Abidali Maner TY A
Abidali Maner TY A
Abidali Maner TY A
INDEX
Subject: Environmental Engineering - II Class: TY A
Roll No: 21 Exam. No:
3 Determination of Solids 9 – 13
Certificate
This is certify that Mr. Abidali Asgarali Manner of TY. Civil class A has completed the
above mentioned Experiments in the subject Environmental Engineering - II in the D. Y.
Patil College of Engineering& Technology, Kasaba Bawada, Kolhapur in year 2019-20.
Date _____________________
2 Determination of 9/6/2021
Alkalinity
3 Determination of
Solids
4 Determination of Oil 16/6/2021
& Grease
5 Determination of 30/6/2021
Dissolved Oxygen
(D.O.)
6 Determination of 16/6/2021
Chloride content
7 Determination of 30/6/2021
Biochemical oxygen
Demand (B.O.D.)
8 Determination of 23/6/2021
Chemical Oxygen
Demand (C.O.D.)
Students shall read the points given below for understanding the theoretical concepts
and practical applications.
3. Organize the work in the group and make a record of all observation.
5. Student should not hesitate to ask any difficulty faced during conduct of
practical/exercise.
6. The student shall study all the questions given in the laboratory manual and
practice to write the answers to these questions.
8. Students shall attempt to develop related hands-on skills and gain confidence.
9. Student shall develop the habit of evolving more ideas, innovations skills etc. than
included in the scope of the manual.
10. Students should develop the habit of not to depend totally on teachers but to
develop self learning techniques.
11. Students should develop habits to submit the practical’s exercise continuously and
progressively on the scheduled dates and should get the assessment done.
Experiment No. 1
Date:
Experiment No. 1
Aim: To determine pH from given wastewater by pH paper method, colorimetric method and
electrometric method
Apparatus: pH paper strip, measuring cylinder, test tube, pipette, beaker etc
Principle:
pH is the measure of intensity of acidity or alkalinity and measure the concentration of H +
ions in the water sample. It doesn’t measure total acidity or alkalinity. In fact the normal
acidity or alkalinity depends upon excess of H+ or OH – ions over the other and measure the
normally or gm equivalent or acid or alkali. If free H + ions are more than OH – ions the water
shall be acidic or alkaline the other way round.
pH value of water indicates the H+ ions concentration in water. pH is expressed as a
logarithm of reciprocal of H+ ion concentration in moles / lit at a given temp. The pH scale
ranges from 0 (acidic) to 14 (very alkaline) with 7 corresponding to exact neutrality at 25 ˚C.
pH is measured using pH meter which comprises of a detecting unit consisting of a glass
electrode, reference electrode usually a calomel electrode connected by KCL bridge, to the
pH sensitive glass electrode and an indicating unit which indicate the pH corresponding to
the electromotive force is then detected.
Procedure:
I) pH paper method:
● Take sufficient quantity of waste water in beaker
● Dip the pH paper strip in sample for 1 or 2 sec and remove from sample
● Observe the colour and compare with colour code on pH paper strip
● Note down the reading (Observation)
II) Colorimetric method:
● Take 10 ml water sample in test tube
● Add 0.2 ml of 1-2 drops of universal indicator
Observations:
Sample Method pH value Nature
Apparatus Required:
Result:
Conclusion:
According to CPCE PH of waste water should be between 5.5 to 9 As the given waste
water sample has PH between 6.5 to 7 , so it is within limt .Hence it is suitable for use
like gradening,tec.
Significance:
1. The pH test is important preliminary parameter for various water treatment and waste
water treatment units
2. pH analysis are important for neutralization precipitation , coagulation , softening of
water is controlled by pH adjustments.
3. Disinfection, coagulation, softening of water is controlled by pH adjustments.
4. Higher pH level in water results in the formation of trihalomethanes which is a major
reason for causing cancer in humans.
As per general standard for discharge of environmental pollutants in inland surface water,
public sewer, land irrigation and coastal area the given standard for waste water discharge
range is 5.5 – 9.0
Experiment No. 2
Date:
Experiment No. 2
Apparatus: Burette with stand, conical flask, measuring cylinder, pipette, etc.
Principle:
1. Alkalinity of water is its capacity to neutralize a strong acid and is characterized by the
presence of all hydrogen ions capable of combining with hydrogen ions
2. Weak acids and strong bases due to free hydroxyl ions and hydrolysis of the same form
alkalinity in natural water
3. When a salt of weak acid and strong base, the weak acid is unable to dissociate more and
when the titration is carried out with a strong acid the equilibrium is shifted to the right
and all salt is hydrolyzed
4. The no. of milli equivalent of acid used in the titration to combine all the hydroxyl ions is
called “Total alkalinity”
5. Phenolphthalein alkalinity can be determined at pH 8.3 by using Phenolphthalein
indicator and total alkalinity can be determined by adding strong acid like HCL or H 2SO4
to pH 4.5
Procedure:
A] Phenolphthalein alkalinity:
1. Take 50 ml sample in conical flask and add 2-3 drops of Phenolphthalein indicator in it
and observe the colour
2. If remain colourless the Phenolphthalein alkalinity is absent, if turns pink then titrate it
with 0.1 N H2SO4 solution and end point is pink to colourless
3. Take 3 burette readings
B] Total alkalinity:
1. Take 50 ml sample in conical flask and add 2-3 drops of methyl orange indicator in it and
observe the colour
2. If red colour appears total alkalinity is absent if yellow colour appears then titrate it with
0.1 N H2SO4 solution and end point is yellow to red
3. Take 3 burette readings.
Observations:
Sample Volume of Burette reading
Type of Alkalinity M.B.R
Code sample I II III
Calculation:
A] Phenolphthalein Alkalinity= M.B.R.*N of H2SO4*eq.wt. of CaCO3*1000
(mg/l of CaCO3) Volume of sample (ml)
Result:
The given sample has alkalinity
Sample A: Phenolphthalein alkalinity = absent
Total alkalinity =130 mg/l
Conclusion:
As per IS Standard the alkalinity of given waste water sample should be
below 200mg/l. As the given waste water sample having total alkalinity as 130mg/l.
which is lesser than standard limit.Hence, it is suitable disposal.
Significance:
1. Alkalinity is important for aquatic organisms because alkalinity protects them against
rapid change in pH
2. It gives buffering capacity to water and protects water against sudden change in pH
3. Permissible limit for drinking as per IS standard is 200 mg/lit. Beyond this limit taste
becomes unpleasant and such water needs to be treated
4. Alkalinity is due to rocks , salts, soil and certain industrial waste water discharge
5. If alkalinity is higher it results in high T.D.S which increases load on filtration unit
6. High TDS also result in sludge formation and gives scaling in pipe line
7. Alkalinity is important in corrosion control slightly alkaline water are less corrosive than
acidic water in the distribution system
Experiment No. 3
Determination of Solids
Date:
Experiment No. 3
Aim: To Determination Total Solids, Total Dissolved Solids and Total Suspended Solids
from given waste water sample
Apparatus: Crucible, hot air oven, weighing balance, Whatman filter Paper No 42, funnel
etc
Principle:
Solids are determined by gravimetric analysis. Various types of solids are determined as
follows:
1. Total solids are determined by evaporating a known volume of the sample to dryness and
weighing the residue
2. Dissolved solids are determined by filtering a known volume of the sample, evaporating
the filtrate to dryness and weighing the residue
3. Fixed solids are determined by volatilizing away all the organic matter in a known
volume of the sample and weighing the residue
4. Settle able solids are determined by allowing coarse suspended solids, with specific
gravity greater than 1, to settle under still conditions over a specific period of time. The
settled sludge is evaporated to dryness and the residue is weighed to determine the
efficiency of sedimentation
Procedure:
A] Total Solids (TS)
i.) Weigh and clean empty crucible (A)………….. W1 mg
ii.) Take a measured volume of the waste water sample in (A), say 25 ml if the sample
appears strong, 50 ml if it appears moderately strong and 100 ml if it appears weak and
evaporates to dryness in a hot air oven at 103˚ 105˚ C
iii.) Cool the crucible to room temperature and weigh ………… W2 mg
TS mg/l = {(W2 – W1) mg ×1000(ml/l)}/Volume of sample taken (ml)
ii.) Take a known volume of the sample, filter it through Whatman filter paper no. 40 and
collect the filtrate (B) as above
iii.) Evaporate the filtrate in (B) to dryness in a hot air oven at 103˚C. Cool the crucible to
room temperature and weigh…………. W4 mg
TDS mg/l = {(W4- W3) mg × 1000 (ml/l)}/Original Volume of sample taken (ml)
Observations:
Weight of crucible
Sample Code Test
Initial wt. Final wt.
Calculation:
A] T.S.mg/l = {(W2- W1) mg ×1000 (ml/l)}/Volume of sample taken (ml)
Conclusion:
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Experiment No.4
Date:
Experiment No.4
Aim: To determine oil and Grease from given waste water sample by separating funnel
method
Apparatus: Separating funnel with stand, evaporating dish, weighing balance, hot plate,
pipette, beaker, measuring cylinder etc.
Reagents: Petroleum ether, Sulphuric acid or HCL, ethyl alcohol i.e. laboratory solvent
Theory:
This method includes the measurement of ether extractable matter from surface and saline
water, industrial and domestic waste. It is applicable to the determination of relatively
nonvolatile hydrocarbons, vegetables, oils, animal fats, waxes, soaps, greases and related
matter.
The term grease applies to the wide variety of organic substances that is extracted from
aqueous solution. Hydrocarbons, oil, fats, waxes and higher molecular weight fatty acids are
the major material dissolved by petroleum ether or hexane. All these materials have a greasy
feel and are associated with the petroleum of water.
Principle:
The method is applicable to measurement of light hydrocarbons that volatilize at temperature
below 70˚C. The sample is acidified to a low pH 2 and serially extracted with petroleum
ether in separating funnel. The solvent is evaporated from the extract and residue weighted.
Procedure:
1) Take 250 ml waste water sample in separating funnel and add 2- 3 ml lab solvent
2) Add 1-2 ml of 1: 1 H2SO4 to separating funnel and shake well
3) Add 10 ml petroleum ether to separating funnel and shake it again
4) Two layers will be formed
5) Discard the lower layer of water
6) Transfer the upper layer carefully in previously weighted crucible
7) Keep this crucible for heating on hot plate at 70˚C
8) After evaporating of solvent take final wt. of crucible
Observations:
Volume of sample Initial wt. of crucible Final wt. of crucible
Sample Code
(ml) (gm) (gm)
Calculations:
Oil and Grease (mg/lit) = {[(Final weight) – (Initial weight)] ×1000}/ volume of sample
={[(27.738*10^3) - (27.68*10^3)]*1000}/250
= 232 mg/lit.
Result:
Oil and Grease content of the given waste water sample is 232 mg/l.
Conclusion:
As per CPCB norms oil & grease limit of waste water should be below 20 mg/lit. for
disposal of waste water in the land surface water, land of irrigation, marine/ costal
areas. So we conclude that the available waste water sample is not safe for disposal &
should be given proper treatment before disposal.
Significance:
1) The main sources of oil and grease in the water body are domestic waste, industrial
waste, accidental leakage of ships, ballast water, sewage, hotel waste containing oily
components within it, greases and servicing centers
2) If they are disposed of without any treatment in the water bodies, shows advance effects
on aquatic ecosystem
3) It forms layer at surface of water body and reduces light penetration and different
atmospheric gases in water
4) Oil accumulates on the gills of fishes and affects respiration
5) For the treatment of oil and grease in water body we can use genetically species. They
degrade the oil and grease
6) As per IS standard for discharge of oil and grease in
Apparatus required:
Experiment No: 5
Date:
Experiment No: 5
Aim: To determine Dissolved Oxygen (D.O.) from given water sample by Wrinkler’s
Iodometric method.
Apparatus: 300 ml BOD stopper bottle, burette, pipette, conical flask, measuring cylinder,
etc.
Reagents:
Manganese Sulphate solution (MnSO4), Alkali Iodide Azide solution (KI+KOH), Conc.
H2SO4 solution, Starch indicator, 0.025 N Sodium Thiosulphate solution (Na2S2O3)
Theory:
The term DO 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 ability of
water to sustain aquatic life. The content of water is influenced by the source, raw water
temperature, treatment and chemical or biological processes taking place in the distribution
system. The presence of oxygen in water is a good sign. Depletion of DO in water supplies
can encourage the microbial reduction of nitrate to nitrite and sulphate to sufide. It can also
cause an increase in the concentration of ferrous iron in solution, with subsequent
discoloration at the tap when the water is aerated.
Principle:
The Manganese sulphate reacts with the alkali to form a white precipitate of Manganese
hydroxide, which in the presence of oxygen gets oxidized to a brown color compound. In the
strong acid medium manganic ions are reduced by iodide ions which get converted in to
iodine equivalent to the original concentration of oxygen in the sample. The iodine can be
titrated against sodium thiosulphate using starch as an indicator.
MnSO4 + 2KOH 🡪 Mn(OH)2 ….white ppt + K2SO4
2Mn(OH)2 + O2 🡪 2MnO(OH)2 Brown ppt
MnO(OH)2 + H2SO4 🡪 MnSO4 + 2H2O + [O]
2KI + H2SO4 + [O] 🡪 K2SO4 + H2O + I2
I2 + I 🡪 I3
2S2O3 + I3 🡪 3I + S4O6
Procedure:
1) Fill the sample in a glass stopper bottle (BOD bottle) of known volume (300ml) by
carefully avoiding any kind of bubbling and trapping of air bubble in the bottle.
2) Pour 2 ml of each Manganese sulphate and alkaline potassium iodide solution, well below
the surface and away from walls.
3) Place the stopper and shake the contents well by inverting the bottle repeatedly. Keep the
bottle for some time to settle down the precipitate.
4) If titration is to be prolonged for few days, keep the sample at the stage with the
precipitate.
5) Add 2 ml. concentrated H2SO4 acid and shake well to dissolve the precipitate.
6) Take 100 ml. sample from bottle in a conical flask for titration.
7) Add 1 ml. starch indicator in it.
8) Titrate it with 0.025 N Na2S2O3 solution within one hour of dissolution of precipitate.
9) End point is blue to colorless. Take three burette readings.
Observation table:
Sample Volume of Burette Reading(ml)
Sr. No. M.B.R.
code sample (ml) I II III
Calculations:
Dissolved Oxygen= M.B.R*N of Na2S2O3*at.no. ofoxygen*1000
(mg/l) (Volume of sample)
i) Dissolved oxygen = 8.3 x 0.025 x 8 x 1000 / 203
for wastewater
= 8.17Mg/lit
Result:
The Dissolved oxygen of the given waste water sample is 8.17mg/l and for Aquaguard is
9.45mg/l.
Conclusion:
Significance:
1) The natural sources of DO in aquatic body are atmospheric diffusion and photosynthesis
activities of aquatic plants.
2) DO plays very important role in survival of aquatic life. If DO depletes then the anaerobic
conditions develops in water body, which results in Eutrophication of water body, which
gives foul odor to water body.
3) High DO level in a community water supply are good because it makes drinking water
taste better.
4) High DO level speed up corrosion in water pipes.
5) Low DO level indicates an excessive demand on the oxygen of the system.
Diagram:
Experiment No. 6
Date:
Experiment No: 6
Apparatus: Burette with stand, conical flask, measuring cylinder, pipette, etc.
Reagents:
0.02 Silver Nitrate solution (AgNO3), Potassium chromate indicator (K2CrO4)
Introduction:
Chloride content of water is due to salts of calcium, potassium and sodium. In potable water
the salty taste produced by chloride concentration is variable and dependent on the chemical
composition of water. The major taste producing salts in water are NaCl and CaCl 2. In some
water which is having only 250 mg/l of chloride may have a detectable salty taste if the
cation (positively charged) present in the water is sodium. On the other hand a typical salty
taste may be absent even if the water is having very high chloride concentration for example
1000mg/l.
Sources:
1) River stream beds with salt containing minerals.
2) Runoff from salted roads.
3) Mixing of sea water with fresh water.
4) The use of water softeners.
5) Irrigation water returned to stream.
6) Chlorinated drinking water, food processing industries, sewage discharge, urinary excreta,
etc.
Principle:
The principle is based on Mohr method where precipitating agent is silver nitrate. The
amount of chloride present in water can be easily determined by titrating the given water
sample with silver nitrate solution.
The silver nitrate reacts with chloride ion according to 1 mole of silver nitrate reacts with 1
mole of chloride. The titrant concentration is generally 0.02M. Silver chloride is precipitated
quantitatively before red silver chromate is formed. The end of titration is indicated by
formation of red silver chromate from excess silver nitrate. The results are expressed n mg/l
of chloride (Cl- with a molecular weight of 35.453 g/mol).
This method of titration using silver ions is known as Mohr’s Argentomertic titration method.
Procedure:
1) Take 100 ml water sample in conical flask by using measuring cylinder.
2) Add 1 ml of potassium chromate solution in it.
3) Titrate it with 0.02 N Silver nitrate solution.
4) End point is yellow to brick red color.
5) Take 3 burette readings.
Observation table:
2 B
Calculations:
Chloride content = M.B.R*N of AgNO3*at.wt. of Chloride*1000
(mg/l) Volume of sample (ml)
= 73.74 mg/lit.
Result:
The chloride content of the given water sample is 73.74 mg/l.
Conclusion:
As per CPCB norms chloride limit of wastewater should be below 250mg/lit. For
disposal of waste water in the land surface water, land og irrigation, marine/coastal
areas. So we conclude that the available waste water is safe for disposal.
Significance:
1) Permissible limit for chloride in drinking water is 250 mg/l. But in absence of alternate
limit can be extended up to 1500 mg/l.
2) Chloride containing water can corrode concrete. Magnesium Chloride in water generates
HCl after heating, which is also highly corrosive and creates problem in boilers.
3) Chloride determination is used to determine the type of desalting apparatus to be used.
4) Chloride determination is used to control pumping of ground water from location where
intrusion of sea water is problem.
5) Chloride interferes in the determination of C.O.D.
6) High value of chloride in water is due to pollution of water from human sewage, animal
manure or industrial waste.
7) Limit for chloride for construction is, for R.C.C.-500 mg/l and for P.C.C.-1000 mg/l
8) Limit for chloride for irrigation is 355 mg/l.
9) If high chloride containing water is used for irrigation, it increases soil salinity. Remedy
for soil salinity is addition of Gypsum.
NaCl is important chloride salt for human body. It is dietary mineral, partially responsible for
nerve function. If consumed in excess, results in high BP, arteriosclerosis, oedema, etc. If
shortage, leads to dehydration, convulsion, muscle paralysis, etc.
Diagram:
Experiment No. 7
Date:
Experiment No. 7
Aim: To determine Biochemical Oxygen Demand (B.O.D.) from given waste water sample.
Apparatus:
BOD bottles (capacity 300 ml), B.O.D. Incubator, burette, pipettes, conical flask, burette
stands, tile, measuring cylinder, glass rod, beakers.
Reagents:
Manganese Sulphate solution, Alkali Iodide Azide, Conc. H2SO4, Starch indicator, 0.025 N
Sodium Thiosulphate solution, Organic free distilled water.
Nutrients-Phosphate Buffer, Magnesium Sulphate, Calcium Chloride, Ferric Chloride,
Theory:
The Biochemical Oxygen Demand (BOD) is an empirical standardized laboratory test which
measures oxygen requirement for aerobic oxidation of decomposable organic matter and
certain inorganic materials in water, polluted waters and wastewater under controlled
conditions of temperature and incubation period. The quantity of oxygen required for above
oxidation processes is a measure of the test. The test is applied for fresh water sources
(rivers, lakes), wastewater (domestic, industrial), polluted receiving water bodies, marine
water (estuaries, coastal water) and also for finding out the level of pollution, assimilative
capacity of water body and also performance of waste treatment plants.
BOD of water or polluted water is the amount of oxygen required for the biological
decomposition of dissolved organic matter to occur under standard condition at a
standardized time and temperature. Usually, the time is taken as 5 days and the temperature
is 20˚C
Principle:
A known volume of a sample of wastewater, diluted using specially prepared distilled water,
is incubated at 20oC for 5 days (or at 27oC for 3 days). DO depletion in the test bottle is a
measure of fair amount of bio-degradable organic matter present in the sample. To avoid
getting zero DO at the end of the incubation period adopted, a dilution technique is used.
Discussion:
Do depletion is the difference between immediate DO of the diluted sample and 5 day or 3
day DO of the diluted and incubated sample. Immediate DO should be determined within 15
minutes of dilution of sample to minimize the effect of time and temperature gradients on
biological activity. Immediate DO should be quite high near the saturation value. A value of
around 7 mg/l however is considered practically satisfactory.
5 day or 3 day DO of diluted and incubate of sample should be at least 2 mg/l and also DO
depletion should not be less than 2 mg/l. So, empirically, the maximum and minimum limits
of DO depletion are (7-2)=5 mg/l and (7-5)=2 mg/l.
Dilution Technique:
This is based on the expected BOD value of the test sample considering the equation
The dilution factor should be so chosen that the expected BOD of sample lies within the
range of minimum and maximum BOD values obtainable.
Table for Consecutive Dilutions for BOD Measurable from 4 mg/l to 20,000mg/l.
1 2 1 2 500 🡪 1000 4 – 10
2 4 1 4 250 🡪 1000 8 – 20
3 5 1 5 200 🡪 1000 10 – 25
4 10 1 10 100 🡪 1000 20 – 50
5 20 1 20 50 🡪 1000 40 – 100
6 40 1 40 25 🡪 1000 80 – 200
7 50 1 50 20 🡪 1000 100 – 25
25 🡪 250
100 🡪 1000
25 🡪 250
50 🡪 1000
25🡪 250
25 🡪 1000
25 🡪 250
100 🡪 1000
25 🡪 250
100 🡪 1000
25 🡪 250
50 🡪 1000
25 🡪 250
25 🡪 1000
When the expected BOD of a sample is fairly known, at least two consecutive dilutions are
adopted for each sample, to provide an expand range of measurable BOD. Experience,
history of the sample and visual observation of color and suspended solids concentration
enables the expected BOD5 to be estimated fairly sensible. If the expected BOD is 100 mg/l,
adopt dilution of 1 to 20 and 1 to 40, so that measurable range of BOD extends from 40 mg/l
to 200 mg/l with an overlap in between. Within this range, the actual BOD of the sample is
determinable.
If the strength of the sample is not known but the BOD of the sample is broadly expected to
be within a range guided by the description of the sample, then three consecutive dilutions
are adoptedone below and one above the expected range to allow for error in judgment.
Procedure:
1. Take the sample in 2 separate BOD bottles.
2. Fill another two BOD bottles with distilled water.
3. Add 1 ml each of phosphate buffer, magnesium sulphate, calcium chloride and ferric
chloride solutions in all above bottles.
4. Find immediately D.O. of the sample and distilled water on 1st day.
5. Incubate at 270C for 3 days the other two bottles. Tightly put the stopper to prevent any
air entry into the bottles.
6. Determine DO content in the incubated bottles at the end of 3 days by using DO estimation
method.
Observations:
Dilutio
BOD5 at
n
Sample Description Bottle DO5 or 200C/
Factor DO0 Remark
No. of sample No. DO3 BOD3 at
Adopte
270C
d
Calculation:
D.O. (mg/lit)= X ml * N. of Na2S2O3 * Eq.Wt. of Oxygen*1000
Volume of sample
DO0= 8 x 0.025x 8 x 1000 /203
= 7.88
DO3= ( 7.88 -4.83 ) x 40
= 122 Mg/lit
DO5 or DO3=
BOD5 (at 20oC) = [(Immediate DO of diluted sample) – (5 day DO of diluted and incubated
sample)] * Dilution Factor
OR
BOD3 (at 27oC) = [(Immediate DO of diluted sample) – (3 day DO of diluted and incubated
sample)] * Dilution Factor
Result:
The amount of BOD determined from the given waste water sample is i) Wastewater : 122
Mg/lit., ii) Aquaguard : 2.65 Mg/lit.
Conclusion:
As per IS standard the limit of BOD value is 30Mg/lit. The BOD (at 27 oC) value of
aquaguard sample is 2.65 Mg/lit, as it lies between the norms it is safe to disposale in
water bodies without treatment. But in case of Domestic waste water the BOD value is
122 Mg/lit which exceeds the limit. Hence, it needs the proper treatment before dispose
it in bodies.
Significance:
1. It is the principle test which gives the idea of biodegradability of a sample and strength of
waste. Hence, the amount of pollution can be easily measured.
2. It is the basic criteria for control of stream floatation efficiency of a treatment plant can be
judged by considering influent BOD affluent BOD.
3. BOD values of several hundred mg/l indicate strong sewage.
4. Drinking water should have BOD less than 1ppm.
Experiment No. 8
Date:
Experiment No. 8
Aim: To determine Chemical Oxygen Demand (C.O.D.) from the given waste water sample.
Apparatus: COD Digester with refluxing flasks, burette, pipette, beaker and measuring
cylinder
Reagents:
1. 0.25 N Potassium Dichromate solution (K2Cr2 O7)- oxidizing agent
2. 0.1N Ferrous Ammonium Sulphate concentration
3. Conc. H2SO4- provides low pH necessary for oxidation by dichromate
4. Ferroin indicator
5. Distilled water,
6. Mercuric Sulphate (HgSO4) & Silver sulphate (AgSO4)
Principle:
Most of the organic matters are destroyed when boiled with a mixture of potassium
dichromate and sulphuric acid producing carbon dioxide and water. A sample is refluxed
with a known amount of potassium dichromate in sulphuric acid medium and the excess of
dichromate is titrated against ferrous ammonium sulphate. The amount of dichromate
consumed is proportional to the oxygen required to oxidize the oxidizable organic matter.
Chemical oxygen demand is a measure of the oxygen required to oxidize all compounds,
both organic and inorganic in water. The chemical oxygen demand (COD) determines the
amount of oxygen required for chemical oxidation of organic matter using a strong chemical
oxidant, such as, potassium dichromate under reflux conditions. This test is widely used to
determine degree of pollution in water bodies and their self-purification capacity, efficiency
of treatment plants and Pollution loads. COD determination has an advantage over BOD test
in that the results can be obtained in less than 5 h whereas BOD determination requires 3 or 5
days. Further the test is relatively easy and precised. Also there are not many interferences as
in the case of BOD.
Table of consecutive dilutions for COD measurable from 160 mg/l to 4,20,000 mg/l
Actual over all dilution
Vol. of Volume of Range of COD
Sr.
D.F. original diluted Vol. of diluted Measurable
No.
Sample Sample mg/l
Sample ml Sample ml
1 1 1 1 20 🡪 20 4 – 10
2 2 1 2 50 🡪 100 8 – 20
3 5 1 5 20 🡪 100 10 – 25
50 🡪 100
4 10 1 10 20 – 50
20 🡪 100
50 🡪 100
5 20 1 20 40 – 100
10 🡪 100
20 🡪 100
6 50 1 50 80 – 200
10 🡪 100
50 🡪 100
10 🡪 100
10 🡪 100
10 🡪 100
20 🡪 100
10 🡪 100
20 🡪 100
10 🡪 100
For distillery spent wash, D.F. may be 100 & 200 or 200 & 250.
For sugar factory molasses, D.F. may be 200 & 500.
Procedure:
1. Take two COD flasks P & Q. Place about 400mg of H2 SO4 in each flask.
2. Add 20 ml of distilled water to flask P (blank flask) & 20 ml of sample direct or diluted
to flask Q.
3. Add 10 ml of 0.25 N K2Cr2O7 accurately using a pipette to each flask.
4. Add 30 ml Conc. H2SO4 to each flask slowly in installments, stirring the contents
carefully.
5. Add about 200mg of Ag2SO4 to each flask.
6. Add 3 to 4 glass beads or rounded quartz pebbles (to minimize bumping of acid mixture
during boiling).
7. Attach both flasks to condensers or COD Digester. Heat & digest for two hours at 150oC.
8. Cool the flasks. Add 80ml of distilled water down each condenser attached to wash down
condensed organics sticking to inner surface.
9. Detach the flasks and cool the flasks to room temperature (This is very important. If the
flask contents are at a high temperature than the titrant, then very large quantities of
titrant will be used up & COD results will be erroneous).
10. Titrate both flasks against standardized ferrous ammonium sulphate using 2 to 3 drops of
Ferroin indicator.
11. Record titrant used (a) ml for blank flask P & (b) ml for sample flask Q.
Observation:
Burette reading
Sample Sample COD
Dilution For Blank For Sample Remarks
No. description mg/l
(a) (b)
Domestic
1 21.1 -
1 waste water - 1
2 21.1 15.8
sample
Calculation:
COD (mg/l) = [(a – b) × N (FAS) × 8 × 1000] /vol of sample (ml)
= [ (21.5-15.8)*0.1*8*1000]/20
= 216 mg/lit.
Result:
The amount of COD determined from the given waste water sample is 216 mg/l.
Conclusion:
As per the IS standard the limit for COD discharge in wastewater is250 mg/lit. As per
the given waste water sample has COD discharge less than standard limit,Hence , It is
suitable or safe to dispose of in water bodies.
Significance:
1. COD test is widely used in operation of treatment facilities
2. Higher the COD value indicate the excessive presence of organic matter which gives
higher pollutant load in water or waste water
3. As per I.S standard the limit for COD discharge in waste water is
a) In marines and coastal areas : 250 mg/lit
4. For COD determination helps in deciding the treatment facilities given for industrial and
domestic waste water
Procedure Chart:
APPENDIX
Cl Chloride
Na2S2O3 Sodiumthiosulphate
Ag2SO4 Silversulphate
KI Potassium iodide
Na Sodium
K Potassium
a) For
process
waste
water-100
b) For
Suspended cooling
Solids, mg/L, 100 600 200 water
max. effluent 10%
above
total
suspended
matter of
effluent
solids,max.
850
microns
Shall not
Total residual
chlorine, 1.0 - - 1.0
mg/L, max.
Ammonical
nitrogen (as 50 50 - 50
N), mg/L, max.
Total kjeldhal
nitrogen 100 - - 100
[N], mg/L, max.
(NH3) mg/L,
Max.
Biochemical
Oxygen Demand
(BOD5)
Chemical Oxygen
Demand 250 - - 250
(COD)
Hexavalent
Chromium (as Cr) 0.1 2.0 - 1.0
mg/L, max.
Total Chromium
(as Cr) 2.0 2.0 - 2.0
mg/L,max.
mg/L, max.
Fluoride (as F)
2.0 15 - 15
mg/L, max.
Dissolved
Phosphate (as P) 5.0 - - -
mg/L, max.
Sulphide (as S)
2.0 - - 5.0
mg/L, max.
Manganese (as
02 02 - 02
Mn) mg/L
Vanadium (as V)
0.2 0.2 - 0.2
mg/L
Nitrate Nitrogen
10 - - 20
mg/L
NOTE: * = All efforts should be made to remove colour and odour as far as
practicable.