Finalenv Lab Manual

Institute of Technical Education & Research, SOA University
DEPARTMENT OF CIVIL ENGINEERING
ENVIRONMENTAL
ENGINEERING LABORATORY
LAB MANUAL
ENVIRONMENTAL
ENV.
EXPERIMENT NO-01
Determination of pH in Drinking Water :
AIM OF THE EXPERIMENT: To determine the pH and the physical characteristics like
temperature, colour, odour of a water sample.
APPARATUS REQUIRED:
1. pH meter
2. Thermometer
3. Wash bottle
4. Beakers
CHEMICALS/REAGENTS REQUIRED:
1. 7.0&4.0 OR 9.2 Buffer Solutions.
2. Universal Indicator
THEORY: pH is a very important measuring parameter for all chemical, bio chemical and bio
logical system. pH also plays a very important role in all chemical and bio chemical reactors
occurring in our human body. pH is a measure of hydrogen or hydronium ion concentration and is
expressed in logarithmic scale i.e. pH=-log[H+].
Pure water ideally contains equal amount of H+ and OH- ions as 10-7 moles/liter each.
Therefore pH of water depends on the concentration of H+ and varying OH- concentration
expressed as product of H+ and OH- concentration.
Kw =[H+][OH-]=10-7 X 10-7=10-14
Therefore [H+] can range from 0 to 10-14 and according to the linear pH scale range is 0-14.
Ideally pure water has a pH of 7. Increase in concentration [H+] ion
i.e. >10-7moles/liter
shall have accompanying decrease in [OH-]. Therefore less than 7 signifies acidic environment,
whereas pH >7 signifies basic nature and 7 being neutral.
Department of Civil Engineering, ITER, SOA University
Page 2
ENVIRONMENTAL
ENV.
pH of natural water depends on important natural phenomena like absorption of carbon

dioxide from atmosphere to water bodies and dissolution of geological minerals like limestone,
dolomite etc into water bodies. Accordingly pH of natural water bodies seldom has ideal pH of 7
but because of a aforesaid reasons, the pH value varies from 6.5to 8.5.
pH is measured by means of an electronic instrument called pH meter. As per Nernst
theory, a change in 59mili volt corresponds to a change in 1 unit of Ph. Alternatively pH can be
measured with the use of Universal Indicator solution with the help of colour comparator with
colour chart with different pH.
Temperature: Temperature is a very important physical parameter in water bodies. It

generally influences the density, viscosity, solubility of salts and saturation of dissolved oxygen
etc. Temperature is measured by means of thermometer.
Colour: Dissolved material like inorganic contaminants, organic impurities like dye,
humic acid from plants impart colour to water body. Natural water always colourless. Colour
measurement is done by different colour compactor. Colour is measured and expressed in
different units in reference to the comparison with different standard colour. Colour produced by
1mg/lit. of platinum as potassium chloroplatinate (K2PtCL6)is taken as one standard unit of
colour. The colour of water sample is in terms of this standard unit.
Odour: potable water should not have any objectionable odour. Taste and odour may be
due to presence of undesirable organic and inorganic contaminants. Quantitative odour
measurement is again compared with standard sample and is expressed as Threshold Odour
Number (TON).
PROCEDURE:
1. pH meter is calibrated with respect to standard pH solution of 4 and 7.
2. Temperature is noted and expressed in degree C.
3. 100ml of sample was taken and pH electrode was dipped inside and reading of pH
was noted with respect to temperature.
4. 10ml of the sample was taken. To this 3-4 drops of Universal Indicator solution
was added. The resultant colour was compared with colour chart.
Page 3
ENVIRONMENTAL
ENV.
ENVIRONMENTAL SIGNIFICANCE:
pH is very important in all important chemical and bio-chemical reactions.
Ambient pH of water supply should be within range of 6.5-8.5.
Very low pH < 6 affects human body.
Very low and very high pH cause material damage by corrosion.
pH is very important factor in biological waste water treatment.
High temperature lowers oxygen solubility.
Presence of objectionable colour and odour indicate the presence of undesirable

contaminants.
Page 4
ENVIRONMENTAL
ENV.
EXPERIMENT NO-02
Determination of Turbidity of Water:
AIM OF THE EXPERIMENT: To determine the turbidity of water sample.
APPARATUS REQUIRED:
1. Turbidity meter (Nephelometer)
2. Sample cell
3. Beakers
Preparation of Formazine suspension which is used as standard turbidity suspension is as
follows:
Solution I: Dissolve 5g of hydrazine sulphate (NH2)2H2SO4 into a 500 ml

volumetric flask and add distilled water to make up to the mark. Leave the mixture
to stand for 4 hours.
Solution II: Dissolve accurately 50 g of hexamethylene tetramine (CH2)6N4 into a

500ml volumetric flask and add distilled water to make up to the mark.
Mix solution I and solution II to form formazine turbidity concentrate. Allow it to

stand in a closed container at 250C to 300C for 48 hours to produce insoluble white
turbidity corresponding to 4000NTU.
THEORY:
Turbidity in water is caused by the suspended particles that interfere with the passage of
light. The size of the suspended particles ranges from colloidal to coarse dispersion. The nature of
the particles may be either organic or inorganic, chemical inert or microbial. Any turbidity in
drinking water is associated with the pollution.
Page 5
ENVIRONMENTAL
ENV.
There are several ways to test turbidity and several ways to standardize the results. The
most scientific measurement uses a nephelometer to electronically measure the amount of light
scattered by the suspended particles in the sample, reporting the results in Nephelometric
Turbidity Units (NTUs).
The higher the intensity of scattered light, the higher turbidity. However, the turbidity is
not a direct measure of suspended particles in water.
PROCEDURE:
1. Switch the instrument ON and allow 10/15 minutes for warm up.
2. Set standard control (CAL knob) to maximum and insert sample cell with distilled water
into cell holder with shield. Using SET ZERO CONTROL adjust the meter reading to
zero.
3. Remove the above Cell and replace with another Cell containing standard solution
(Formazine).
4. Adjust STANDARDIZE CONTROL to get the desired turbidity reading on the scale.
5. Instrument is now ready for test samples. Insert the cell containing samples of unknown
turbidity in the cell holder and note the readings on meter.
As per IS 10500 the desirable limit and permissible value of Turbidity in potable water
should be in less than 5 & 10 NTU respectively.
Turbidity diffuses sunlight and slows photosynthesis. Plants begin to die, reducing
the amount of dissolved oxygen and increasing the acidity. Both of these effects harm
aquatic animals.
Turbidity raises water temperature because the suspended particles absorb the sun's heat.
Warmer water holds less oxygen, thus increasing, the effects of reduced photosynthesis. In
addition, some aquatic animals may not adjust well to the warmer water, particularly
during the egg and larval stages.
Page 6
ENVIRONMENTAL
ENV.
Turbidity adversely affects self purification processes like aeration and light penetration in
water bodies.
Highly turbid water can clog the gills of fish, stunt their growth, and decrease their
resistance to diseases.
The organic materials that may cause turbidity can also serve as breeding grounds for
pathogenic bacteria. When drinking water reservoirs are turbid, the water treatment plant
usually filters the water before disinfecting it.
Industrial processes and food processing, require clear water. Turbid water can clog
machines and interfere with making food and beverages.
Page 7
ENVIRONMENTAL
ENV.
EXPERIMENT NO-03
Determination of Total Solids in Water:
AIM OF THE EXPERIMENT: To determine the amount of different types of solids in
the given water sample.
APPRATUS REQUIREMENT:
1. Evaporating disc of 100 ml capacity (made of porcelain or high silica glass).
2. Muffle Furnace
3. Drying Oven
4. Electronic balance
5. Funnel
6. Beaker
7. Stand
8. Filter paper
THEORY:
Natural rain water when comes in contact with earth soil and while flowing across the
surface gets contaminated with impurities mostly in the form of solids. Solids may be of different
types like suspended solids, colloidal solids and dissolved solids depending upon their size.
Suspended solids refers to larger size solids with particle size greater than 10-5m, remain
in suspended form and can be easily settled down in a finite detention time. Dissolved solids
refers to small size solids with particle size less than 10-9 m, comparable to size of water molecule
and therefore these particles remain in solution.
Colloidal solids refer to those smaller solids. Size range in between suspended and
dissolved solids i.e. 10-5 m to 10-9 m. these are not visible to naked eye but can be clearly seen
through microscope. Their zig zag motion with non-settleable characteristics is popularly called
Brownian motion. Colloidal solids particles are suspended but not settleable in finite time. These
Page 8
ENVIRONMENTAL
ENV.
can be settled with the help of external chemical agents called coagulant and hence the process is
called coagulation. Total solid refers to the total amount of solids present in a water sample.
Total Solid (TS) = Total Suspended Solids (TSS) + Total Dissolved Solids.
Total Suspended Solids also includes the amount of colloidal solids. Floatable solids
refer to those which being less dense than water remain floating on the surface water
and can be removed by screening.
Total volatile solid refers to organic volatile fraction of the total solids.
Total fixed solid refers to inorganic residual part of the total solids.
PROCEDURE:
1. Take a dry and clean porcelain dish of 100 ml capacity and take its mass in an electronic
balance. Let this mass as W1 gm.
2. Take 100 ml of representative sample and pour it into porcelain disc.
3. Place the disc in a drying oven, maintained at 1000 C for 24 hours.
4. Take out the disc from oven and let it be cool down it to room temperature. Let the mass
be W2 gm.
5. Now keep the disc with mass W2 in muffle furnace maintained at temperature of
550500C for 4-5 hours. Then take it out of the muffle furnace and cool it to room
temperature in a desiccator.
6. The fixed residual mass refers to inorganic fixed solids. (TFS). Let this mass be W3 gm.
7. Total volatile solids(TVS) is the lost mass represents the organic volatile fraction was
found by difference.
8. For determination of suspended solid and dissolved solids take representative 100 ml
well shaken sample for filtration through filter paper Whatman -40. Take the weight of
the filter paper and record it as W4gm.
9. Dry and cool the residue on the filter paper. Let the mass of the filter paper and residue
as W5 gm.
Page 9
ENVIRONMENTAL
ENV.
CALCULATION:
All the results are to be reported in mg/l or parts per million (ppm).
1. Sample taken
= ___________
2.
X 1000 in mg/l
3.
X 1000 in mg/l
4.
5.
X 1000 in mg/l
6.
ENVIORNMENTAL SIGNIFICANCE:
Suspended solid contributes turbidity to water which causes problem in water supply when its
value is more than 5 NTU.
Natural dissolved solid in the form of hardness are the essential mineral nutrient in water. But
dissolved impurities like fluoride, cyanide, chromate toxic heavy metals are unacceptable.
These parameters must be within permissible limits of IS-10500.
Page 10
ENVIRONMENTAL
ENV.
EXPERIMENT NO-04
Determination of Alkalinity:
AIM OF THE EXPERIMENT: To determine the different types of alkalinity in a given
sample of water.
APPRATUS REQUIREMENT:
1. Burette of 50 ml capacity
2. Conical Flask
3. Measuring cylinder
4. Funnel
5. Beaker
CHEMICAL REQUIREMENT:
1. Standard Sulphuric Acid Solution N/50
2. Phenolphthalein Indicator Solution
3. Methyl Orange Indicator Solution
THEORY:
Alkalinity of water is its acid neutralizing capacity. There are three major types of
alkalinity present in water and waste water system. These are hydroxide alkalinity (OH -),
carbonate alkalinity (CO3 2-) and bicarbonate alkalinity(HCO- 3 ).
As per Stumm and Morgan :
Total alkalinity = Hydroxyl alk + 2 X Carbonate alk + bicarbonate alk hydrogen ion
All the concentration expressions are usually in mol/L
Major source of alkalinity in natural water is the atmospheric carbon-dioxide solubility
and dissolution of rocks and minerals such as calcium and dolomite etc.
Alkalinity in water sample is measured in titration against standard sulfuric acid solution
in presence of suitable indicators. Above pH 8.3 the alkalinity present is in the form of hydroxyl
and carbonate below pH 8.3 up to 4.5, the alkalinity exists as carbonate and mostly in bicarbonate
Page 11
ENVIRONMENTAL
ENV.
form. In order to maintain the uniformity in reporting, all alkalinity concentration values are
reported in mg/l CaCO3.
The titration value corresponding to neutralization with N/50 H2SO4 in presence of
phenolphthalein indicator is termed as p-alkalinity which comprises of entire hydroxide alkalinity
and part of carbonate alkalinity. The titration value corresponding to neutralization with N/50
H2SO4 in presence of methyl orange indicator up to pH 4.5 is termed as M-alkalinity which
comprises of entire bicarbonate alkalinity and rest of carbonate alkalinity.
Total alkalinity (T-alk)= P-alk + M-alk in mg/L as CaCO3
That is all the alkalinity present is in the form of carbonate and bicarbonate alkalinity.
PROCEDURE:
1. Take N/50 solution acid and load it in a 50ml burette fitted with a burette stand.
2. Take 50 ml of supplied water sample in a 250ml conical flask. To this add 3 to 4 drops
phenolphthalein indicator.
3. If the solution is colourless then P-alkalinity is absent.
4. If the colour of the solution turns pink then determine p-alkalinity by titration against the
standard N/50 H2SO4
5. Titrate the water sample till the colour changes from pink to colourless.
6. This corresponds to the end point of p-alkalinity about a pH value of 8.3.
7. Now add 3 to 4 drops of methyl orange indicator. The colour will turned to yellow.
8. Take initial burette reading. Then titrate the solution against N/50 H2SO4, till the colour of
the sample changes to orange red from yellow.
9. This corresponds to end point of M-alkalinity at about pH of 4.5. Note down the final
burette reading.
CALCULATION:
Titration value for P-alkalinity in ml is calculated from the difference of final burette
reading and initial burette reading say V1 ml. Similarly the titration value for M-alkalinity in ml is
calculated from the difference of final burette reading and initial burette reading say V2 ml.
Page 12
ENVIRONMENTAL
ENV.
X1000
X1000
Total alkalinity = P-alkalinity +M-alkalinity is reported in mg/L as CaCO3
Alkalinity is a measure of acid neutralizing capacity of water and waste water system. It acts
as a buffering capacity against the reduction of pH in many water and waste water treatment
practice.
Natural alkalinity acts as buffer to the pH reduction by addition of the alum in coagulants
type water treatment. In the absence of natural alkalinity, lime has to be added to maintain
the optimum pH for optimum coagulation and setting.
Alkalinity is also a key parameter in biological aerobic and anaerobic type of wastewater
treatment.
Microbial activity in biological treatment is very sensitive to lower pH condition and

therefore sufficient natural or induced alkalinity is required to maintain the ambient pH
condition.
A minimum alkalinity in water is required to prevent material loss because of corrosion.
Page 13
ENVIRONMENTAL
ENV.
EXPERIMENT NO-05
Determination of Free Mineral Acidity in Drinking
Water:
AIM OF THE EXPERIMENT: To determine the amount of Free Mineral Acidity (FMA)
and
Carbon Dioxide (CO2) in a given sample of water/waste water.
APPARATUS REQUIRED:
1. Burette with burette stand.
2. 250ml conical flask.
3. Pipette with elongated tips.
4. Measuring cylinder.
5. Wash bottle
6. Beakers.
1. Standard Sodium Hydroxide (NaOH) solution of strength N/50.
2. Phenolphthalein Indicator Solution
3. Methyl Orange Indicator Solution
THEORY:
Acidity of water is its base neutralizing capacity (BNC). It determines the amount of
hydroxyl ion required to neutralize the available free hydrogen ion concentration in water sample.
Free mineral acids are mainly inorganic like sulphuric acid, hydrochloric acid,
hydrofluoric acid, nitric acid, phosphoric acid etc. these are mostly strong acids with very low pH
less than 4. Free mineral acidity is not expected in natural water supply unless it is contaminated
by acidic industrial/mining effluent. Acidity in natural water is influenced by dissolution of
carbon dioxide resulting in mild acidity with pH value can reach about 5. Another source of
natural acidity is the dissolution of some acid minerals particularly of sulphuric minerals.
Page 14
ENVIRONMENTAL
ENV.
Microbial decomposition particularly anaerobic decomposition in stagnant water bodies is

responsible for acidity in natural water with formation of organic acids.
Acid rain problem in industrial environment may reduce the pH value of water bodies to
less than 4. Similarly industrial and mining acidic effluent can contaminant the water bodies
reduce the Ph z value of water bodies to less than 4. FMA is determined by titration against
standard alkali solution up to pH 4.5 using methyl orange indicator. Therefore the determination
of FMA ascertains the contamination from some anthropogenic sources particularly from
industrial effluent. Dissolution of CO2 is responsible for mild acidity, which can be determined
by titration against standard alkali solution up to Ph 8.3 using Phenolphthalein indicator.
In order to have uniform expression of result and comparison with alkalinity and hardness,
acidity results are also expressed in mg/l or ppm as CaCO3.
PROCEDURE:
1. Rinse the burette with 0.02N Sodium hydroxide and then discard the solution.
2. Fill the burette with 0.02N sodium hydroxide and adjust the burette.
3. Fix the burette to the stand. Take initial burette reading.
4. Take 100 ml of supplied water in a 250 ml conical flask.
5. Add 3 to 4 drops of methyl orange indicator in the conical flask.
6. If the colour of the solution is yellow then FMA is absent.
7. If the colour changes to orange then Free Mineral Acidity is present. Now titrate the
sample against the N/50 NaOH solution until the orange colour changes to yellow.
8. Note down the burette reading after titration .
9. This corresponds to the end point of free mineral acidity at about a pH value of 4.5.
10. The titrate value can be found out by difference in burette reading.
11. Now to this sample add 3 to 4 drops of Phenolphthalein indicator solution.
12. Note down the initial burette reading and continue the titration, until the colour changes
from yellow to faint pink colour.
13. This corresponds to end point of CO2 determination at about pH of 8.3.
14. Note down the final burette reading. This volume is used for calculating the total acidity.
Page 15
ENVIRONMENTAL
ENV.
CALCULATION:
Mineral Acidity
Titration valu in ml x 1000

Volume of sample taken
Carbon Dioxide Acidity =
Titration valu in ml x 1000

Acidity is a measure of the base neutralizing capacity of water and wastewater system.
The presence of Free Mineral Acidity indicates the possible large scale contamination
of industrial/mining acid effluent. Anaerobic decomposition in stagnant condition
results in formation of large amount organic acids which may lead to free acidity in
water bodies. Water with free mineral acidity causes great deal of damages to flora
and fauna. It drastically affects the aquatic eco-system.
Free Mineral Acidity causes a very low pH condition which leads the dissolution of
many toxic heavy metals which are otherwise insoluble under ambient conditions.
Water with acidity causes severe corrosion problem to materials and structures.
Therefore water with Free Mineral Acidity warrants the suitable treatment in the form
of neutralization with lime.
Dissolution of CO2 in water bodies maintains a kind of dynamic equilibrium of

exchange reactions between alkalinity in the form of carbonate and bicarbonate ions
and causes no such harm unless the equilibrium condition is disturbed by some
anthropogenic contamination.
Page 16
ENVIRONMENTAL
ENV.
EXPERIMENT NO-06
Determination of Total Hardness and Calcium Hardness.
AIM OF THE EXPERIMENT:
To determine the Magnesium and Calcium Hardness in a
given water sample.

APPARATUS REQUIRED:
1. Burette of 50ml capacity with burette stand.
2. Conical flask
3. Beaker
5. Funnel
1. Ammonia Buffer Solution.
2. 0.01M EDTA standard solution
3. Murexide indicator
4. 1N sodium hydroxide buffer solution
THEORY:
Hardness is caused by divalent metallic cations.
These are capable of reacting with the
soap to form precipitation. The principle hardness causing cations are calcium (Ca), magnesium
(mg), strontium (Sr) and ferrous(Fe). Total hardness is to be estimated as the total dissolved salts
of calcium and magnesium particularly of bicarbonate of carbonate, sulphate, chloride, hydroxide
etc. Hardness not being a single entity and to have uniform comparison with other equivalent
analytical parameter like alkalinity and acidity, hardness result are normally expressed in mg/l as
CaCO3 . When total hardness greater than sum of carbonate and bicarbonate alkalinity, the
amount of excess of alkalinity is called the non carbonate hardness.
Ethylene Diamine Tetracitic Acid (EDTA) or its disodium salt forms soluble chelate
complex with many metal ions, preferably with divalent metal ion like Ca, Mg, Sr, Fe, etc.
Page 17
ENVIRONMENTAL
ENV.
M2+ + EDTA = M-EDTA complex (solute)

In presence of soluble metal ion indicator like Erichrome Black T (EBT) indicator at a
soluble pH of 10 shall term soluble complexes with metal like.
M2+ + In- -------- M-In
Then these metal ion indicator react with EDTA solution to term Metal-EDTA soluble
complex and metal ion indicator form the complex.
M-In + EDTA ---------------- M-EDTA + In (free)
Therefore this is a typical complexometric titration and reaction involved here are
complex in nature.
PROCEDURE:
DETERMINATION OF TOTAL HARDNESS
1. Take 100 ml of supplied water sample in a 250 ml conical flask.
2. Add 1 ml of ammonia buffer solution to the sample to maintain a constant pH of 10.
3. Load 0.01M EDTA solution acid in a 50 ml burette fitted with a burette stand.
4. Then add 3- 4 drops of EBT indicator showing M-In complex as wine red colour.
5. Titrate the sample against standard 0.01M EDTA solution till the colour changes from
wine red to deep blue indicating the end point of the reaction.
6. Calculate the titration volume in ml from the difference in initial and final reading.
DETERMINATION OF CALCIUM HARDNESS
Calcium salts contribute the major amount of hardness salt. Calcium hardness are determined
separately by using different indicator.
1. Take 100 ml of supplied water sample in a 250 ml conical flask.
2. Add 1 ml of 1N NaOH buffer solution to the sample to maintain a constant pH of 12.
3. Then add a pinch of complex metal ion indicator showing a pink colour of metal ion
complex.
4. Titrate the sample against standard 0.01M EDTA solution till the colour changes from
pink to purple colour indicating the end point of the reaction.
Page 18
ENVIRONMENTAL
ENV.
5. Calculate the titration volume in ml from the difference in initial and final reading.
CALCULATION:
Basis of calculation: 1000 ml of EDTA solution = 100 gm of CaCO3
Total hardness in mg/L CaCO3
= Titration value in ml (v1)

X 1000
Calcium hardness in mg/L CaCO3 = Titration value in ml (v2)

Acidity is a measure of the base neutralizing capacity of water and wastewater system.
The presence of Free Mineral Acidity indicates the possible large scale contamination
of industrial /mining acid effuent. Anarobic decomposition in stagnant condition
results in formation of large amount of organic acids which may lead to free acidity in
water bodies.
Water with Free Mineral Acidity causes great deal of damages tovflora and fauna. It
drastically
Page 19
ENVIRONMENTAL
ENV.
EXPERIMENT NO-07
Determination of Optimum Coagulant Dosage for a Coagulation Process
To determine the optimum alum dosage in a given
sample of water/wastewater.
APPARATUS REQUIRED:
1.
2.
3.
4.
5.
6.
Jar test apparatus

Conical flask
Beaker
Measuring cylinder
Funnel
Nephelometer
1. Alum solution 5gm/liter
2. Saturated lime solution
THEORY:
Natural rain water when comes in contact with earth soil and while flowing across the
surface gets contaminated with impurities mostly in the form of solids. Then solid may be of
different types like suspended solids, colloidal solids and dissolved solids depending upon their
size. Suspended solids refers to large size solids with particle size greater than 10-6m,remain in
suspended form and can be easily settled in a finite detention time.
Dissolved solids refers to smallest size particle with size less than 10-9m, comparable to
size of water molecule and therefore these particles remain in solution.
Colloidal solids refers to those smaller solids, size range in between suspended solids and
dissolved solids i.e. 10-6 m to 10-9 m. these are not visible to naked eye but can be clearly seen
through microscope. Their zig zag motion with non-settleable characteristics is popularly called
Brownian motion. Colloidal solid particles are suspended but not settleable in finite time. These
can be settled with the help of external chemicals agents called coagulant and hence the process
followed by gravity settling and hence is called flocculant setting.
Page 20
ENVIRONMENTAL
ENV.
Alum as the hydrated salt of aluminum sulphate is one of the most popular coagulant.
Besides alum, the other popular coagulants are ferric alum, alumina, aluminated coppers etc. nowa-days synthetic polymeric compounds called poly-electrolytes have been developed which can
be used to get best results.
When alum is added to water , in general following simplified reaction may take place.
In presence of Natural alkalinity as Ca(HCO3)2
AL2(SO4)3.18H2O + 3 Ca(HCO3)2 = 2AL (OH)3 + 3 CaSO4 + 6 CO2 + 18 H2O
In presence of alkalinity IN THE FORM OF LIME AS Ca(OH)2
AL2(SO4)3.18H2O + 3 Ca(OH)2 = 2AL (OH)3 + 3 CaSO4 + 18 H2O
The Product compounds except AL(OH)3 is the insoluble precipitate floc. The above
equation are oversimplified. In fact a series of positively charged in soluble alumino-hydroxy
complexes including that of AL (OH)3 called floc are formed. The formation of this positively
charged insoluble floc is responsible for destabilizing with the development of a zeta potential
provides the necessary electrostatic driving force for particle aggregation among the colloidal
particles and colloidal particles forming larger and heavier particles agglomerates. Followed by
gravity action these heavier particles agglomerates shall settle down easily. This is the principal
mechanism of flocculent setting applicable for non settleable colloidal particles.
Optimum alum dozing can be estimated in laboratory jar test at an optimum pH range of
7.0 to 7.5.
PROCEDURE:
1. Take10nos of 400ml beakers with 100ml of sample in each beaker.
2. To these beakers add 1,2,3,4,5,6,7,8,9 and 10 mL of alum solution. Agitated The samples
in a jar test floccuator at a rate 500 to 1000 rpm for two minutes and then at a slow speed
for 15 minutes. Then keep the samples for 15 minutes for settle down.
3. Measure pH of each sample.
4. Measure the turbidity of each sample in a Nephelometer.
Page 21
ENVIRONMENTAL
ENV.
5. Alum is an acid salt and can lower down pH if sufficient natural alkalinity is not present.
If after adding alum the pH value came below 7, then lime is to be added to maintain the
optimum pH range of 7.0 to 7.5.
RESULT AND CALCULATION:

Plot a graph between alum dosage concentration along X-axis and turbidity in NTU along
Y-axis. Estimate Optimum alum dosage by extrapolating with minimum turbidity point. Express
the result in mg/liter.
Optimum Coagulant Dosage requirement is to insure the effective coagulation and

sedimentation process.
Coagulation and sedimentation followed by filtration in water treatment should

insure the desirable turbidity level of less thsn 5 NTU in drinking water suplly as
per IS 10500.
This test also estimate the Optimum Coagulant Dosage requirement in many
industrial and mining wastewater.
Page 22
ENVIRONMENTAL
ENV.
EXPERIMENT NO-08
Determination of Percentage of Available Chlorine in Bleaching Powder.
AIM OF THE EXPERIMENT: To determine the percentage of available chlorine in the
given bleaching powder sample.
APPARATUS REQUIRED:
2. Conical flask
3. Beaker
1. 0.1N SodiumThiosulphate Solution
2. Potassium Iodide Solution
3. Glacial Acetic Acid
4. Strach Indicator
5. Bleaching Powder
THEORY:
This determination is based on the principle of iodometric titration. Bleaching powder as
Ca(OCL)2 is used as disinfectant. The disinfecting action of bleaching powder due to the presence
of chlorine in it. The librated chlorine dissolves in water to given HCL & HOCL which is
responsible for disinfection and bleaching action of bleaching powder.
Ca(OCl)2 + H2O ---------------- Ca(OH)2 +Cl2
Cl2 + H2O ----------------------- HCl + HOCl
The percentage of available chlorine is defined as the amount of chlorine of chlorine
librated in hundred parts of the bleaching powder sample. The chemical formula of bleaching
powder is Ca(OCl)2 and its chemical name is calcium hypochlorite . It is hygroscopic and
undergoes continouos determination during srorage. in this method a suspension of bleaching
Page 23
ENVIRONMENTAL
ENV.
powder is titrated with standard sodium thiosulphate (Hypo) solution in presence of glacial acetic
and KI solution. The librated chlorine from bleaching powder sets free an equivalent amount of
iodine, using strach as indicator. The titration in which liberated iodine is titrated with hypo
solution is known as iodometric titration.
i.
Ca(OCl)2 + 2CH3COOH ---------------------- (CH3COO)2Ca + Cl2 + H2O
ii.
Cl2+2KI ------------------------------------------2KCl+l2
iii.
2NaS2O3+12--------------------------------------2Nal+Na2S4O6
KI is to be used in excess amount
Glacial Acetic Acid is used to maintain the pH of the solution 3 to 4
PROCEDURE:
1. Dissolve 1gm of freshly prepared bleaching powder in 1 liter of distilled water.
2. Take 100ml of this homogeneous solution of bleaching powder in a 250ml conical flask.
3. To this add 2ml of glacial acetic acid followed by 10ml of 10% KI solution.
4. Keep the conical flask in the dark place for 5 minutes.
5. Then titrate this against 0.1N sodium thiosulphate solution till light yellow appears. Then
add 5 drops of freshly prepared starch solution to get blue colour and continue the titration
till the blue colour of the solution disappear, indicating the end point.
6. Repeat the titration to get at least three concordant values.

The weight of the bleaching powder sample = W gm
The volume of thiosulphate used = V ml
Strength of the thiosulphate = 0.1N
1000 ml In thiosulphate = 35.5 gm chlorine
1ml of 0.1N Na2S2O3 = 3.55 mg of chlorine.
V ml of 0.1N thiosulphate = 3.55 x V mg of chlorine
That is 100 ml of bleaching powder solution contains 3.55 x V mg chlorine
100ml of bleaching powder solution contain w mg of bleaching powder
Page 24
ENVIRONMENTAL
ENV.
W mg of bleaching powder contains 3.55 mg of available chlorine

100 mg of bleaching powder contain that is mass % of available
Chlorine =
Bleaching powder is a popular disinfectant particularly for small-scale household

application.
Its disinfection action results from the available free chlorine in solution. But the
available free chlorine in a freshly prepared bleaching powder hardly exceeds 30%.
More over it is not stable and loses chlorine over time.
Therefore bleaching powder is not popular in large scale commercial application.
Page 25
ENVIRONMENTAL
ENV.
EXPERIMENT NO-09
Determination of Break Point Chlorine & Chlorine demand
To determine the break point chlorine and chlorine
demand of a water sample.
APPARATUS REQUIRED:
1. 10nos of conical flask
2. pipette
4. Burette with stand
1. 0.025N Sodium Thiosulphate Solution
2. Glacial acetic acid
3. Potassium iodide solution
4. Starch Indicator
THEORY:
Chlorine gas or chlorine based compounds are popularly used as disinfectants in water
treatment practice. These compounds fulfill the following desirable disinfectant characteristics.
They have fast rate of killing of pathogenic microbes. They dont produce undesirable substances.
They are fairly stable & are cheap & commercially available. Chlorine reacts with other
constituent in water like inorganic reducing substances, organic matter and ammonia etc. before
being used up destroying pathogenic microbes. The amount of chlorine utilized for the aforesaid
reactions is the chlorine demand of the particle water sample. The major constituent of chlorine
demand is the amount of chlorine used up for the oxidizing inorganic reactant like sulphite, nitrite
etc. The amount of chlorine utilized for the formation of chlororganic and chloramines. This
amount of chlorine utilized for destruction of so formed chlororganic and chloramines. The point
d is called the break point chlorination. The chlorine demand can be calculated by deducting the
Page 26
ENVIRONMENTAL
ENV.
residual chlorine at break point chlorination from the amount of chlorine dosage required to
obtain break point chlorination. The dosage of beyond break point is available for disinfection
action and is defined as free available chlorine. Usually residual chlorine of 0.5ml/L after break
point is maintained to have the satisfactory disinfection in water treatment practices.
When a graph between the amounts of chlorine dosage in X axis is plotted against
appearance of residual chlorine in mg/L in Y-axis a nature of curve as depicted below included
the typical component of chlorine demand in mg/L.
Chlorine demand in mg/L =
Amount of chlorine up to break point Residual chlorine at break point i.e. DF DG
PROCEDURE:
1. Take each of 100 ml of water sample in 10nos of conical flask.
2. Prepare a chlorine solution / bleaching powder solution of particular strength.
3. Add different dosage of chlorine solution to each container. Keep them for 30minutes for
reaction.
4. Analyze the content of each container for residual chlorine by means of chloroscope
instrument or by the use of iodometric titration using hypo solution

1. Plot the curve between chlorine dosage in mg/L and appearance of residual chlorine.
2. Identify the different demand regions and minimum inflection point indicating the break
point chlorination.
3. Calculate the chlorine demand as the optimum dosage of chlorine from the curve at the
point of free residual chlorine of 0.5mg/L after reaching break point chlorination.
Page 27
ENVIRONMENTAL
ENV.
Chlorine and chlorine demand based compound are considered to be disinfectant as they
satisfy almost all the desirable characteristics of a good disinfectant.
Disinfection in an essential process in drink water treatment process. This ensure the
effective disinfection of pathogenic microbes which are responsible for out-break of many
water-born diseases.
Surface water supply is mostly contaminated by domestic sewage and in some cases
industrial effluent which is responsible for presence of pathogenic microbes in water
supply. The growth water in urban area also affected by microbial contamination by
sewage.
In adequate chlorination does not lead to satisfactory disinfection. Whereas excess

chlorination may leads to change in quality of water with to taste and odour. Sometimes
excess of chlorination may produces some undesirable substances.
Page 28
ENVIRONMENTAL
ENV.
EXPERIMENT NO-10
Determination of Biochemical Oxygen Demand (BOD)
AIM OF THE EXPERIMENT: Determination of Biochemical Oxygen Demand (BOD)
of a given wastewater sample.
APPARATUS REQUIRED:
1.
2.
3.
4.
5.
BOD incubator
BOD bottle of 300ml capacity
pipette
Measuring cylinder
Burette with stand
1. Phosphate Buffer solution:
Dissolve 8.5 g of potassium dihydrogen phosphate (KH2PO4); 21.75 g Dipotassium
Hydrogen Phosphate (K2HPO4); 33.4 g Disodium Hydrogen Phosphate (Na2HPO4), 7H2O
and 1.7 g Ammonium Chloride (NH4Cl) in distilled water and dilute to 1 L. pH of this
solution is 7.2
2. Magnesium sulphate solution:
Dissolve 22.5 g Magnesium sulphate in distilled water and dilute to 1 L.
3. Calcium chloride solution:
Dissolve 27.5 g calcium Chloride (CaCl2) in distilled water and dilute to 1 L.
4. Ferric chloride solution:
Dissolve 0.25 g Ferric Chloride in distilled water and dilute to 1 L.
5. Manganous sulphate solution:
Dissolve 480 g MnSO4, 4H2O, 400 g MnSO4, 2H2O or 364 g MnSO4, H2O in distilled water,
filter and dilute to 1 L.
6. Alkaline KI solution
Dissolve 500 gm of sodium hydroxide /700 gm of potassium Hydroxide , 20 gm of sodium
azide and 150gm of potassium iodide in 1liter distilled water.
Page 29
ENVIRONMENTAL
ENV.
7. Concentrated sulphuric acid

8. Starch solution
9. N/40 Sodium thiosulphate titrant:
Dissolve 24.82 gm of sodium thiosulphate in 1 liter distilled water. This is 0.1N stock
solution. Dilutr 250ml of this 1 liter to obtain 0.025 N standard solution.
THEORY:
The biochemical oxygen demand is an indirect measure of organic matters present in
water. BOD is defined as the amount of oxygen required by bacteria to stabilise the decomposable
organic matter in aerobic condition. Bacteria utilize organic matter as carbon source for synthesis
of new cells and derive required energies from their oxidation. Hence, BOD is essentially a
bioassay procedure involving the measurement of oxygen consumed by living organisms while
utilising the waste. The BOD test is important in stream-pollution-control activities and is widely
used to determine the pollutional strength of domestic and industrial wastes in term of oxygen that
they will require if discharged into natural water courses in which aerobic condition exists. The
test has its widest application in measuring waste loading to treatment plants and in evaluating
BOD-removal efficiency of such treatment systems.
Since BOD is essentially a bioassay procedure, it is important to maintain the
environmental conditions suitable for bacterial growth. This condition means that toxic
substances must be absent and that all accessory nutrients needed for bacterial growth, such as
nitrogen, phosphorus and certain trace elements, must be present. pH of test sample is maintained
around 6.5 to 7.5 using phosphate buffer. Biological degradation of organic matters under natural
conditions is brought about by a diverse group of organisms that carry the oxidation essential to
completion, i.e., almost entirely to carbon dioxide and water. Therefore, it is important that a
mixed group of organisms, commonly called "seed", be present in the sample. In order to make
the test quantitative, the experiment is carried out in closed system to prevent re-aeration as the
dissolved oxygen (DO) level diminishes. In addition, because of the limited solubility of oxygen
in water, about 9.2 mg/L at 200C, strong wastes must be diluted to levels of demand in keeping
with this value to ensure that dissolved oxygen will be present throughout the period of the test.
PREPARATION OF DILUTION WATER
Saturate the tap water with a supply of compressed air. Add 1 mL each of phosphate
buffer, MgSO4, CaCl2 and FeCl3 solution per litre of water. These are micro-nutrients required by
bacteria. Seed dilution water, if the sample does not contain enough microorganisms. Domestic
wastewater or effluent from biological wastewater treatment plants contains satisfactory seed. 1 to
2 mL of domestic wastewater per litre should be enough for seeding the dilution water.
Page 30
ENVIRONMENTAL
ENV.
PROCEDURE:
1. Take suitable amount of sample in 300 ml BOD bottle. Then dilute the sample to 300
ml in BOD bottle. Therefore dilution factor = 300ml BOD bottles/sample of
wastewater. Determine the initial DO of the sample.
2. Stopper the bottles carefully to exclude air bubbles, water-seal and incubate for 5 days
at 200 C within a BOD incubator.
3. For DO measurement, add 2ml of MnSO4 solution in BOD bottle dipping end of the
pipette against below the surface of water.
4. Add 2ml of alkaline KI in similar manner and mix it thoroughly by shaking the bottle.
Allow the brown precipitate to settle.
5. Then dissolve the brown precipitate by adding 2ml of concentrated sulphuric acid.
6. Take 100ml of the sample and titrate it against N/40 sodium thiosulphate solution.
Determine the end point of titration with the help of starch indicator where the colour
changes from dark blue to colourless at end point.
7. DO values of the incubated sample can be determined by repeating step 3 to 5
The 5-day BOD or BOD5 is calculated as follows:

BOD5, mg/L = {(D1-D2)-(B1-B2) f}
p
D1= DO of diluted sample before incubation, mg/L.
D2= DO of diluted sample after 5 days incubation at 200C, mg/L.
B1= DO of dilution water blank before incubation, mg/L.
B2= DO of dilution water blank after 5 days incubation at 200C, mg/L.
f= volumetric fraction of dilution water in diluted sample.
p= volumetric fraction of sample in diluted sample.
Page 31
ENVIRONMENTAL
ENV.
Dissolved oxygen is vital source of oxygen supply for aquatic life.

Gaseous oxygen is sparingly soluble in water with saturation dissolved oxygen hardly
exceeds 9 mg/L under ambient condition.
Biodegradable organic as oxygen demanding waste, while undergoing biodegradation in
water bodies depletion of dissolved oxygen. As a result aquatic organisim are adversely
affected.
Depletion of DO below certain minimum level may eliminate some aquatic specifies
altogether.
Therefore it is to determine BOD value of the water and stabilize the high BOD waste
water adequate and proper biological treatment before discharging into water bodies.
Page 32
ENVIRONMENTAL
ENV.
EXPERIMENT NO-11
Colorometric Determination of Chromium
AIM OF THE EXPERIMENT: Colorimetric determination of Hexavalent chromium.
APPARATUS REQUIRED:
1. Spectrophotometer in the visible range
2. Pipette
4. 100ml capacity volumetric flasks
5. Conical flasks
1. Standard solution of chromate with K2Cr2O7
2. 1:1 Sulphuric acid
3. Dephenyl Carbazide solution:-250mg of DPC in 50ml acetone and the solution is stored
in a dark place.
THEORY:
Colorimetry is concerned with the determination of the concentration of the substance by

measurement of relative absorption of light with to known concentration of the substance. In
colorimetry whitr light is generally used as light source and determination is usually made with
photoelectric cell. In cholorometric light contained in a comparatively narrow range of
wavelength furnished by passing white light through filter of colored glass glass gelatin etc. is
employed for transmitting only limited spectral region. In spectrophotometery a definite
wavelength of radiation are chosen possessing a band width of less than 1 mm. the signal
corresponding to difference between transmitted radiation of a reference material and that of a
sample at selected wavelength are measured. As per Lamberts law when monochromatic light
Page 33
ENVIRONMENTAL
ENV.
passes through a transparent medium unit intensity of emitted light decreases exponentially as the
thickness of the absorbing medium increases arithmetically.
It =I0e-kt
I0 = Intensity of incident light
It = Intensity of transmitted light
k = constant for the wavelength
I0 = thickness of medium
The ratio is the fraction of incident light transmitted by a thickness 1 of the medium and is
called transmitted (T). the reciprocal of transmitted is called opacity. The absorbance of the
medium (formerly called optical density D)
A = log It /I0
As per Beers law the intensity of a beam of monochromatic light decreases exponentially
as the concentration of the absorbing substance increases arithmetically.
It = I0 x 10-acl
A = log It /I0 =acl
a = molar absorption coefficient
c = concentration of substance under measurement
I = medium path length
Absorption is linearly proportional to concentration or transmittance is inversely
proportional to concentration. This is the fundamental relationship in spectrophotometry and is
called as Beer-Lambert law.
Chromium has three popular oxidation states like as elementmetal Cr and trivalent
Cr3+ and Hexavalent Cr6+ chromium. While Cr3+ is highly insoluble and least available and hence
Page 34
ENVIRONMENTAL
ENV.
least harmful, Cr6+ is highly soluble and bioavailable and hence it is a very toxic substance. Cr3+
can be determined in the laboratory colorometrically with the help of a spectrophotometer.
Acidified chromate solution forms a stable violet to purple colour complex with Dephenyl
Carbazide solution. The intensity of this colour is linearly proportional to the concentration of
Hexavalent chromium present in the sample following Beer-Lambert law in the linear region of
the calibration curve at the absorption wavelength of 540 mm. unknown concentration of the
sample can be determined from the known calibration curve.
PROCEDURE:
1. Prepare Chromium stock solution by dissolving 707mg of AR grade K2Cr2O7 in 500 ml

distilled water. Chromium standard solution of 5 mg/L was prepared by diluting 1 ml of
stock solution to 100 times. 1 ml of this standard solution contains 0.005 mg chromium.
2. Add different chromium solutions each of 100 ml strength with chromium
concentration of 0.05,0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9,1.0,1.5& 2.0 mg/L to each of
these solutions. Allow the violet to purple colour was allowed to develop in
5-10minute.
3. Add 2 ml of this 1:1 concentrated sulfuric acid followed by 2ml of DPC solution to
each of these solutions. Allow the violet to purple colour to develop in 5-10 minute.
4. Then measure the absorbances of different sample with the different colour intensities
with the help of a spectrophotometer at wavelength of 540 nm.
5. Then plot the concentration Vs absorbance calibration curve. It should have a distinct
linear portion in which Beer-Lamberts law is followed.
6. Similarly treat the unknown samples and record their absorbance value with the help of
the spectrophotometer.
7. Extrapolate the absorbance of the unknown sample with calibration curve to know the
concentration in the unknown sample. Report the results in mg/L or ppm.
Page 35
ENVIRONMENTAL
ENV.
Chromium has a typical toxicity characteristic. It has two popular oxidation states in
the form of Cr3+ and Cr6+. Cr3+ is highly immobile in the ambient pH and temperature
range and therefore these compounds are not bioavailable.
Moreover very often trace Cr3+ compound is useful to human bodies. But the other
popular oxidation state of chromium as Cr6+ is highly soluble and bioavailable.
Hexavalent chromium is highly toxic and is s carcinogen. Effluents from metallurgical

industries, plating industries, chemical industries and tanneries, etc. contain
appreciable amount of Hexavalent chromium. Therefore these effluents are to be
suitable treated before discharging to water bodies.
Page 36

Finalenv Lab Manual

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Finalenv Lab Manual

Uploaded by

Copyright:

Available Formats

Institute of Technical Education & Research, SOA University

DEPARTMENT OF CIVIL ENGINEERING

Department of Civil Engineering, ITER, SOA University

pH of natural water depends on important natural phenomena like absorption of carbon

Temperature: Temperature is a very important physical parameter in water bodies. It

pH is very important in all important chemical and bio-chemical reactions.

Ambient pH of water supply should be within range of 6.5-8.5.

Very low pH < 6 affects human body.

Very low and very high pH cause material damage by corrosion.

pH is very important factor in biological waste water treatment.

High temperature lowers oxygen solubility.

Presence of objectionable colour and odour indicate the presence of undesirable

Department of Civil Engineering, ITER, SOA University

Solution I: Dissolve 5g of hydrazine sulphate (NH2)2H2SO4 into a 500 ml

Solution II: Dissolve accurately 50 g of hexamethylene tetramine (CH2)6N4 into a

Mix solution I and solution II to form formazine turbidity concentrate. Allow it to

Department of Civil Engineering, ITER, SOA University

Department of Civil Engineering, ITER, SOA University

Department of Civil Engineering, ITER, SOA University

Department of Civil Engineering, ITER, SOA University

Department of Civil Engineering, ITER, SOA University

These parameters must be within permissible limits of IS-10500.

Department of Civil Engineering, ITER, SOA University

Department of Civil Engineering, ITER, SOA University

Microbial activity in biological treatment is very sensitive to lower pH condition and

A minimum alkalinity in water is required to prevent material loss because of corrosion.

Department of Civil Engineering, ITER, SOA University

Carbon Dioxide (CO2) in a given sample of water/waste water.

Microbial decomposition particularly anaerobic decomposition in stagnant water bodies is

Titration valu in ml x 1000

Carbon Dioxide Acidity =

Titration valu in ml x 1000

Dissolution of CO2 in water bodies maintains a kind of dynamic equilibrium of

Department of Civil Engineering, ITER, SOA University

To determine the Magnesium and Calcium Hardness in a

given water sample.

These are capable of reacting with the

M2+ + EDTA = M-EDTA complex (solute)

= Titration value in ml (v1)

Calcium hardness in mg/L CaCO3 = Titration value in ml (v2)

Department of Civil Engineering, ITER, SOA University

To determine the optimum alum dosage in a given

Jar test apparatus

Department of Civil Engineering, ITER, SOA University

RESULT AND CALCULATION:

Optimum Coagulant Dosage requirement is to insure the effective coagulation and

Coagulation and sedimentation followed by filtration in water treatment should

Department of Civil Engineering, ITER, SOA University

Ca(OCl)2 + 2CH3COOH ---------------------- (CH3COO)2Ca + Cl2 + H2O

RESULT AND CALCULATION:

W mg of bleaching powder contains 3.55 mg of available chlorine

Bleaching powder is a popular disinfectant particularly for small-scale household

More over it is not stable and loses chlorine over time.

Therefore bleaching powder is not popular in large scale commercial application.

Department of Civil Engineering, ITER, SOA University

To determine the break point chlorine and chlorine

demand of a water sample.

RESULT AND CALCULATION:

Department of Civil Engineering, ITER, SOA University

In adequate chlorination does not lead to satisfactory disinfection. Whereas excess

Department of Civil Engineering, ITER, SOA University

Department of Civil Engineering, ITER, SOA University

7. Concentrated sulphuric acid

Department of Civil Engineering, ITER, SOA University