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Environmental Engg. Lab Manual Final PDF
Environmental Engg. Lab Manual Final PDF
Environmental Engg. Lab Manual Final PDF
Program Learning
Outcome: This lab is designed in conjunction with the following PLOs.
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:
List of Experiment
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 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
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).
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
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.
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.
Results
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.
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:
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:
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 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
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
Results
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 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
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
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.
Result
The Conductivity of Sample =
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.
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.
Precautions
Department of Civil Engineering
Environmental Engineering CE- 402
• 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
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.
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
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.
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.
Result
Total Dissolved Solids, ( mg/l ) =
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
• Wash Bottle
• Beakers
Chemicals Required
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.
Observation &Calculations
Formula Used
Total Hardness = EDTA Used (ml) / Sample ( ml)
Result
Total Hardness of Water Sample (mg/1) =
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.
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
• 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.
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) =
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
• 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.
• 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
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
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.
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.
Results
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.
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:
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:
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 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
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.
Results
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.
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.
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
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.
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
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.
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.
Result
Total Dissolved Solids, ( mg/l ) =
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
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
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
Results
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
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
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.
Fill the burette with the ferrous ammonium sulphate solution, adjust to zero and fix
the burette to the stand.
Add few drops of ferrion indicator. The solution becomes bluish green in color.
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.
Add few drops of ferrion indicator. The solution becomes green in colour.
Note down the volume of ferrous ammonium sulphate solution added for the sample
(B) is 13.2 ml.
1 A
2 B
Results
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.
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.).
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 **
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
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
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.
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.
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
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.
Results