniques, instruments and apparatus designed specifically for the
subjects concerned. This laboratory course involves not only the hardware aspects of experimentation, but also
the study of instrumentation and measurements techniques, as well as the philosophical content that should
help serve as a foundation for the future professional career of Civil engineers. . Hence, success in the course
will depend upon the student's own initiative and ideas toward the problem solving in a given experiment.
 LAB MANUAL

Water Supply Engineering

List of Experiments
Lab # Experiment Name

To measure the Turbidity of Waste Water.

I
Determination pH Value of water.
II

III To Find out the Suspended Solids.

To Find out the Dissolved Solids.

IV
To Find out the Total Solids in given Sample Of Water.
V
To find Out The Concentration of Chloride in water.
VI
VII To Find Out The Hardness In given Sample Of Water.
VIII Determine The Chemical Oxygen Demand (COD) In Water.

IX Determine The Biochemical Oxygen Demand (BOD) In Water.

X Determine The Dissolved Oxygen In a Sample.
 Experiment No. 01: Determination of Turbidity of Water.

1. Standard Designation:

2. Aim:
To determine the turbidity of the given water sample.

3. Introduction:
Turbidity is the technical term referring to the cloudiness of a solution and it is a quantitative
characteristic which is imparted by solids particles obstructing the transmittance of light through a
water sample. Turbidity often indicates the presence of dispersed and suspended solids like clay,
organic matters, silt, algae and other microorganisms.

4. Environmental Significance:
When the turbid water in a small, transparent container such as drinking glass is held up to the light, an
aesthetically displeasing opaqueness or milky coloration is apparent. The colloidal material which
exerts turbidity provides adsorption sites for chemicals and for biological organism that may not be
harmful. They may be harmful. They may be harmful or cause undesirable taste and odors.
Disinfection of turbid water is difficult because of the adsorption characteristics of some colloids and
because the solids may partially shield organisms from disinfectant. In natural water bodies, turbidity
may impart a brown or other color to water and may interfere with light penetration and photosynthetic
reaction in stream and lakes. Turbidity increases the load on slow sand filters.
The filter may go out of operation, if excess turbidity exists. Knowledge of the turbidity variation in raw
water supplies is useful to determine whether a supply requires special treatment by chemical
coagulation and filtration before it may be used for a public water supply. Turbidity measurements are
used to determine the effectiveness of treatment produced with different chemicals and the dosage
needed. Turbidity measure help to gauge the amount of chemicals needed from day-to-day operation
of water treatment works.

5. Principle:
Turbidity is based on the comparison of the intensity of light scattered by the sample under defined
conditions with the intensity of the light scattered by a standard reference suspension under the same
conditions. The turbidity of the sample is thus measured from the amount of light scattered by the
sample taking a reference with standard turbidity suspension. The higher the intensity of scattered light
the higher is the turbidity. Formazin polymer is used as the primary standard reference suspension.
6. Apparatus Required:
I. Turbidity meter. ii. Sample cells. iii. Standard funnel.

II. Funnel. v. Wash bottle. vi. Tissue. paper

7. Chemicals Required:
I. Hexamethylenetetramine. ii. Hydrazine sulphate. iii. Distilled water.

8. Sample Handling and Preservation:

● Water samples should be collected in plastic cans or bottles.

● All bottles must be cleaned thoroughly and should be rinsed with turbidity free water.

● Volume collected should be sufficient to insure a representative sample, allow for replicate
analysis (if required), and minimize waste disposal. No chemical preservation is required.
● Keep the samples at 4°C and do not allow the samples to freeze.

● Analysis should begin as soon as possible after the collection of samples.

● If storage is required, samples maintained at 4°C may be held for up to 48 hours.

9. Precautions:

● The following precautions should be observed while performing the experiment:

● The presence of colored solutes causes measured turbidity values to be low. Precipitation of
dissolved constituents (for example, Fe) causes measured turbidity values to be high.
 ● Light absorbing materials such as activated carbon in significant concentrations can cause low
readings.
● The presence of floating debris and coarse sediments which settle out rapidly will give low
readings. Finely divided air bubbles can cause high readings.

10. Procedure:

● For testing the given water sample first reagents are to be prepared. Then the turbidity
meter is required to be calibrated.

10.1. Preparation of Reagents

10.1.1. Hexamethylenetetramine

● Weigh accurately 1og of hexamethylenetetramine and dissolve it in turbidity free distilled

water.
● Take 100mL standard measuring flask and place a funnel over it.

● Transfer it to a 100mL standard flask and make up to 100mL using turbidity free distilled
water.

10.1.2. Hydrazine Sulphate

● Weigh accurately 1g of hydrazine sulphate and dissolve it in turbidity free distilled water.

● Take 100mL standard measuring flask and place a funnel over it.

● Transfer it to a 100mL standard flask and make up to 100mL using turbidity free distilled water.

10.1.3. Standard 4000 NTU Solution

● Mix 5mL of hydrazine sulphate and 5mL of hexamethylenetetramine solution in a 100mL

standard measuring flask.
● Allow the mixture to stand for 24 hours.

● After 24 hours, make up the volume to 100mL using turbidity free distilled water.

● The standard 4000 NTU solution is ready.

 10.2. Calibration of Turbidity Meter
Using the standard solution, calibrate the instrument.

Step 1.
To the sample cell, add turbidity free distilled water up to the horizontal mark, wipe gently with soft
tissue. Place it in the turbidity meter such that the vertical mark in the sample cell should coincide with
in the turbidity meter and cover the sample cell. Now using the set zero knob, adjust the reading to
zero.

Step 2.
According to our need, prepare a standard solution. In this case, a 200 NTU solution is prepared by
diluting the standard 4000 NTU solution and add to the sample cells, up to the horizontal marks, wipe
gently with soft tissue. Place it in the turbidity meter such that the vertical mark in the sample cell
should coincide with the mark in the turbidity meter and cover the sample cell.

Step 3.
If the instrument is not showing 200 NTU, using the calibration knob adjust the reading to 200 NTU.
Repeat the procedure for two/three times. Now the instrument is calibrated.

PROCEDURE CHART
 11. Testing of Water Samples:

● To the sample cell, add sample water up to the horizontal mark, wipe gently with soft tissue
and place it in the turbidity meter such that the vertical mark in the sample cell should coincide
with the mark in the turbidity meter and cover the sample cell.

● Check for the reading in the turbidity meter. Wait until you get a stable reading.

● Note the reading.

12. Calculation:
For determining the turbidity of the given water sample the reading are required to be tabulated.

Sample No. Temperature of Sample (°C) Turbidity (NTU)

1
2
3

Experiment No. 02: Determination of PH of Water.

1. Standard Designation:

2. Aim:

To determine the pH of the given water sample.

3. Introduction:
The term pH refers to the measure of hydrogen ions concentration in a solution and defined as the
negative log of H+ ions concentration in water and wastewater. The value of pH 0 to a little less than 7
are termed as acidic and the value of pH a little above 7 to 14 are termed as basic. When
concentration of H+ and OH- ions are equal then it is termed as neutral PH.

4. Environmental Significance:
Determination of pH is one of the important objectives in biological treatment of the wastewater. In
anaerobic treatment, if the pH goes below 5 due to excess accumulation of acids the process id
severely affected. Shifting of pH beyond 5 to 10 upsets the aerobic treatment of the wastewater. In
these circumstances, the pH is generally adjusted by addition of suitable acid or alkali to optimize the
treatment of the wastewater. PH value range is of immense importance for any chemical coagulation,
disinfection, water softening and corrosion control and governed by pH adjustment.
 Dewatering of sledges, oxidation of cyanides and reduction of hexavalent chromium into trivalent
chromium also need a favorable pH range, it is used in the calculation of carbonate, bicarbonate, CO2
corrosion, stability index and acid base equilibrium.
Lower value of pH below 4 will produce sour taste and higher value above 8.5 a bitter taste. Higher
values of pH hasten the scale formation in water heating apparatus and also reduce the germicidal
potential of chlorine. High pH induces the formation of trihalomethanes, which are causing cancer in
human beings.

5. Principle:

The pH electrode used in pH measurement is a combined glass electrode. It consists of sensing half-
cell and reference half-cell, together form an electrode system. The sensing half-cell is a thin pH
sensitive semi permeable membrane, separating two solutions, viz., the outer solution, the sample to
be analyzed and the internal solution enclosed inside the glass membrane and has known pH value.
An electric potential is developed inside and another electric potential is developed outside, the
difference in the potential is measured and is given as the pH of the sample.

6. Apparatus Required:

I. PH meter. II. Standard flask. III. Magnetic Stirrer. IV. Funnel.

V. Beaker. VI. Wash Bottle. VII. Tissue Paper. VIII. Forceps.

7. Chemicals Required:

I. Buffer Solution of pH 4.01, 7, 9.2. II. Potassium chloride. III. Distilled water.

8. Sample Handling and Preservation:

● Preservation of sample is not practical. Because biological activity will continue after
a sample has been taken, changes may occur during handling and storage.
● The characteristics of the water sample may change.
 ● To reduce the changes in samples taken for the determination of pH, keep samples at
4°C. Do not allow the sample to freeze.

9. Precautions:
● The following precautions should be observed while performing the experiment:

● Temperature affects the measurement of pH at two points.

● The first point is caused by the change in electrode output at different temperatures.
The interference can be controlled by the instruments having temperature
compensation or by calibrating the electrode-instrument system at the temperature of
the samples.
● The second change of pH inherent in the sample at different temperatures. This type
of error is sample dependent and cannot be controlled; hence both the pH and
temperature at the same time of analysis should be noted.
● In general, the glass electrode is not suitable to solution interference like color, high
salinity, colloidal matter, oxidants, turbidity or reductants.
● Oil and grease, if present in the electrode layer, should be removed by gentle wiping
or detergent washing, followed by rising with distilled water, because it could impair
the electrode response.
● Before using, allow the electrode to stand the dilute hydrochloric acid solution for at
least 2 hours.

● Electrodes used in the pH meter are highly fragile, hence handle it carefully.
 10. Procedure:

● Three major steps are involved in the experiment, they are.

I. Preparation of reagents. II. Calibrating the instrument. III.

Testing of sample.

10.1 Preparation of Reagents

⮚ Buffer Solution of pH 4.01

● Take 100mL standard measuring flask and place a funnel over it.

● Using the forceps carefully transfer one buffer tablet of pH 4.01 to the funnel.

● Add little amount of distilled water, crush the tablet and dissolved it.

● Make up the volume to 100mL using distilled water.

⮚ Buffer Solution of pH 7.0

● Take 100mL standard measuring flask and place a funnel over it.

● Using the forceps carefully transfer one buffer tablet of pH 7.0 to the funnel.

● Add little amount of distilled water, crush the tablet and dissolved it.

● Make up the volume to 100mL using distilled water.

⮚ Buffer Solution of pH 9.2

● Take 100mL standard measuring flask and place a funnel over it.

● Using the forceps carefully transfer one buffer tablet of pH 9.2 to the funnel.
 ● Add little amount of distilled water, crush the tablet and dissolved it.

● Make up the volume to 100mL using distilled water.

10.2 Calibrating the Instrument

Using the buffer solutions calibrate the instrument.

Step 1.
● In a 100mL beaker take pH 9.3 buffer solution and place it in magnetic stirrer, insert the
Teflon coated stirring bar and stir well.
● Now place the electrode in the beaker containing the stirred buffer and check for the reading
in the pH meter.
● If the instrument is not showing pH value 9.2, using the calibration knob adjust the reading to
9.2.
● Take the electrode from the buffer, wash it with distilled water and then wipe gently with soft
tissue.

Step 2.

● In a 100mL beaker take pH 7.0 buffer solution and place it in magnetic stirrer, insert the
Teflon coated stirring bar and stir well.
● Now place the electrode in the beaker containing the stirred buffer and check for the
reading in the pH meter.
● If the instrument is not showing pH value 7.0, using the calibration knob adjust the
reading to 7.0.
● Take the electrode from the buffer, wash it with distilled water and then wipe gently with
soft tissue.

Step 3.

● In a 100mL beaker take pH 4.01 buffer solution and place it in magnetic stirrer, insert the
Teflon coated stirring bar and stir well.
● Now place the electrode in the beaker containing the stirred buffer and check for the
reading in the pH meter.
● If the instrument is not showing pH value 4.01, using the calibration knob adjust the
reading to 4.01.
 ● Take the electrode from the buffer, wash it with distilled water and then wipe gently with
soft tissue.

11. Testing of Sample:

● In a clean dry 100mL beaker take the water sample and place it in a magnetic stirrer,
insert the Teflon coated stirring bar and stir well.
● Now place the electrode in the beaker containing the water sample and check for the
reading in the pH meter. Wait until you get a stable reading.
● Note the reading.

● Take the electrode from the water sample, wash it with distilled water and then wipe
gently with soft tissue.

12. Calculation:
To determine the value of pH of the given water sample the reading obtained are required
to be tabulated.

Sample No Temperature of Sample (°C) PH

1.
2.
3.
Experiment No. 03: Determination of Total Suspended Solids in
Water.
1. Standard Designation:

2. Aim:

To determine total suspended solids in the given water sample.

3. Introduction:
The total suspended solids parameter is used to measure the quality of wastewater influent and
effluent. Suspended solids determination is extremely valuable in the analysis of polluted
waters. It is a very important parameter in wastewater treatment. The data obtained from this
test is used in the design of wastewater treatment plants.
The total suspended solids refers to the solid material in water or wastewater sample, which is
retained by a filter of 2.0 μm (or smaller) nominal size under specified conditions.
They can also be referred to as the solid materials which are not dissolved in water and are non-
filterable in nature.
They can be further classified as Settle able and Non-Settle able depending upon their settling
velocities or they can be classified as Organic and Inorganic as shown in Fig.
TSS can include a wide variety of material, such as silt, decaying plant and animal matter,
industrial wastes, and sewage.
 4.
Environmental Significance:
Suspended material is aesthetically displeasing and provides adsorption sites for chemical
and biological agents. Suspended organic solids which are degraded anaerobically may
release obnoxious odors.
Biologically active suspended solids may include disease causing organisms.

5. Principle:

A well-mixed sample is filtered through a standard glass fiber filter, and the filtrate is evaporated to
dryness in a weighed dish and dried to constant weight. The increase in dish weight represents the total
dissolved solids.
If the suspended material clogs the filter and prolongs filtration, the difference between the total solids
and total dissolved solids may provide an estimate of the total suspended solids.

6. Apparatus Required:

I. China Dish/Evaporating Dish. II.Oven. III. Electronic Balance.

IV. Measuring Cylinder. VI. Filter Paper. VIII. Forceps.

IX. Desiccator (sealable enclosures containing desiccants used for preserving moisture-sensitive items)

X. Filtration Assembly with Vacuum Pump XI. Petri Dish

7. Chemicals Required:

● Water Sample

● Sample Handling and Preservation:

● Preservation of sample is not practical. Because biological activities will continue after a
sample has been taken, changes may occur during handling and storage.

● Both the characteristics and the amount of solids may change.

● To reduce this change in samples taken for solids determinations, keep all samples at
4oC. Do not allow samples to freeze. Analysis should begin as soon as possible.

8. Precautions:
 ● Water or wastewater samples which contain high concentration of calcium, chloride, magnesium or
sulphate can rapidly absorb moisture from the air. Such sample may need to be dried for a longer
period of time in order to achieve a reasonable constant weight.

● We should be aware that prolonged drying may result in loss of constituents, particularly nitrates
and chlorides.

● Great care must be taken when taking the china dish/Petri dish out of the oven, as it is usually very
hot. The use of dish tongs is preferred.

● Forceps must always be used for handling the filter paper and it should never be handled directly
by hand.

● The filter paper must be allowed to sufficiently cool to room temperature in a desiccator to get an
accurate measurement of weight.

9. Procedure:

● Weigh the petri dish or china dish along with a filter paper using the electronic balance.
Let its weight be “A” milligrams.

● Place the filter paper on the filtration assembly and turn on the vacuum pump.

● Pour 50 ml of water sample over the filter paper using a measuring cylinder and wait for
it to pass down into the flask.

● Carefully remove the filter paper from the filtration assembly and transfer it to the
already weighed petri dish or china dish.
 ● Place the filter paper along with the petri dish in an oven at a temperature of 105ᵒC for 30
– 60 minutes and allow it to dry.

● After drying, allow the filter paper and petri dish to cool to room temperature in a
desiccator.

● Weigh the petri dish along with the filter paper again. Let its weight be “B” milligrams.

● Calculate the Total Suspended Solids in mg/liter by using Eq. (1),

( B−A ) × 1000
Total Suspended Solids (mg/L) =
Volume of sample ∈millieters

10. Calculations:

● Weight of china dish + Filter Paper = A = milligrams

● Weight of china dish + dried filter paper + non-filterable solids = B = milligrams

● Using Eq. (1),

● Total Suspended Solids (mg/L) = (B−A) ×100050= 𝑚𝑔/𝐿

Experiment No. 04: Determination of Total Dissolved Solids in
Water.

1. Standard Designation:

2. Aim:

To determine total dissolved solids in the given water sample.

3. Introduction:

Total dissolved solids are measured in waters and wastewaters because they influence other
qualities of water such as taste, hardness, corrosion etc. Its amount in water is a consideration
for the suitability of that water for drinking and other purposes.

The total suspended solids refers to the solid material in water or wastewater sample, which
passes through a filter of 2.0 μm (or smaller) nominal size under specified conditions.

They can also be referred to as the solid materials which are completely dissolved in water
and are filterable in nature. It is defined as the residue upon evaporation of filterable sample.

They can be further classified as Organic and Inorganic as shown in Fig.

Total dissolved solids (TDS) comprise inorganic salts and small amounts of organic matter that are
dissolved in water. The principal constituents are usually the cautions calcium, magnesium, sodium
and potassium and the anions carbonate, bicarbonate, chloride, sulphate and, particularly in
groundwater, nitrate (from agricultural use).

4. Environmental Significance:
 Dissolved minerals, gases and organic constituents may produce aesthetically displeasing
color, taste and odor. Some dissolved organic chemicals may deplete the dissolved oxygen in
the receiving waters and some may be inert to biological oxidation, yet other has been
identified as carcinogens.

High concentration of dissolved solids about 3000 mg/L may also produce distress in livestock. In
industries, the use of water with high amount of dissolved solids may lead to scaling in boilers,
corrosion and degraded quality of the product.

Estimation of total dissolved solids is useful to determine whether the water is suitable for drinking
purpose, agriculture and industrial purpose.

5. Principle:
A well-mixed sample is filtered through a weighed standard glass fiber filter, and the filtrate
is dried to a constant weight at 103 – 105ᵒC. The increase in weight represents the total
dissolved solids.

6. Apparatus Required:
I. China Dish/Evaporating Dish. II. Oven. III. Electronic Balance.
IV. Measuring Cylinder. V. Filter Paper. VI. Filtration Assembly with
Vacuum Pump.
VII. Forceps. VIII. Petri Dish. IX. Desiccator (sealable enclosures
containing desiccants used for preserving moisture-sensitive items)

7. Chemicals Required:
I. Water Sample.

8. Preservation:
Preservation of sample is not practical. Because biological activities will continue after a
sample has been taken, changes may occur during handling and storage.

Both the characteristics and the amount of solids may change.

 To reduce this change in samples taken for solids determinations, keep all samples at 4°C.
Do not allow samples to freeze. Analysis should begin as soon as possible.

9. Precautions:

● Water or wastewater samples which contain high concentration of calcium, chloride,

magnesium or sulphate can rapidly absorb moisture from the air. Such sample may need
to be dried for a longer period of time in order to achieve a reasonable constant weight.

● We should be aware that prolonged drying may result in loss of constituents, particularly
nitrates and chlorides.

● Great care must be taken when taking the china dish/Petri dish out of the oven, as it is
usually very hot. The use of dish tongs is preferred.

● Forceps must always be used for handling the filter paper and it should never be handled
directly by hand.

● The china dish must be allowed to sufficiently cool to room temperature in a desiccator
to get an accurate measurement of weight.
10. Procedure:

● Weigh the china dish using the electronic balance. Let its weight be “A” milligrams.

● Place the filter paper on the filtration assembly and turn on the vacuum pump.

● Pour 50 ml of water sample over the filter paper using a measuring cylinder and wait for
it to pass down into the flask.

● Take the filtrate and transfer it to the already weighed china dish.

● Place the china dish containing the filtrate in an oven at a temperature of 105ᵒC for
roughly 24 hours and allow it to dry.

● After drying, allow the china dish to cool to room temperature in a desiccator.

● Weigh the china dish with the residue again. Let its weight be “B” milligrams.

● Calculate the Total Dissolved Solids in mg/liter by using Eq. (1),

( B− A ) × 1000
Total Dissolved Solids (mg/L) = Volume of sample ∈millimeters
(1)
 11. Calculation:

● Weight of china dish = A = milligrams

● Weight of china dish + dried residue = B = milligrams

● Using Eq. (1),

( B−A ) ×1000 mg
● Total Dissolved Solids (mg/L) = = L
50

Experiment No. 05: Determination of Total Solids in Water.

1. Standard Designation:

2. Aim:
To determine the total solids in the given water sample.

3. Introduction:
This experiment is applicable to waters of wide range of quality including surface water,
industrial and domestic effluents, treated wastewaters etc. Total solids measurements can be
useful as an indicator of the effects of runoff from construction, agricultural practices,
logging activities, sewage treatment plant discharges, and other sources.
Water and wastewater consists of pure water along with various dissolved, colloidal and
suspended contaminants.
3.1 Solids
Solids are defined as,

“The matter that remains as residue upon evaporation of free water at 103 -105ᵒC”

All the materials that exert significant vapor pressure at such temperatures are, of course, lost
during the evaporation and drying process. The solids or the residue that remains represents
only that material in the sample, which has a negligible vapor pressure at such temperatures.
 A solid holds its shape because its atoms are not allowed to move too much, unlike the
liquids and gases where molecules are bouncing and floating around, free to move where
they want.

The term “solids” is generally used when referring to any material suspended or dissolved in
water or wastewater that can be physically isolated either through filtration or through
evaporation.

Solids can be classified as non-filterable (suspended) or filterable (dissolved). For example,

salts are often found dissolved in water such as NaCl, KCl, CaCl2. The salts exist in the form
of ions in water. Non-filterable solids may either be settle able or non-settle able.

Whether solids are settle able on non-settle able depends upon their settling velocity. Settle
able solids may settle within 5 - 10 min in water whereas, non-settle able solids may take
years to do so. Solids can also be classified as organic or inorganic. Measurement of solids
can be made in different water samples (industrial, domestic and drinking water).

Thus, Total solids are nothing but summation of total dissolved solids and total suspended solids.

4. Environmental Significance:

Amount of total solids in water have a widespread significance. Total solids affect water
clarity. Higher solids decrease the passage of light through water which might in turn
adversely affect photosynthesis by aquatic plants. These particles also show a tendency to
hold more heat, as a result of which water will heat up and affect the aquatic life that has
adapted to a lower temperature regime.

As with turbidity, concentrations often increase sharply during rainfall, especially in

developed watersheds. They can also rise sharply during dry weather if earth-disturbing
activities are occurring in or near the stream without erosion control practices in place.
Regular monitoring of total solids can help detect trends that might indicate increasing
erosion in developing watersheds.

4.1. In Case of Water

 Water with total solids is generally of inferior palatability (acceptability to taste) and may
induce an unfavorable physiological reaction. It may be esthetically unsatisfactory for
purposes such as bathing.

Presence of high total solids affect the effectiveness of disinfection process of killing
microorganisms, as they will be shielded by these particles.

It is used to assess the suitability of potential supply of water for various uses. In the case of water
softening, amount of total solids determine the type of softening procedure.

4.2 In Case of Wastewater

Solids analyses are important in the control of biological and physical wastewater treatment
processes and for assessing compliance with regulatory agency wastewater effluent
limitations.

Although the wastewater or sewage normally contains 99.9% of water and only 0.1% of
solids, but it is the solids that have the nuisance value. The amount of solids in wastewater is
frequently used to describe the strength of the water. The more solids present in a particular
wastewater, the stronger that wastewater will be.

If solids in wastewater are mostly organic, the impact on a treatment plant is greater than if the solids
are mostly inorganic.

5. Principle:

The sample is evaporated in a weighed dish and is dried to a constant mass in an oven at 103
– 105ᵒC or 179-181ᵒC.

Total solids/residue is calculated from increase in mass.

6. Apparatus Required:
I. China Dish/Evaporating Dish. II. Oven.
III. Electronic Balance. V. Measuring Cylinder.

VI. Desiccator (sealable enclosures containing desiccants used for preserving moisture-
sensitive items)

7. Chemicals Required:
I. Water Sample
8. Preservation:

● Preservation of sample is not practical. Because biological activities will continue after a
sample has been taken, changes may occur during handling and storage.

● Both the characteristics and the amount of solids may change.

● To reduce this change in samples taken for solids determinations, keep all samples at
4°C. Do not allow samples to freeze. Analysis should begin as soon as possible.

9. Precautions:

● Water or wastewater samples which contain high concentration of calcium, chloride,

magnesium or sulphate can rapidly absorb moisture from the air. Such sample may need
to be dried for a longer period of time in order to achieve a reasonable constant weight.

● We should be aware that prolonged drying may result in loss of constituents, particularly
nitrates and chlorides.

● Great care must be taken when taking the china dish out of the oven, as it is usually very
hot. The use of dish tongs is preferred.
10. Procedure:

● Weigh the china dish on the electronic balance. Let its weight be “A” milligrams.
 ● Using a measuring cylinder (or pipette), add 50 ml of water sample (tap water in this
case) to the china dish.

● Place the china dish in the oven at a temperature of 105ᵒC. The oven should be preheated
to ensure adequate drying.

● Allow the water to evaporate.

● After complete drying take the china dish out of the oven and cool to room temperature in a
desiccator.

● Again weigh the china dish, let its weight be ‘B’ milligrams.

● Calculate the Total Solids in mg/liter by using Eq. (1),

( B− A ) ×1000
Total Solids (mg/L) =
Volume of Sample ∈millimeters

11. Calculation:

● Weight of china dish = A = milligrams.

● Weight of dried residue + china dish = B = milligrams

● Using Eq. (1),

( B−A ) ×1000
● Total Solids (mg/L) = = mg/L
50
Experiment No. 06: Determination of Chlorides in Water.

1. Introduction:

Chlorides occur in all natural waters in widely varying concentration, the chloride content normally
increases as the mineral content increases. Upland and mountain supplies usually are quite low in
chlorides, whereas river and groundwater usually have a considerable amount. Sea and ocean waters
represent the residues resulting from partial evaporation of natural waters that flow into them and
chloride levels are very high. Chlorides gain access to natural waters in many ways. The solvent power
of water dissolves chlorides from topsoil and deeper formations. Spray from the ocean is carried inland
as droplets or as minute salt crystals, which result from evaporation of the water in the droplets. These
sources constantly replenish the chlorides in inland areas where they fall. Ocean and seawaters invade
the rivers that drain into them, particularly the deeper rivers. The salt water, being denser, flows
upstream under the fresh water, which is flowing downstream. There is a constant intermixing of the
salt water with the fresh water above. Groundwater in areas adjacent to the ocean is in hydrostatic
balance with seawater. Over-pumping of groundwater produces a difference in hydrostatic head in
favor of the seawater, and it introduce into the fresh water area. Such intrusion has occurred in many
areas of the coastal southern region of Bangladesh.
Human excreta, particularly urine, contain chloride in an amount about equal to the chlorides
consumed with food and water. This amount average about 6 gm of chlorides per person per day and
increases the amount of CC in municipal wastewater about 15 mg/l above that of the carriage water.
Thus, wastewater effluents add considerable chlorides to receiving streams. Many industrial wastes
(e.g., tannery waste) also contain appreciable amount of chlorides.

2. Environmental significance:
 Chlorides in reasonable concentrations are not harmful to human. At concentrations above 250 mg/L
they give a salty taste to water, which is objectionable to many people. For this reason, chlorides are
generally limited to 250 mg/L in supplies intended for public use. In many areas of the world where
water supplies are scarce, source be containing as much as 2,000 mg/L are used for domestic
purposes without the development of adverse effects, once the human system becomes adapted to the
water.

3. Guideline:

According to Bangladesh Environment Conservation Rules (1997), drinking water standard for chloride
is 150 - 600 mg/L; but for coastal regions of Bangladesh, the limit has been relaxed to 1000 mg/L.

4. Principle: (Mohr’s Method):

This method determines the chloride ion concentration of a solution by titration with silver nitrate. As
the silver nitrate solution is slowly added, a precipitate of silver chloride forms.
Ag+(aq) + Cl–(aq) → AgCl(s) 6.1
The end point of the titration occurs when all the chloride ions are precipitated. Then additional silver
ions react with the chromate ions of the indicator, potassium chromate, to form a red-brown precipitate
of silver chromate.
2Ag+(aq) + CrO42–(aq)→ Ag2CrO4(s) 6.2
This method can be used to determine the chloride ion concentration of water samples from many
sources such as seawater, stream water, river water and estuary water. The pH of the sample
solutions should be between 6.5 and 10. If the solutions are acidic, the gravimetric method or Volhard’s
method should be used.
The end point of titration cannot be detected visually unless an indicator capable of demonstrating the
presence of excess Ag+ is present. The indicator normally used is potassium chromate, which supplies
chromate ions. As the concentration of CI- ions becomes exhausted, the silver ion concentration
increases and a reddish brown precipitate of silver chromate is formed.
2Ag++CrO42- = Ag2CrO4 (reddish brown precipitate) 6.3
This is taken as evidence that all chloride has been precipitated. Since an excess Ag+ is needed to
produce a visible amount of Ag2CrO4, the indicator error is subtracted from all titrations.
The indicator error or blank varies somewhat with the ability of individuals to detect a noticeable color
change. The usual range is 0.2 to 0.4 mL of titrant. An error of 0.2 mL will be used in the class.

5. Precautions:

● A uniform sample size must be used, preferably 100 ml (or 50 mL), so that ionic concentrations
needed to indicate the end point will be constant.
● The pH must be in the range of 7 to 8 because Ag+ is precipitated as AgOH at high pH levels and
the CrO4 2−¿Type equationhere . ¿ is converted to Cr2O72- at low pH levels,
● A definite amount of indicator must be used to provide a certain concentration of CrO4; otherwise
Ag2CrO4 may form too soon or not soon enough.
 ● The chromate solution needs to be prepared and used with care as chromate is a known
carcinogen.
● Silver nitrate solution causes staining of skin and fabric (chemical burns). Any spills should be
rinsed with water immediately.

6. Apparatus:
I Burette. II. Measuring cylinder. III. Beaker.

IV. Dropper. V. Stirrer.

7. Reagents:
I. Potassium chromate indicator. II. Silver nitrate solution (0.0141 N).

8. Procedure:

● Take 50 mL of the sample in a beaker and add 5 drops (about 1 mL) of potassium chromate
indicator to it.
● Add standard (0.0141 N) silver nitrate solution to the sample from a burette, a few drops at a time,
with constant stirring until the first permanent reddish color appears. This can be determined by
comparison with distilled water blank. Record the mL of silver nitrate used.
● If more than 7 or 8 mL of silver nitrate solution are required, the entire procedure should be
repeated using a smaller sample diluted to 50 ml with distilled water.

9. Calculation:
−¿¿
Chloride, Cl (mg/L) = (mL of AgNO3 used - "error" or "blank") × Multiplying Factor (M.F)

Normality of AgN O 3 × equivalent wt of cl × 1000

Where, M.F. =
mL of sample taken
Experiment No. 07: Determine the Total Hardness, of different
water samples.
To determine the Total Hardness, of different water samples.

Related Theory
Scope
This method is applicable for drinking water.
Hard water
Hard Water was originally described as the soap-destroying power of water, caused by the presence of
calcium and magnesium salts and measured by titration against a standard soap solution.
Sources of Hardness Minerals in Drinking Water
Water is a good solvent and picks up impurities easily. Pure water -- tasteless, colorless, and odorless is
often called the universal solvent. When water is combined with C O2 to form very weak carbonic acid, an
even better solvent results. 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 degree of hardness becomes greater as the calcium and magnesium
content increases and is related to the concentration of multivalent cations dissolved in the water. Calcium
is dissolved in water as it passes over and through limestone deposits. Magnesium is dissolved as water
passes over and through dolomite and other magnesium bearing formations. Because groundwater is in
contact with these geologic formations for a longer period of time than surface water, groundwater is usually
harder than surface water.
Types of Hardness
There are two types of hardness.

i. Temporary Hardness
It is due to the presence of bicarbonate of calcium and magnesium and can be removed by boiling. It is also
called the carbonate hardness. It is sensitive to heat and precipitate readily at high temperature.
ii. Permanent Hardness
It is attributed to other salts such as sulfate and chloride salts, which cannot be removed by boiling. It is also
called the non-carbonate hardness and is not sensitive to temperature.
Classification of Hardness
The degree of hardness consumers consider objectionable will vary, depending both on the water
and the degree of hardness to which consumers has become accustomed. The following table shows a
classification of water hardness:
 Description of Hardness mg/L as CaCO3
So 0-
ft 50
Moderately Soft 50-
100
Slightly Soft 100-
150
Moderately Hard 150-
200
Har 200-
d 300
Very Hard >30
0

Environmental Significance

 Water hardness is important to fish culture and is a commonly reported aspect of water quality. Calcium
has an important role in the biological processes of fish. It is necessary for bone formation, blood
clotting and other metabolic reactions. Fish can absorb calcium for these needs directly from the water
or food. The presence of free (ionic) calcium at relatively high concentrations in culture water helps
reduce the loss of other salts (e.g. sodium and potassium) from fish body fluids (i.e. blood). Sodium
and potassium are the most important salts in fish blood and are critical for normal heart, nerve and
muscle function. In low calcium water, fish can lose (leak) substantial quantities of these salts into the
water. Fish must then use energy supplied by their feed to re-absorb lost salts. That can reduce the
energy available for growth and may extend the time necessary to grow fish to market Size. For some
species (e.g. red drum and striped bass), environmental calcium is required for good survival.
• Hardness was originally defined as the capacity of water to precipitate soap. Calcium and magnesium
precipitate soap, forming a curd which causes “bathtub ring” and dingy laundry (yellowing, graying, loss
of brightness, and reduced life of washable fabrics), and feels unpleasant on the skin (red, itchy, or dry
skin). To counteract these problems, synthetic detergents have been developed. These detergents
have additives known as sequestering agents that “tie-up” the hardness ions so they cannot form the
troublesome precipitates. Although synthetic detergents overcome these problems, both soap and
detergent are wasted by hardness.
• Hard water interferes with almost every cleaning task from laundering and dishwashing to bathing and
personal grooming. Clothes laundered in hard water may look dingy and feel harsh and scratchy.
Dishes and glasses may be spotted when dry. Hard water may cause a film on glass shower doors,
shower walls, bathtubs, sinks, faucets, etc. Hair washed in hard water may feel sticky and look dull.
Water flow may be reduced by deposits in pipes.
• Hard water is not a health hazard. In fact, the National Research Council (National Academy of
Sciences) states that hard drinking water generally contributes a small amount toward total calcium and
magnesium human dietary needs. They further state that in some instances, where dissolved calcium
and magnesium are very high, water could be a major contributor of calcium and magnesium to the
diet.

Measurement
a. Apparatus
 i. Automatic burette (or conventional one)
ii. Titration glassware

b. Reagents
i. Ammonia buffer solution; for Total Hardness ii.
Eriochrome Black T, for Total Hardness
iii. Standard EDTA titrant, 0.01
c. Procedure
Hardness can be determined by Complex-o-metric titration.
For Total Hardness
1. Take 25 ml of water sample in titration flask.
2. Add 25 ml Distilled water in it to dilute the water solution (to avoid formation of CaCO3).
Distilled water does not participate in ion exchange in reaction.
3. Add 1-2 ml of Buffer solution (Ammonia Buffer NH4Cl + NH4OH) to maintain pH in solution 7-9.
4. Add small amount of EBT (Ecrichrome Black T) as indicator. As a result of addition of
EBT, solution of color changes to wine red.
5. Titrate it against 0.01N EDTA solution. Add EDTA from burette until color changes to blue.
6. Test three samples and determine mean volume of titrant used.
7. Total Hardness (mg/L) as CaCO3 is calculated from the following formula:
Where;
Normality of EDTA = 0.01N
Volume of sample used=25ml
MW of CaCO3 = 100
LAB MANUAL WSE

Experiment No.08: Estimation of Chemical Oxygen

Demand of Waste water sample

1. Theory and Principle:

These are some organic matter especially from industrial waste that is toxic to bacteria and then it is
difficult to calculate bacteria. COD is calculated for these types waste.

2. COD definition:
It is the amount of oxygen required by the strong oxidizing agent to completely oxidize the organic
matter under acidic conditions. The BOD, the organic matter is not completely oxidized. Biologically
degradable organic matter is only oxidized. But in COD both the biologically degradable and
biologically inactive organic matter is oxidized, so COD is always more than BOD.

3. Advantages of COD test:

● This test can be performed in short duration (3hrs) whereas BOD takes 5 days.

● If sufficient data is available on BOD and COD of particular sewage accumulated, ration of BOD
and COD can be determined.
● The most readily oxidizing agent K2Cr2O7 can be used.

4. Reagents required:

● Standard K2Cr2O7 solution (0.025N)

● Sulphuric Acid H2SO4

● Standard ferrous ammonium sulphat solution (0.1N)

● Ferrous indicator solution

● Mercuric sulphate.

● Sulphuric acid (require only if the interference of nitrate is to eliminated)

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5. Standards:
NEQS (National Environmental Quality
Standards) standards value is 150 mg/liter

6. Apparatus:
I. Reflux Apparatus. II. COD
apparatus. III. Reflux Apparatus.

7. Procedure:

● 0.4 ml of mercuric sulphate is taken in a fluxing flask appropriately. Then 20 ml of sewage sample
and 10 ml of standard K2Cr2O7 solution is added to the above flask along with several granular of
glass beats to stop splitting of liquid during boiling.
● The flask is connected to the condenser 30 ml of Concentrated H 2SO4 containing Ag SO4 is
added slowly through open end of condenser and it is mixed thoroughly by swirling while adding
the acid. The reflux mixture is mixed thoroughly before heat is supplied if this is not done local
heating occurs in the bottom of the flask and the mixture may be blown out of condenser.
● The mixture is heated for two hours; it is cooled and waved down the condenser with distilled
water. The mixture is diluted to about 150 ml with distilled water, cooled at room temperature, and
excess of dichromate standard ferrous ammonium sulphate using ferrous indicator. (2 drops).

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● The end point is sharp color change from blue green to reddish brown.

● The experiment is repeated and refluxed in the same manner without sample (blank) consisting of
20 ml of distilled water together with the reagents.

Experiment No.09: Determination of the Biological

Oxygen Demand (BOD) of a Waste Water Sample.
1. Theory:
Biochemical oxygen demand is the amount of oxygen required for the microorganism (bacteria)
present in the waste water to convert the organic substance to stable compounds such as CO 2 and
H2O.

Organic Substance+ Oxygen +Bacteria CO 2 + H 2 O

2. Apparatus:
I. BOD bottle. II. Burette. III. Pipit.

IV. Pipit filler. V. Graduated cylinder.

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3. Chemicals:
I. Manganese sulphate. II.alkaliiodine acid. III.concentrated Sulphuric Acid.

IV. Standard thaiosulphide and starch indicator.

4. Procedure:

● Take two BOD bottles and half fill it with distilled water.

● Add 3ml of waste water (polluted water) to the BOD bottle with the help of pipit.

● Now filled the tube with distilled water and fix stopper on it.

● Put one of the tubes in indicator at 200C for five days.

● Add 2ml of manganese sulphate MnSO4 to other tube with the help of pipit and shake it well.
(if oxygen is present the color will be brown otherwise white).

● Add 2ml of concentrated H2SO4 and shake well which will give a color which is in
resemblance to mustard oil.

● Take 200 ml from this solution in graduated cylinder and add 1ml of starch indicator to it
which will give a yellowish color.

● Put the graduated cylinder below the burette containing the standard solution of sodium
thiosulphate and note the initial reading.

● Find dissolved oxygen by subtracting the initial reading from final reading.

● After incubation of the first tube the dissolved is found in similar way.

● Find the BOD by using the formula.

BOD (mg/l) = (Zero day DO – 5 days DO)*300mg/l of sample

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5. Standards:

● The BRCES (British royal commission effluent standard) allow a BOD of 20 mg/l in a treated
sewage to be discharged in to any water body.

● BOD value according to NEQS = 80 mg/liter

6. Observations and calculations:

● For 5 ml Sample:

At zero day (DO) 0 = ---------

After 5 days (DO) 5 = ---------

BOD of Sample = (DO at zero day – DO after 5 days)/Volume *300

BOD of Sample = ------------ mg/liter

● For 10 ml Sample:

At zero day (DO) 0 = ---------

After 5 days (DO) 5 = ---------

BOD of Sample = (DO at zero day – DO after 5 days)/Volume *300

BOD of Sample = ------------ mg/liter

● For 20 ml Sample:

At zero day (DO) 0 = ------------

After 5 days (DO) 5 = -------------

BOD of Sample = (DO at zero day – DO after 5 days)/Volume *300

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BOD of Sample = ------------ mg/liter

Result:

BOD of Sample = (BOD1+BOD2+BOD3)/3

BOD of Sample = -------------- mg/liter

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Experiment # 10:
Determination of Dissolved Oxygen Demand of Waste water
sample

1. Standard Designation:

2. Aim:

To determine the dissolved oxygen in the given water sample.

3. Introduction:
This test covers the determination of the dissolved oxygen in a given wastewater sample. This
dissolved oxygen value is further used in the calculation of Biochemical Oxygen Demand (BOD) as
well. Moreover, dissolved oxygen (DO) is essential for the maintenance of healthy lakes and rivers.
It is a measure of the ability of water to sustain aquatic life.

The term Dissolved Oxygen is used to describe the amount of oxygen dissolved in a unit volume of
water.

The dissolved oxygen content of water is influenced by the source, raw water temperature,
treatment and chemical or biological processes taking place in the distribution system.

The presence of oxygen in water is a good sign. Depletion of dissolved oxygen in water supplies
can encourage the microbial reduction of nitrate to nitrite and sulfate to sulfide.

Hence, analysis of dissolved oxygen is an important step in water pollution control and wastewater
treatment process control. There are various methods available to measure Dissolved Oxygen,
which we will discuss in detail.

In a healthy body of water such as a lake, river, or stream, the dissolved oxygen is about 8 parts per
million. The minimum DO level of 4 to 5 mg/L or ppm is desirable for survival of aquatic life.

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Now imagine that a source of oxygen demanding wastes, such as feed lot, a paper mill or a food
processing plant, is built besides the river. The facility begins operating and discharging wastes into
the river.

This increases the BOD and affects the concentration of DO in the waters downstream.

The wastes serve as the food for certain aerobic bacteria. As it moves downstream, the conc. of
bacteria increases. Because these bacteria remove oxygen from water, their population increase
causes a decline in the amount of DO.

Beyond certain point, most of the wastes break down. The conc. of DO rises as the river recovers
oxygen from the atmosphere and aquatic plants. Thus DO test is the basis for BOD test which is an
important parameter to evaluate organic pollution potential of a waste.

It is necessary for all aerobic biological wastewater treatment processes to control the rate of
aeration.

4. Environmental Significance:

● Drinking water should be rich in dissolved oxygen for good taste.

● DO test is used to evaluate the pollution strength of domestic and industrial waste.

● Higher values of DO may cause corrosion of Iron and Steel.

● Algae growth in water may release oxygen during its photosynthesis and DO may even
shoot upto 30 mg/L.

● Oxygen is poorly soluble in water. Its solubility is about 14.6 mg/l for pure water at 0°C
under normal atmospheric pressure and it drops to 7 mg/l at 35°C.

● Higher temperature, biological impurities, Ammonia, Nitrates, ferrous iron, chemicals

such as hydrogen sulphide and organic matter reduce DO values.

● Aerobic bacteria thrive when oxygen is available in plenty. Aerobic conditions do

prevail when sufficient DO is available within water. End products of aerobiosis are
stable and are not foul smelling.

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● It is necessary to know DO levels to assess quality of raw water and to keep a check on
stream pollution.

● DO test is the basis for BOD test which is an important parameter to evaluate organic
pollution potential of a waste.

● DO test is necessary for all aerobic biological wastewater treatment processes to control
the rate of aeration.

● Fresh water always has a high DO than standing water. DO of standing water can be
increased by installing fountains such as in parks.

5. Principle:
Dissolved Oxygen can be measured either by titrimetric or electrometric method.

5.1 Titrimetric Method:

Titrimetric method is based on the oxidizing property of DO while the electrometric method (using
membrane electrodes) is based on the rate of diffusion of molecular oxygen across a membrane. It
is most accurate method to determine DO.

There are different titrimetric methods based on the nature of sample to be tested.

I. Winkler Method. II. Azide Modification.

III. Alum Flocculation Modification. IV. Permanganate Modification.

5.2 Electrometric Method (Using DO meter):

● The electrode method offers several advantages over the titrimetric method including
speed, elimination or minimization of interferences, field compatibility, continuous
monitoring and instrument measurement.

● Dissolved oxygen can be measured by a special sensor kept in an electrochemical cell.

The cell comprises a sensing electrode, a reference electrode and a supporting
electrolyte, a semi-permeable membrane, which served dual function.

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● It separates the water sample from the electrolyte, and at the same time, permits only the
dissolved oxygen to diffuse from the water sample through the membrane into the
supporting electrolyte.

6. Apparatus Required:

I. Burette. II. Burette Stand. III. Wash Bottle

IV. 500 mL conical flask. V. Pipette or graduated cylinder. VI.
Pipette Bulb.
VII. 300 mL glass stoppered BOD bottles.
7. Chemicals Required:
I. Manganese Sulphate (MnSO4). II. Alkali Azide (NaN3).
III. Concentrated Sulphuric Acid (H2SO4).
IV. Starch Indicator.V. Dilution Media. VI. Distilled Water.
VII. 0.025N Sodium Thiosulphate (Na2S2O3).

8. Preservation:
Preservation of sample is not practical. Because biological activity will continue after a sample has
been taken, changes may occur during handling and storage. If analysis is to be carried out within
two hours of collection, cool storage is not
necessary. If analysis cannot be started within
two hours of sample collection to reduce the
change in sample, keep all sample at 4oC.

Do not allow samples to freeze. Analysis

should begin as soon as possible. Do not open
sample bottle before analysis. Begin analysis
within six hours of sample collection.

9. Precautions:

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● Make sure there are absolutely no air bubbles in the BOD bottles.

● Perform titration slowly drop-by-drop, noting the color carefully, otherwise the sample
may have to be discarded.

10. Procedure:

● Take eleven 300-mL glass stoppered BOD bottle and fill nine of them with sample to be
tested. Fill three bottles with 2mL of the sample in each (A1, A2 and A3), next three
bottles with 5mL of sample
● In each (B1, B2 and B3), next three bottles with 10mL of sample in each (C1, C2 and
C3) and leave the last two bottles blank (Blank 1 & Blank 2).

● Add dilution media in all BOD bottles to completely fill them up (the dilution media is
added to ensure the bacterial growth so that after 5 days, DO has not been reduced to
zero, rather it should be at least 2 mg/L. Place the stopper on the bottles so as to avoid
any kind of bubbling and trapping of air bubbles. Remember – no bubbles!

● Place all bottles except A1, B1, C1 and Blank 1 in the incubator at 20ᵒC for 5 days
(these samples shall be used later on for the BOD test).

● Determine the 0-day DO of rest of the samples by following the steps below.

● Add 1mL of manganese sulfate to the BOD bottle by using the pipette.

● Add 1mL of Alkali Azide (NaN3) to the BOD bottle by using pipette.

● Formation of brown clouds in the upper region of the bottle indicates that there is some
DO in the sample. If instead white clouds are formed, then this indicates that there is no
DO in the sample and it should be discarded.

● Now place the stopper on the remaining bottles and shake them 20 times each, and allow
the brown ppt. to settle down.

● Now add 1mL of conc. H2SO4 in all samples. Again place the stopper and shake until
all the solution is uniformly colored brown.

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 LAB MANUAL WSE

● Separate the solutions in the four bottles into 2 samples of 200 mL and 100mL from
each of the bottle to have a total of 8 samples.

● Add one of these samples to the titration flask and titrate it against sodium thiosulphate
(0.025N Na2S2O3) until the color changes to light yellow.

● Then add 1 – 2 mL of starch as indicator, this will change the color to blue if the color in
the previous step was light yellow, otherwise the solution will turn to black color.

● Continue titration until the blue color changes to colorless.

● Note the volume of titrant used.

11. Calculations:

DO is calculated by using the formula given below,

𝐷𝑂 (𝑚𝑔𝐿⁄) = 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑖𝑡𝑟𝑎𝑛𝑡 𝑢𝑠𝑒𝑑 ×𝑁 ×𝐸𝑞.𝑤𝑡.𝑜𝑓 𝑜𝑥𝑦𝑔𝑒𝑛 ×1000𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒

𝑢𝑠𝑒𝑑 × F

Where,

N = Normality of sodium thiosulphate solution 𝐹= 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐵𝑂𝐷 𝑏𝑜𝑡𝑡𝑙𝑒−𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓

𝐶h𝑒𝑚𝑖𝑐𝑎𝑙𝑠 𝑎𝑑𝑑𝑒𝑑 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐵𝑂𝐷 𝑏𝑜𝑡𝑡𝑙𝑒

Vol. of Chemical added = 1 mL MnSO4 + 1 mL NaN3 + 1 mL of conc. H2SO4

Repeat steps 11 through 15 for the remaining 100 mL of sample.

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LAB MANUAL WSE

Department of Civil Engineering, COMSATS University Islamabad, Sahiwal Campus - Page 53 of 53