Environmental Engg. Lab Manual Final PDF

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Environmental Engineering CE- 402

Program Learning
Outcome: This lab is designed in conjunction with the following PLOs.

PLO 1 Engineering Knowledge: An ability to apply knowledge of


mathematics, science, engineering fundamentals and an engineering
specialization to the solution of complex engineering problems

PLO 6 The Engineer and Society:An ability to apply reasoning


informed by contextual knowledge to assess societal, health, safety,
legal and cultural issues and the consequent responsibilities relevant to
professional engineering practice and solution to complex engineering
problems.

PLO 9 Individual and Team Work: An ability to work effectively,


as an individual or in a team, on multifaceted and /or multidisciplinary
settings.

Lab Learning
Outcome (CLO): Upon successful completion of this Lab, students will be able to:

CLO 3 Performing the different quality parameter tests on water and waste
water samples.
CLO 4 Perform COD, BOD, chloride concentration, hardness, optimum
coagulant dosage in waste water sample.
CLO 5 To respond and present (verbally and in writing) the subject knowledge
based on Lab contents.

Mapping of CLOs to
PLOs and Learning
Domains:

Course Learning Program Learning


Learning Domain
Outcome Outcome
CLO-3 PLO-9 P-2

CLO-4 PLO-6 P-2

CLO-5 PLO-1 A-2

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Environmental Engineering CE- 402

List of Experiment

Sr. No Title CLO’s PLO’s

1 Perform PH Test on given water sample in laboratory using PH meter CLO 3 PLO 9

Perform the Turbidity test on given water sample in laboratory using turbidity
2 CLO 3 PLO 9
meter.

3 Perform the conductivity test on given water sample using conductivity meter. CLO 3 PLO 9

Perform the DO test on given water samples to determine amount of dissolved


4 CLO 3 PLO 9
oxygen.

Perform TDS test on given water samples to determine the amount of total
5 CLO 3 PLO 9
dissolved solids present.

6 Implement EDTA method to determine the total hardness in water CLO 4 PL0 6

7 Perform the Alkalinity test on given water sample. CLO 4 PL0 6

Open End Lab CLO 3 PLO 9


1 Follow the procedure to Collect, Preserve and Storage of waste water sample. CLO 3 PLO 9

2 Perform PH test on given waste water sample using PH meter CLO 3 PLO 9

3 Perform turbidity test on given waste water sample using turbidity meter. CLO 3 PLO 9
Perform DO test on given waste water samples to determine the amount of
4 CLO 3 PLO 9
dissolved oxygen present.

Perform TDS test determine the total solids, total suspended solids in waste water
5 CLO 3 PLO 9
sample.

Perform the Jar Test on given waste water samples to determine the optimum
6 CLO 4 PL0 6
coagulant dosage.

Perform COD test on given waste water samples to determine the Chemical
7 CLO 4 PL0 6
Oxygen Demand (COD).

Perform BOD test on given waste water samples to determine the Biological
8 CLO 4 PL0 6
Oxygen Demand (BOD).

9 Implement the titrimetric method to determine the amount of Sulphide present in


CLO 4 PL0 6
waste water sample.

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Environmental Engineering CE- 402

Experiment No. 1
Perform PH Test on given water sample in laboratory using PH meter.

Definition

PH is the measure of the acidity or alkalinity of a solution. pH has no fundamental meaning as a unit
its official definition is a practical one. pH is a measurement of the concentration of hydrogen ions in
a solution.

pH = Power of hydrogen, H+

Importance

The basic objective of this experiment is to measure the pH of given sample solutions. pH
measurements are important in:

 Medicine
 Biology
 Food science
 Civil Engineering
 Environmental sciences

Acid and Base

Acids have a lot of Hydrogen ions (H+) and bases have a lot of Hydroxide ions (-OH). A solution is
neutral if its pH equals seven.

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PH Meter

A pH meter is an electronic device used for measuring the pH of a liquid. A typical pH meter consists
of a special measuring probe (a glass electrode) connected to an electronic meter that measures and
displays the pH readings.

Procedure

 Sample solutions.
 Glass beakers
 Electronic ph meter

Procedure

 After using of apparatus for various liquids standard solution pH, so in order to
perform next experiment we have to make standard solution pH within neutral range.
 For this purpose buffer solutions are used for neutralization.
 After that, switch on the instrument
 Take the sample whose pH is to be determined
 Now, insert glass electrode probe of the pH meter in the sample solution and wait for
minimum 5 minutes when blinking quotation of stabilizing on the screen of pH meter
stops, note that reading.

Observations and Calculations

SR.No SAMPLE SOLUTION pH READING REMARKS

Results

Conclusion and Comments

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Environmental Engineering CE- 402

Experiment No. 2
Perform the Turbidity test on given water sample in laboratory using turbidity meter.

Definition

Turbidity is a measure of water clarity how much the material suspended in water decreases
the passage of light through the water. Suspended materials include soil particles (clay, silt,
and sand), algae, plankton, microbes, and other substances. These materials are typically in the
size range of 0.004 mm (clay) to 1.0 mm (sand). Turbidity can affect the colour of the water.

Turbidity and Human Health

Excessive turbidity, or cloudiness, in drinking water is aesthetically unappealing, and may also
represent a health concern. Turbidity can provide food and shelter for pathogens. If not
removed, turbidity can promote regrowth of pathogens in the distribution system, leading to
waterborne disease outbreaks, which have caused significant cases of gastroenteritis
throughout the world. The amount and character of turbidity depends upon two things:

 Type of soil over which flows


 The velocity of flowing water

When water becomes stationary, the heavier and larger suspended particles settle down quickly
and the lighter and finely divided particles settles very slowly and even takes months. Ground
water is less turbid because of low velocity of water. turbidity may be helpful for controlling
growth of paganisms by not allowing proper sunlight to water which is necessary for their
growth on the other hand it is harmful as the organisms are handling to the suspended particles.

When water becomes stationary, the heavier and larger suspended particles settle down quickly
and the lighter and finely divided particles settles very slowly and even takes months. Ground
water is less turbid because of low velocity of water. There are various units for the
measurement of turbidity which are:

 Standard turbidity unit[mg/lit or ppm]


 Jackson turbidity unit [J.T.U]
 Nephelometric turbidity unit [N.T.U]

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A device called nephelometric turbidity measures the turbidity of water in N.T.U the intensity
of light after passing through the water gives a measure of turbidity of water.

WHO Guideline Value

WHO suggested a guideline value for turbidity as [N.T.U ] for disinfection the turbidity of
water should be less than 1 N.T.U.

Apparatus

 W.H.O Nephelometric turbidity meter for mazine solution of the sample by


multiplying the scale reading by 0.9 N.T.U, 9 N.T.U, 99 N.T.U
 Test tubes
 Water samples.

Procedure

1. Switch on the power supply and check the battery of the turbidity meter.
2. Press the 1 N.T.U button and coincide the scale with zero by using focusing template.
3. Again press 1 N.T.U button and coincide the scale with zero using the focusing
template.
4. A Standard formazine solution of N.T.U is placed on turbidity meter in the path of
rays and scale is brought 9 n.t.u.
5. The Water sample is taken in a test and is placed in turbidity meter.
6. Use a Cell rise if the turbidity is more than 100 N.T.U and get the turbidity dilution
factor.

Turbidity Range

0 to 5 NTU GOOD (PERFECT FOR DRINKING)

5 to 100 NTU NORMAL TURBIDITY (DRINKABLE)

100 to 300 NTU HIGH TURBIDITY

Above 300 NTU VERY HIGH TURBIDITY (NON-


DRINKABLE)

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Observation and calculations:

S.No SAMPLE TURBIDITY REMARKS


(NTU)
1

Results

Conclusion and Comments

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Environmental Engineering CE- 402

Experiment No. 3
Perform the conductivity test on given water sample using conductivity meter.

Standard
Test procedure is in accordance to:
Methods for Chemical Analysis of Water and Wastes,
EPA-600/4-79-020 US EPA-Method 120.1

Introduction

“Conductivity is a measure of the ability of water to pass an electric current”.

Conductivity in water is affected by the presence of


 In-organic dissolved solids such as chloride, nitrate, sulphate, and phosphate anions
(ions that carry a negative charge)
 Sodium, magnesium, calcium, iron, and aluminium cations (ions that carry a positive
charge)
 Organic compounds like oil, phenol, alcohol, and sugar do not conduct electrical very
well and therefore have a low conductivity when in water.

Conductivity is also affected by temperature:


The warmer the water, the higher the conductivity. For this reason, conductivity is reported as
conductivity at 25 degrees Celsius. Discharges to streams can change the conductivity
depending on their make-up.

Conductivity Units
Conductivity is reported in a unit called a siemen ,or its smaller versions,the milli –Siemen
which is one-one thousandth of a siemen ,and the micro-siemen, which is one millionth of a
Siemen. Conductivity can also be expressed as mhos (reciprocal of ohm)

Apparatus
• Conductivity meter
• Glass Beaker
• Water samples

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Procedure
 Rinse the electrode thoroughly with deionized water and then wipe with a tissue
paper.
 Measure 200 mL of water sample and transfer it to a beaker.
 Then place the beaker on the magnetic stirrer.
 Dip the electrode into the sample solution taken in a beaker and wait for a steady
reading.
 Make sure that the instrument is giving stable reading.
 Repeat the procedure a number of times.
 Note down the reading in the display directly

Observations & Calculations


Sample No. Temperature of Sample Conductivity(µmhu)
1
2
3

Precautions
• Switch on the conductivity meter for at least 30 minutes before starting the experiment
so that the instrument gets stabilizes.
• As conductance is influenced by temperature, always use a conductivity meter with
temperature control.
• Always dip the electrode in distilled water and do not expose it to air.

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Result
The Conductivity of Sample =

Conclusion and comments

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Environmental Engineering CE- 402

Experiment No. 4
Perform the DO test on given water samples to determine amount of dissolved oxygen.

Standard
The given procedure for determining dissolved oxygen is stated in:
Methods for Chemical Analysis of Water and Wastes,
EPA-600/4-79-020, USEPA, Method 360.1

Objective
The Dissolved Oxygen determination is an analytical test in which standardized lab procedures
are used to determine the oxygen concentration of water, wastewater, effluent and polluted
water. These tests will measure the oxygen by means of an optical electrode compared to a
membrane electrode.

Introduction
The term dissolved oxygen is used to describe the amount of oxygen dissolved in a unit
volume of water.
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 presence of oxygen in water is a good sign. Depletion of DO
in water supplies can encourage the reduction of nitrate to nitrite and sulphate to sulphite. It
can also cause an increase in the concentration of ferrous iron.
In a healthy body of water such as lake, river or stream, the DO is about 8 PPM. The
minimum DO level of 4 to 5 mg/1 or ppm is desirable for survival of aquatic life.

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. Highest values of DO may cause
corrosion of iron and steel. 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.

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Environmental Engineering CE- 402

DO Meter
Dissolved oxygen meters give you a way to measure oxygen levels in water. Testing with
portable oxygen meters determines whether or not you have optimal dissolved oxygen levels
necessary for good water quality.

Apparatus
• Electronic DO Meter
• Glass Beakers
• Sample Solutions

Procedure
• Rinse the electrode thoroughly with deionized water and then wipe with a tissue
paper.
• Measure some amount of water sample and transfer it to a beaker.
• Dip the electrode into the sample solution taken in a beaker and wait for a steady
reading.
• Make sure that the instrument is giving stable reading.
• Note down the reading in the display directly. Repeat the procedure many times.

Observations & Calculations


Dissolved Oxygen Temperature Remarks
Sr. No
1
2
3

Precautions
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• Switch on DO meter for at least 30 minutes before starting the experiment so that
instrument get stabilize.
• As DO is influenced by temperature, always use DO meter with temperature control.
• Always dip the electrode in distilled water and do not expose it to the air.

Result

Conclusion and comments

Department of Civil Engineering


Environmental Engineering CE- 402

Experiment No. 5
Perform TDS test on given water samples to determine the amount of total dissolved solids
present.

Objective
This procedure is applicable to waters of wide range of quality including surface water,
industrial water, domestic effluents, treated waste-waters etc. In addition to these samples, this
method can also be applied for the analysis of moisture content in sludge, soil etc.

Introduction
Ordinary water and waste-water, both are the combination of two things:
Pure water + various dissolved and suspended contaminants
The suspended contaminants in turn may be settle-able or non-settle-able. These may be either
organic or in-organic in nature. Strictly speaking, all matter except the water contained in liquid
materials is classified as solid matter.
Total Solids
“It refers to the material residue left in a dish or vessel after evaporating of a sample and its
subsequent drying in an oven at a defined temperature ".
Total solids include total suspended solids and total dissolved solids.

Sampling & Storage


• Obtain an appropriate quantity of sample in glass or plastic bottle.
• If suspended matter adheres to the container walls prefer glass container.
• Analyze sample as soon as possible.
• If preservation required, store it at 4 °C to avoid biological degradation.
• Preferably analyze within 24 hours or within 7 days
• Bring sample to room temperature before analysis.

Apparatus
• Muffle furnace for operating at 550 °C
• Desiccator, Low-form beaker
• Drying oven, for operating at 180 °C
• Analytical balance capable of weighing 0.1mg
• Magnetic stirrer, Wide-mouth pipettes
• Evaporating dishes of 100 mL capacity

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Procedure
• In order to measure total dissolved solids, heat clean dish to 180 °C for 1 hour in an
oven.
• Store and cool the dish in desiccator until needed. Weigh immediately before use.
• Choose sample volume to yield between 2.5 and 200 mg dried residue.
• Pipette a measured volume of well-mixed sample to a pre-weighed evaporating dish.
• Now hold the sample for some time for evaporation.
• Now dry the evaporated sample for at least 1 hour in an oven at 103 to 105 °C.
• Cool in a desiccator to balance temperature and weigh.
• When weighing dried sample, be alert to change in weight due to sample
degradation.

Observations & Calculations


Weight of dried residue and dish (g) = A = Weight of dish (g) = B =
Sample Volume (ml) =

Formula Used

(𝑨 — 𝑩) 𝒙 𝟏𝟎𝟎𝟎
Total Solids, (mg/L) = 𝑺𝒂𝒎𝒑𝒍𝒆 𝑽𝒐𝒍𝒖𝒎𝒆 (𝒎𝒍)

Precautions
• Use gloves while performing the experiment.
• Use glass containers, if matter adheres.
• Analyze the sample as soon as possible.
• Before analysis, bring the sample to room temperature.

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Result
Total Dissolved Solids, ( mg/l ) =

Conclusion and comments

Department of Civil Engineering


Environmental Engineering CE- 402

Experiment No. 6
Implement EDTA method to determine the total hardness in water

Scope
The ions that cause the water to become hard do not pose any health threat, but they can engage
in reactions that leave insoluble mineral deposits. These deposits can make hard water
unsuitable for many uses, and so variety of means have been developed to soften hard water,
i.e. remove the calcium Ca2+ and magnesium Mg2+ ions, which are the principle harness
causing cations. Except that, in fresh waters, the principle hardness causing ions are calcium,
magnesium, strontium, iron, barium and manganese ions also contribute.

Introduction
The water is applied to soap; if it gives lather then it is soft water. But;
"If soap precipitates, when water is applied to it, and does not make enough lather then it is
hard water”
Hard water is the water containing divalent cations with a charge (+2), especially Ca2+, Mg2+,
Mn2+, Fe2+, Sr2+. Normally, hardness is due to Ca2+ and Mg2+.
More degree of ions present in water, the more is the hardness. Due to these ions the water
precipitates soap instead of lather. That's why in hard water more soap is consumed. Minerals
deposits on cooking dishes or rings of insoluble soap scum in bathtub are signs of hard water
from the municipal water supply.
Hardness can be measured by the reaction of polyvalent metallic ions in a water sample with
chelating agent such as EDTA and is commonly expressed as an equivalent concentration of
calcium carbonate hardness can also be estimated by determining the concentrations of the
individual components of hardness and expressing their sum in terms of and equivalent quantity
of calcium carbonate.

Titration Theory
When a small amount of dye EBBT is added to the solution containing hard water, the indicator
forms its complex with metal ions and gives wine red color. But EDTA is capable f forming
more stable with EBBT by the addition of EDTA. EDTA replaces EBBT ions and gain the blue
color of solution is obtained due to free indicator ions.

Apparatus
• Burette with Burette stand and porcelain title
• Pipettes with elongated tips
• Conical flask (Erlenmeyer flask)
• 250 mL Measuring cylinders
• Standard flask

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• Wash Bottle
• Beakers

Chemicals Required

• Standard sulphuric acid


• EDTA, EBT, EBBR, Buffer Solution
• Distilled Water

Procedure
FOR TOTAL HARDNESS
• Take 25 ml of water sample in titration flask.
• Add 25 ml distilled water in it to dilute the water solution (to avoid the formation of
CaCO3). Distilled water does not participate in ion exchange in reaction.
• Add 1-2 ml of buffer solution (Ammonia Buffer NH4C1 + NH4OH) to maintain pH in
solution 7-9.
• Add small amount of EBT (Ecrichrome Black T) as indicator. As a result of addition of
• EBT, solution color changes to wine red.
• Titrate it against O.O1M EDTA solution. Add EDTA from burette until the color
changes to blue.
• Test three samples and determine mean volume of titrant used.
• Total hardness (mg/1) as CaCO3 is calculated using formula.

FOR CALCIUM HARDNESS


• Take 25 ml of water sample in titration flask.
• Add 25 ml distilled water in it to dilute the water sample.
• Add 2-3 ml of NaOH buffer solution.

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• Add small amount of EBBR (Ecrichrome Blue Black R) as indicator. As a result of


addition of EBBR, solution color changes to wine red.
• Titrate it against O.O1M EDTA solution. Add EDTA from burette until the color
changes to blue.
• Test three samples and determine mean volume of titrant used.
• Calcium Hardness (mg/1) as CaCO3 is calculated using formula.

Observation &Calculations

Formula Used
Total Hardness = EDTA Used (ml) / Sample ( ml)

Result
Total Hardness of Water Sample (mg/1) =

Conclusion and comments

Department of Civil Engineering


Environmental Engineering CE- 402

Experiment No. 7
Perform the Alkalinity test on given water sample.

Standard
T0 determine the alkalinity of given water sample with the stipulations as per
IS: 3025 (Part 23) - Reaffirmed 2003

Significance
Alkalinity is important for fish and aquatic life because it protects or buffers againstrapid PH
changes higher alkalinity levels in surface water will buffer acids rain and other acid wastes
and prevent PH changes that are harmful to aquatic life.
The alkalinity acts as a pH buffer in coagulation and softening of water.

"Alkalinity is a measure of the capacity of water to neutralize acids ".


In other words, alkalinity is basically the ability of water to maintain constant PH. Alkaline
compounds in the water such as bicarbonates (baking soda is one type), carbonates, and
hydroxides remove H+ ions and lower the acidity of the water (which means increased pH).
Alkalinity is basically ANC (acid neutralizing capacity). Alkalinity should not be confused
with ph. pH is a measure of the hydrogen ion (H+) concentration, and the pH scale shows the
intensity of the acidic or basic character of a solution at a given temperature,
Whereas alkalinity is measured to figure out how "buffered" the water is against sudden
changes in PH.

Principle
Total alkalinity is measured by titrating (step-wise addition of reagent) the water sample with
Sulphuric acid (H2SO4) to a pH endpoint of 4.5.
Once the water sample reaches a pH of 4.5, the three main forms of alkalinity icarbonate,
carbonate, and hydroxide) have been neutralized.

Apparatus;
Equipment Required:
• Burette with Burette stand and porcelain title
• Pipettes with elongated tips
• Conical flask (Erlenmeyer flask)
• 250 mL Measuring cylinders
• Standard flask

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• Wash Bottle
• Beakers

Chemicals Required;
 Standard sulphuric acid Phenolphthalein
 Mixed Indicator
 Bromocresol Green
 Methyl Orange
 Distilled Water

Procedure
A. PHENOLPHTHALEIN ALKALINITY:
• Rinse the burette with 0.02N Sulphuric acid and discard the solution.
• Fill the burette with 0.02N Sulphuric acid and adjust it to zero.
• Fix the burette in the stand.
• Using a measuring cylinder exactly measure 50 Or100 mL of sample and pour it into a
250 mL of conical flask.
• Add few drops of phenolphthalein indicator to the contents of conical flask.
• The color of the solution will turn to pink. This color change is due to alkalinity of
• Hydroxyl ions in the water sample.
• Titrate it against 0.02N Sulphuric acid till the pink color disappears.

B. METHYL ORANGE ALKALINITY:


 In the same flask, add few drops of methyl orange indicator to the contents of conical
flask.
 The color of the solution will now change. This color change is due to alkalinity of
hydroxyl ions in the water sample.
 3.Titrate it against 0.02N Sulphuric acid till the solution color changes to orange.

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Observations & Calculations


A. PHENOLPHTHALEIN ALKALINITY:

Burette Reading (ml) Volume of


Volume of
Sr, No Sulfuric Acid
Sample (ml) Initial Final
(ml)
1
2
3

B. METHYL ORANGE ALKALINITY:

Burette Reading (ml) Volume of


Volume of
Sr, No Sulfuric Acid
Sample (ml) Initial Final
(ml)
1
2
3

Precautions
• Do not keep the indicator solution open since it contains the alcohol which tends to
Evaporate into the atmosphere.
• The mixed indicator solution is containing dye in it; care should be taken so that it is not
spilled to your skin.
• If it spills on your skin, the scar will remain at least for two to three days.

Result
Average Alkalinity (mg/1) =

Conclusion and comments

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Environmental Engineering CE- 402

Open Ended Lab

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Environmental Engineering CE- 402

Experiment No. 1
Follow the procedure to Collect, Preserve and Storage of waste water sample.

Objective

The objective of sampling is to collect a portion of material small enough in a volume that is
conveniently transported and handled in the laboratory while still accurately representing the
material being sampled.

Introduction

The collection of water samples may seem relatively simple task. However to obtain waste
water sample and to preserve their integrity, it requires a series of steps, procedures and
practices to be performed carefully. This implies firstly that the relative portion of
concentration of all pertinent compounds must be the same in the samples as in the material
being sampled and secondly that the material must be handled in such a way that the significant
change in composition occur before the tests are performed that is why sampling and storage
are critical for accurate analysis.

Apparatus

• Beakers
• Incubator
• Sample bottles

Procedure

Collecting Water Sample

• Obtain the best sample by careful collection in general collect sample ear the counter
or channel and below the surface.
• Raise the container several times first the water to be sampled.
• Most economical sample containers are made of propylene or polyethylene whereas
container made of quartz.

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• Take the sample as close as possible to the sources of supply; let the water run long
enough to flush the system.
• Fill the sample containers slowly with the gentle stream to avoid turbulence and
bubbles.
• Collect the water samples from well.
• Collect the use sample taken at different times from several location and depths.

Precautions

• Use clean beakers for sampling.


• Use poly propylene containers.
• Preserve sample at 4 °C.
• Take sample as close as possible to the source.
• Hold the sample bottle / container carefully.

Conclusion and Comments

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Environmental Engineering CE- 402

Experiment No. 2
Perform PH Test on given Waste water sample in laboratory using PH meter.

Definition

PH is the measure of the acidity or alkalinity of a solution. pH has no fundamental meaning as a unit
its official definition is a practical one. pH is a measurement of the concentration of hydrogen ions in
a solution.

pH = Power of hydrogen, H+

Importance

The basic objective of this experiment is to measure the pH of given sample solutions. pH
measurements are important in:

 Medicine
 Biology
 Food science
 Civil Engineering
 Environmental sciences

Acid and Base

Acids have a lot of Hydrogen ions (H+) and bases have a lot of Hydroxide ions (-OH). A solution is
neutral if its pH equals seven.

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PH Meter

A pH meter is an electronic device used for measuring the pH of a liquid. A typical pH meter consists
of a special measuring probe (a glass electrode) connected to an electronic meter that measures and
displays the pH readings.

Procedure

 Sample solutions.
 Glass beakers
 Electronic ph meter

Procedure

 After using of apparatus for various liquids standard solution pH, so in order to
perform next experiment we have to make standard solution pH within neutral range.
 For this purpose buffer solutions are used for neutralization.
 After that, switch on the instrument
 Take the sample whose pH is to be determined
 Now, insert glass electrode probe of the pH meter in the sample solution and wait for
minimum 5 minutes when blinking quotation of stabilizing on the screen of pH meter
stops, note that reading.

Observations and Calculations

SR.No SAMPLE SOLUTION pH READING REMARKS

Results

Conclusion and Comments

Department of Civil Engineering


Environmental Engineering CE- 402

Experiment No. 3
Perform the Turbidity test on given Waste water sample in laboratory using turbidity meter.

Definition

Turbidity is a measure of water clarity how much the material suspended in water decreases
the passage of light through the water. Suspended materials include soil particles (clay, silt,
and sand), algae, plankton, microbes, and other substances. These materials are typically in the
size range of 0.004 mm (clay) to 1.0 mm (sand). Turbidity can affect the colour of the water.

Turbidity and Human Health

Excessive turbidity, or cloudiness, in drinking water is aesthetically unappealing, and may also
represent a health concern. Turbidity can provide food and shelter for pathogens. If not
removed, turbidity can promote regrowth of pathogens in the distribution system, leading to
waterborne disease outbreaks, which have caused significant cases of gastroenteritis
throughout the world. The amount and character of turbidity depends upon two things:

 Type of soil over which flows


 The velocity of flowing water

When water becomes stationary, the heavier and larger suspended particles settle down quickly
and the lighter and finely divided particles settles very slowly and even takes months. Ground
water is less turbid because of low velocity of water. turbidity may be helpful for controlling
growth of paganisms by not allowing proper sunlight to water which is necessary for their
growth on the other hand it is harmful as the organisms are handling to the suspended particles.

When water becomes stationary, the heavier and larger suspended particles settle down quickly
and the lighter and finely divided particles settles very slowly and even takes months. Ground
water is less turbid because of low velocity of water. There are various units for the
measurement of turbidity which are:

 Standard turbidity unit[mg/lit or ppm]


 Jackson turbidity unit [J.T.U]
 Nephelometric turbidity unit [N.T.U]

Department of Civil Engineering


Environmental Engineering CE- 402

A device called nephelometric turbidity measures the turbidity of water in N.T.U the intensity
of light after passing through the water gives a measure of turbidity of water.

WHO Guideline Value

WHO suggested a guideline value for turbidity as [N.T.U ] for disinfection the turbidity of
water should be less than 1 N.T.U.

Apparatus

 W.H.O Nephelometric turbidity meter for mazine solution of the sample by


multiplying the scale reading by 0.9 N.T.U, 9 N.T.U, 99 N.T.U
 Test tubes
 Water samples.

Procedure

7. Switch on the power supply and check the battery of the turbidity meter.
8. Press the 1 N.T.U button and coincide the scale with zero by using focusing template.
9. Again press 1 N.T.U button and coincide the scale with zero using the focusing
template.
10. A Standard formazine solution of N.T.U is placed on turbidity meter in the path of rays
and scale is brought 9 n.t.u.
11. The Water sample is taken in a test and is placed in turbidity meter.
12. Use a Cell rise if the turbidity is more than 100 N.T.U and get the turbidity dilution
factor.

Observation and calculations:

S.No SAMPLE TURBIDITY REMARKS


(NTU)
1

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Results

Conclusion and Comments

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Experiment No. 4
Perform the DO test on given Waste water samples to determine amount of dissolved
oxygen.

Standard
The given procedure for determining dissolved oxygen is stated in:
Methods for Chemical Analysis of Water and Wastes,
EPA-600/4-79-020, USEPA, Method 360.1

Objective
The Dissolved Oxygen determination is an analytical test in which standardized lab procedures
are used to determine the oxygen concentration of water, wastewater, effluent and polluted
water. These tests will measure the oxygen by means of an optical electrode compared to a
membrane electrode.

Introduction
The term dissolved oxygen is used to describe the amount of oxygen dissolved in a unit
volume of water.
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 presence of oxygen in water is a good sign. Depletion of DO
in water supplies can encourage the reduction of nitrate to nitrite and sulphate to sulphite. It
can also cause an increase in the concentration of ferrous iron.
In a healthy body of water such as lake, river or stream, the DO is about 8 PPM. The
minimum DO level of 4 to 5 mg/1 or ppm is desirable for survival of aquatic life.

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. Highest values of DO may cause
corrosion of iron and steel. 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.

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DO Meter
Dissolved oxygen meters give you a way to measure oxygen levels in water. Testing with
portable oxygen meters determines whether or not you have optimal dissolved oxygen levels
necessary for good water quality.

Apparatus
• Electronic DO Meter
• Glass Beakers
• Sample Solutions

Procedure
• Rinse the electrode thoroughly with deionized water and then wipe with a tissue
paper.
• Measure some amount of waste water sample and transfer it to a beaker.
• Dip the electrode into the sample solution taken in a beaker and wait for a steady
reading.
• Make sure that the instrument is giving stable reading.
• Note down the reading in the display directly. Repeat the procedure many times.

Observations & Calculations


Dissolved Oxygen Temperature Remarks
Sr. No
1
2
3

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Precautions
• Switch on DO meter for at least 30 minutes before starting the experiment so that
instrument get stabilize.
• As DO is influenced by temperature, always use DO meter with temperature control.
• Always dip the electrode in distilled water and do not expose it to the air.

Result

Conclusion and comments

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Experiment No. 5
Perform TDS test on given waste water samples to determine the amount of total dissolved
solids present.

Objective
This procedure is applicable to waters of wide range of quality including surface water,
industrial water, domestic effluents, treated waste-waters etc. In addition to these samples, this
method can also be applied for the analysis of moisture content in sludge, soil etc.

Introduction
Ordinary water and waste-water, both are the combination of two things:
Pure water + various dissolved and suspended contaminants
The suspended contaminants in turn may be settle-able or non-settle-able. These may be either
organic or in-organic in nature. Strictly speaking, all matter except the water contained in liquid
materials is classified as solid matter.
Total Solids
“It refers to the material residue left in a dish or vessel after evaporating of a sample and its
subsequent drying in an oven at a defined temperature ".
Total solids include total suspended solids and total dissolved solids.

Sampling & Storage


• Obtain an appropriate quantity of sample in glass or plastic bottle.
• If suspended matter adheres to the container walls prefer glass container.
• Analyze sample as soon as possible.
• If preservation required, store it at 4 °C to avoid biological degradation.
• Preferably analyze within 24 hours or within 7 days
• Bring sample to room temperature before analysis.

Apparatus
• Muffle furnace for operating at 550 °C
• Desiccator, Low-form beaker
• Drying oven, for operating at 180 °C
• Analytical balance capable of weighing 0.1mg
• Magnetic stirrer, Wide-mouth pipettes
• Evaporating dishes of 100 mL capacity

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Procedure
• In order to measure total dissolved solids, heat clean dish to 180 °C for 1 hour in an
oven.
• Store and cool the dish in desiccator until needed. Weigh immediately before use.
• Choose sample volume to yield between 2.5 and 200 mg dried residue.
• Pipette a measured volume of well-mixed sample to a pre-weighed evaporating dish.
• Now hold the sample for some time for evaporation.
• Now dry the evaporated sample for at least 1 hour in an oven at 103 to 105 °C.
• Cool in a desiccator to balance temperature and weigh.
• When weighing dried sample, be alert to change in weight due to sample
degradation.

Observations & Calculations


Weight of dried residue and dish (g) = A = Weight of dish (g) = B =
Sample Volume (ml) =

Formula Used

(𝑨 — 𝑩) 𝒙 𝟏𝟎𝟎𝟎
Total Solids, (mg/L) = 𝑺𝒂𝒎𝒑𝒍𝒆 𝑽𝒐𝒍𝒖𝒎𝒆 (𝒎𝒍)

Precautions
• Use gloves while performing the experiment.
• Use glass containers, if matter adheres.
• Analyze the sample as soon as possible.
• Before analysis, bring the sample to room temperature.

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Result
Total Dissolved Solids, ( mg/l ) =

Conclusion and comments

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Experiment No. 6
Perform the Jar Test on given waste water samples to determine the optimum coagulant
dosage.

Introduction

Solids can be dispersed in liquids under several forms. The nature of such dispersions depends
on the size of the solid particles.
In general, one the following states are considered:
· Solutions
· Colloidal dispersions
· Suspensions

Wastewaters often contain pollutants that are present is colloidal form


In such cases the colloidal suspension may contain:
 organic materials
 metal oxides
 insoluble toxic compounds
 stable emulsions
 material producing turbidity

This material must be removed prior to discharge. Because of the nature of the colloidal
suspension these particles will not sediment or be separated with conventional physical
methods (such as filtration or settling) unless they are agglomerated through coagulation

Coagulation
Coagulation is the process by which colloidal particles and very fine solid suspensions initially
present in a wastewater are combined into larger agglomerates that can be separated via
sedimentation, flocculation, filtration, centrifugation or other separation methods. Coagulation
is commonly achieved by adding different types of chemicals (coagulants) to the wastewater
to promote destabilization of the colloid dispersion and agglomeration of the resulting
individual colloidal particles The addition of some common coagulants to a wastewater not

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only produces coagulation of colloids but also typically results in the precipitation of soluble
compounds, such as phosphates, that can be present in the wastewater.
In addition, coagulation can also produce the removal of particles larger that colloidal particles
due to the entrapment of such particles in the flocs formed during coagulation The selection of
a coagulant and its dosage cannot be made without carrying out laboratory experiments
Typically two types of tests are the most effective in the determination of the optimal dosage
of coagulant and optimal pH for coagulation. These are:
- jar test
-Zeta Potential

Jar Test
The jar test is the most common laboratory coagulation test and consists of:
 placing a sample of the wastewater in a jar:
 rapidly adding the coagulant and intensely mixing the sample for a short time
(coagulation/destabilization phase);
 allowing the floc to form under gentle mixing conditions (flocculation phase)
 allowing the floc to sediment in the quiescent sample (settling)
 comparing the turbidity of the sample with the initial turbidity
Strategy to Conduct Laboratory
Coagulation Tests
Since two variables (coagulant dosage and pH are) are involved it is typically more
convenient to fix one of the variables initially, scan for the optimal value of the other
variable, and finally scan for the optimal value of the first variable

Apparatus
 Jar test apparatus
 Glass beakers
 Pipette
 Nephelometer
 pH meter

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Jar Test Procedure


A wastewater sample is placed in a beaker and magnetically stirred. The pH must be adjusted
to a desired valued (typically 6);A known amount of coagulant is added and the agitation is
maintained at a high value for 1 minute to promote coagulation. Then the sample is agitated
slowly for 3 minutes to promote flocculation. New additions are made until avisible floc is
obtained; Using this concentration of coagulant the coagulation experiment is now repeated at
different pH values using a longer flocculation time (typically about 10 to 40 minutes),
followed by settling with no agitation (15-60 minutes);The amount of residual pollutant in
solution is measured at the end of each pH experiment. The optimal coagulation pH is obtained;
Using this optimal pH value a new series of experiments is conducted in which the coagulant
dosage is changed. The optimal coagulant dosage is obtained;
Plots of residual pollutant concentration vs. pH and residual pollutant concentration vs.
coagulant dosage can be constructed.

Observations and Calculations

Sr. No Alum Dosage in mg/l Turbidity in NTU

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Results

Conclusion and Comments

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Experiment No. 7
Perform COD test on given waste water samples to determine the Chemical Oxygen
Demand (COD).

Introduction

The chemical oxygen demand (COD) test is commonly used to indirectly measure the
amount of organic compounds in water. Most applications of COD determine the amount
of organic pollutants found in surface water (e.g. lakes and rivers), making COD a useful
measure of water quality. It is expressed in milligrams per liter (mg/L), which indicates the
mass of oxygen consumed per liter of solution.

COD is the measurement of the amount of oxygen in water consumed for chemical
oxidation of pollutants.

COD determines the quantity of oxygen required to oxidize the organic matter in water or
waste water sample, under specific conditions of oxidizing agent, temperature, and time.

This method covers the determination of COD in ground and surface waters, domestic
and industrial wastewaters. The applicable range is 3-900 mg/L.

Environmental Significance:
COD values are particularly important in the surveys designed to determine and control the
losses to sewer systems. The ratio of BOD to COD is useful to assess the amenability of waste
for biological treatment. Ratio of BOD to COD greater than or equal to 0.8 indicates that waste
water highly polluted and amenable to the biological treatment. COD can be treated to TOC,
however, doesnot account for oxidation state of the organic matter. BOD value is always lower
than COD value. For domestic and some industrial wastewater, COD value is about 2.5 times
BOD value.

Apparatus:

 COD Digester
 Burette and Burette Stand
 COD vials with Stand
 250 ml conical flask

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 Pipettes
 Pipette bulb
 Tissue papers
 Wash bottle
 Chemicals:
 Potassium dichromate
 Sulfuric acid
 Ferrous ammonium sulphate
 Silver sulfate
 Mercury sulfate
 Ferrion Indicator
 Organic free distilled water

Procedure

 Take three vials with stopper (two for the sample and one for the blank)

 Add 2.5 ml of the sample to the each of the two COD vials and the remaining COD
is for blank; to this COD blank add distilled water to it

 Add 1.5 ml of potassium dichromate reagent – digestion solution to each of the three
COD vials

 Add 3.5 ml of sulphuric acid reagent – Catylist solution in the same manner

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 Caution: COD vials are hot now

 Cap tubes tightly. Switch on the COD Digester and fix the temperature at 150 Degree
centigrade and set the time at 2 hours

 Place the COD vials into a block digester at 150oC and heat for two hours.

 The digester automatically switches off. Then remove the vials and allow it to cool to
room temperature.

 Meanwhile, get ready with the burette for the titration.

 Fill the burette with the ferrous ammonium sulphate solution, adjust to zero and fix
the burette to the stand.

 Transfer the contents of the blank vial to the conical flask.

 Add few drops of ferrion indicator. The solution becomes bluish green in color.

 Titrate it with the ferrous ammonium sulphate taken in the burette.

 End point of the titration is the appearance of the reddish brown color.

 Note down the volume of ferrous ammonium sulphate solution added for the blank
(A) is 14.1 ml.

 Transfer the contents of the sample vial to conical flask.

 Add few drops of ferrion indicator. The solution becomes green in colour.

 Titrate it with ferrous ammonium sulphate taken in the burette.

 End point of the titration is the appearance of reddish brown colour.

 Note down the volume of ferrous ammonium sulphate solution added for the sample
(B) is 13.2 ml.

Observations and Calculations


For determining COD in a given sample, the readings should be tabulated.

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Sr.No Sampl Volume of Initial Final Vol of 0.1N


e sample (mL) reading reading FAS (mL)
(mL)
(mL)

1 A

2 B

COD =( A – B x N x 8 x 1000 ) / Vol of sample

Results

Conclusion and Comments

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Environmental Engineering CE- 402

Experiment No. 8
Perform BOD test on given waste water samples to determine the Biochemical Oxygen
Demand (BOD).

Introduction

In the presence of free oxygen, aerobic bacteria use the organic matter found in wastewater as
“food”. The BOD test is an estimate of the “food” available in the sample. The more “food”
present in the waste, the more Dissolved Oxygen (DO) will be required. The BOD test
measures the strength of the wastewater by measuring the amount of oxygen used by the
bacteria as they stabilize the organic matter under controlled conditions of time and
temperature.
The BOD test is used to measure waste loads to treatment plants, determine plant efficiency
(in terms of BOD removal), and control plant processes. It is also used to determine the effects
of discharges on receiving waters. A major disadvantage of the BOD test is the amount of time
(5 days) required to obtain the results.
When a measurement is made of all oxygen consuming materials in a sample, the result is
termed “Total Biochemical Oxygen Demand” (TBOD), or often just simply “Biochemical
Oxygen Demand” (BOD). Because the test is performed over a five day period, it is often
referred to as a “Five Day BOD”, or a BOD5.
In many biological treatment plants, the facility effluent contains large numbers of nitrifying
organisms which are developed during the treatment process. These organisms can exert an
oxygen demand as they convert nitrogenous compounds (ammonia and organic nitrogen) to
more stable forms (nitrites and nitrates). At least part of this oxygen demand is normally
measured in a five day BOD.
Sometimes it is advantageous to measure just the oxygen demand exerted by organic
(carbonaceous) compounds, excluding the oxygen demand exerted by the nitrogenous
compounds. To accomplish this, the nitrifying organisms can be inhibited from using oxygen
by the addition of a nitrification inhibitor to the samples. The result is termed “Carbonaceous
Biochemical Oxygen Demand”, or CBOD.

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Safety and Hygiene

When testing for BOD, the concerns for safety involve wastewater hazards and exposure to
chemicals.
Precautions to follow include the following:

 Cover all abrasions and wear good quality latex gloves when in direct contact with raw
wastewater.
 Wash hands frequently, and always wash hands prior to eating or smoking.
 Clean up all spills of wastewater or buffers immediately.
 Wear a protective smock, apron, or lab coat, and surgical or rubber gloves when
working in the laboratory to protect clothes and skin.
 Read all labels carefully and know what to do in case of a spill.
 Always use a pipette bulb. NEVER pipette anything by mouth.
 Always pour acids or bases into water, never add water to the acid or base. Mixing
concentrated acids or bases with water can create a significant amount of heat.
 Use care when handling sharps (broken glass etc.).

BOD Description Of Method


A sample is pipetted into a BOD bottle containing aerated dilution water. The DO content is
determined and recorded and the bottle is incubated in the dark for five days at 20°C. At the
end of five days, the final DO content is determined and the difference between the final DO
reading and the initial DO reading is calculated. The decrease in DO is corrected for sample
dilution, and represents the biochemical oxygen demand of the sample.

Section 8: Equipment and Reagent

Test reagents are as follows:


 Phosphate buffer solution
 Magnesium sulfate solution (MgSO4 7H2O) *

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 Calcium chloride solution (CaCl2) *


 Ferric chloride solution (FeCl3) *
 Sodium hydroxide (NaOH), 1 N *
 Sulfuric acid (H2SO4), 1 N *
 Sodium sulfite (Na2SO3), 0.025 N
 Potassium iodide solution (KI), 10%
 Acetic acid solution (CH3CO2H), (1+1) *
 Sulfuric acid solution (H2SO4), (1+50) *
 Starch indicator solution
 Glucose-glutamic acid solution
 Nitrification inhibitor (2-chloro-6-(trichloromethyl) pyridine) *
 Distilled water

Equipment
 BOD meter with probe for measurement of dissolved oxygen in 300 mL BOD bottles
 300 mL BOD bottles
 Incubator, capable of maintaining 20 +/- 1°C
 250 mL graduated cylinders
 100 mL graduated cylinders
 25 mL measuring pipettes (wide-mouth)
 10 mL measuring pipettes (wide-mouth)
 100 mL beaker
 1000 mL beaker
 250 mL Erlenmeyer flask
 Burette graduated to 0.1 mL
 Dilution water bottle of suitable volume for the number of tests to be performed
 Pipette bulb
 Equipment for pH measurements **
 Magnetic stirrer and stirring bars **

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Determination Of Sample Size


The BOD test relies on a measurable depletion of DO over a specified period of time. Because
most samples of wastewater will have a BOD higher that the amount of oxygen available in
the BOD bottle during the incubation period, the samples must be diluted. This dilution is done
by adding dilution water to the sample in the BOD bottle. If the sample is not diluted, the
biological activity of the microorganisms will use up the DO in the BOD bottle before the five
day incubation time is up. If the final DO is too low, the BOD cannot be determined. There is
no way of knowing at what point during the five days the DO reached zero.
One of the most difficult steps in the BOD procedure is deciding how much sample to place in
the BOD bottles for incubation. Some plants have influent and effluent BOD’s that do not vary
greatly over time, while others fluctuate greatly from day to day. In all cases, several different
dilutions of each sample should be prepared to obtain the desired DO depletions. Once a general
range for the BOD of a sample has been determined, the dilutions can be established which
will ensure that at least one dilution will meet the criteria for valid BOD results. The following
procedure can be used to calculate volumes for sample dilution from the estimated BOD.

A. mL sample added to BOD bottle = (minimum allowable depletion, mg/L x Volume of


BOD bottle, mL)/estimated BOD, mg/L

Example:
Minimum mL sample = [(8 mg/L - 6 mg/L) x 300 mL]/400 mg/L
Minimum mL sample = (2 x 300)/400 = 600/400 = 1.5 mL

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B. mL sample added to BOD bottle = (maximum allowable depletion, mg/L x Volume of


BOD bottle, mL)/estimate
BOD, mg/L

Example:
maximum mL sample = [(8 mg/L - 1 mg/L) x 300 mL]/400 mg/L
maximum mL sample = (7 x 300)/400 = 2100/400 = 5.25 mL

Since the BOD value used is only an estimate, and BOD bottles do not always have a volume
of exactly 300 mL, several bottles with different volumes of sample are set up to ensure that
test requirements are met. For the examples above, four bottles would be used with 1 mL, 3
mL, 4 mL, and 6 mL, and the results averaged for the final BOD.

NOTE: Those sample dilutions which deplete less than 2 mg/L, or have a final DO of less
than 1 mg/L would not be used in the calculation of the average sample BOD.
Laboratory Procedure

 Completely fill two BOD bottles with dilution water.


 Into additional BOD bottles, partially filled with dilution water, carefully measure out
the proper volume of sample. Add dilution water until the bottles are completely filled.

NOTE: If the modified Winkler procedure is to be used for DO measurements, two BOD
bottles should be prepared for each dilution; one for determination of the initial DO and one
for incubation and final DO measurement. If the meter method is used for DO measurements
the initial and final DO determinations can be performed on the same bottle.

ADDITIONAL NOTE: If the nitrification inhibition is to be used to determine the


carbonaceous BOD fraction (CBOD) of the sample, a separate dilution series of uninhibited
sample can be prepared to determine the combined nitrogenous and carbonaceous BOD for the
sample. To inhibit the nitrifying bacteria in the sample, add 3.33 mg of nitrification inhibitor

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to one set of sample dilutions, while the second set of dilutions remains untreated. Continue
with the remaining procedural steps with both sets of dilutions.

 Stopper each bottle taking care to avoid trapping air bubbles inside the bottles as the
bottle stoppers are inserted.
 Fill the top of each bottle neck around the stopper with dilution water.
 Determine the initial DO content on one of each set of duplicate bottles, including the
dilution water blank by one of the approved methods and record data on the lab sheet.
 Place the remaining bottles in the incubator at 20°C and incubate for five days.
 At the end of exactly five days (+/-3 hours), test the DO content of the incubated bottles.
 Calculate the BOD for each dilution. The most accurate BOD will be obtained from
those dilutions that have a depletion of at least 2 mg/L DO and at least 1.0 mg/L DO
residual. If there is more than one dilution that meets these criteria, the BOD results
should be averaged to obtain a final BOD value.
 The dilution water blanks are used only to check the quality of the dilution water. If
the quality of the water is good and free from impurities, the depletion of DO should be
less than 0.2 mg/L. In any event, do not use the depletion obtained as a blank correction.
 If nitrification inhibition is used, the BOD test must also be performed on a series of
sample dilutions which have not been inhibited.
 Report the results of the nitrification inhibited samples as CBOD5 and uninhibited
samples as BOD5.

Observations And Calculations

Sample No Concentration Initial DO (D1) Final DO (D2) BOD5 mg/l

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BOD value in mg/l = ( D1 – D2 ) / P


Where, D1= initial dissolved oxygen
D2= Dissolved oxygen at the end of 5 days
P= Volume of sample used
To determine the value of the BOD in mg/L, use the following formula:

BOD, mg/L = [(Initial DO - Final DO) x 300]/mL sample


For example:
Initial DO = 8.2 mg/L
Final DO = 4.4 mg/L
Sample size = 5 mL
BOD mg/L = [(8.2 - 4.4) x 300]/5 = (3.8 x 300)/5 = 1140/5 = 228 mg/L

Whenever a sample is dechlorinated, it must be seeded. If the sample is seeded, a correction


factor must be calculated to determine the effects that the seed material has on the DO
depletion. A number of BOD’s must be run on the seed material to determine the seed
correction factor.

Interferences
Since the BOD test is dependent on biological activity, the major interferences will be those
substances which inhibit the growth of the microorganisms. These will include chlorine,
caustic alkalinity or acidity, mineral acids, and heavy metals (such as copper, zinc, chromium,
and lead).
Excessive nitrites can interfere with the BOD determination. Growth of algae in the presence
of light can cause problems by actually increasing the DO of the sample before testing, which
must be removed by deaeration.

Results

Conclusion and Comments

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Experiment No. 9
Implement the titrimetric method to determine the amount of Sulphide present in waste
water sample.

Introduction
Sulphides often occur in ground water especially in hot springs, in wastewater and polluted
waters. Hydrogen sulphide escaping into the air from sulphide containing wastewater causes
odour nuisance. It is highly toxic and cause corrosion of sewers and pipes. Sulphides include
H2S and HS– and acid soluble metallic sulphides present in the suspended matter. Iodine reacts
with sulphide in acid solution, oxidising it to sulphur; a titration based on this reaction is an
accurate method for determining sulphides at concentration above 1mg/L if interferences are
absent and if loss of H2S is avoided.
Apparatus
 Burette
 Pipette
 Erlenmeyer flask.
Reagents
 Hydrochloric acid
 Standard iodine solution (0.025N)
 Standard sodium thiosulphate solution (0.025N)
 Starch solution
Procedure
 Measure from a burette 10mL of iodine into a 500 mL flask.
 Add distilled water and bring the volume to 20 mL.
 Add 2 mL of 6 N HCl.
 Pipette 200 mL sample into the flask, discharging the sample under the surface of
solution.
 If the iodine colour disappears, add more iodine so that the colour remains.
 Titrate with sodium thiosulphate solution, adding a few drops of starch solution, as the
end point is approached and continuing until the blue colour disappears.

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Observation and Calculations

Sample No Vol of Iodine Vol of Sodium Vol of sample Sulphide mg/l


Thiosulphate

mg/L sulphide = 400 (a – b)/ml of sample

Where; a = mL 0.025 N iodine used


b = mL 0.025 N sodium thiosulphate solution used.

Results

Conclusion and Comments

Department of Civil Engineering

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