EE Lab Manual

T.K.M.
COLLEGE OF ENGINEERING
KOLLAM-5
DEPARTMENT OF CIVIL ENGINEERING

ENVIRONMENTAL ENGINEERING LAB MANUAL
Environmental Engineering Lab Manual
Department of Civil Engineering

PROGRAMME OUTCOMES
The programme is targeted at developing the following abilities amongst students:

PO 1. Apply knowledge of mathematics, science and engineering for the solution of Civil
Engineering problems.
PO 2. Identify, formulate and analyse Civil Engineering problems.
PO 3. Design Civil Engineering systems, components or process to meet desired needs
within realistic constraints.
PO 4. Conduct investigations of complex Civil Engineering problems using research
methods, design and conduct experiments, analyse data and arrive at valid conclusions.
PO 5. Use modern engineering tools and software necessary for solution of Civil
engineering problems.
PO 6. Assess societal, health, safety and legal issues relevant to professional engineering
practice.
PO 7. Understand the impact of engineering solutions in a global, economic, environmental
and societal context and understand the need for sustainable development.
PO 8. Acquire and demonstrate ethical principles required for professional practice.
PO 9. Function effectively as an individual and as a member in diverse teams.
PO 10. Communicate effectively in verbal, written and visual forms.
PO 11. Understand and demonstrate engineering and management principles required for
construction projects.
PO 12. Adapt to the technological advancements through life-long learning.
Department of Civil Engineering, TKMCE, Kollam Page i

Department of Civil Engineering

CE 431:Environmental Engineering Lab
COURSE OBJECTIVES
To equip the students in doing analysis of water and wastewater samples
EXPECTED OUTCOME
The students will be able to assess quality of water for various purposes
Department of Civil Engineering, TKMCE, Kollam Page ii

INSTRUCTIONS TO STUDENTS
1. Be regular and punctual to the laboratory sessions

2. Students must wear the lab coat inside the lab.
3. All students shall have the instruction manual and fair record as they come to the
class.
4. Be vigilant and careful while handling the glasswares and chemicals.
5. Do not crowd near the issue table.
6. After taking observations, return the apparatus to the technical staff.
7. Complete the calculations before leaving the class.
Attention
 In case of any emergency, notify the staff members
 First aid and drinking water are available in the laboratory.
 Do not litter the laboratory; maintain absolute discipline and cleanliness.
 Keep silence inside the class room.
SAFETY RULES
All laboratory users are required to know and abide by these rules
1. Always wear shoes that completely cover your feet and pants that completely cover
your legs
2. Do not wear bulky, loose or trailing clothes.
3. Tie back long hair.
4. Never lift objects that are heavier than you can safely handle. Always seek the
assistance of others in your group for lifting, carrying, positioning or adjusting heavy
equipment.
5. Use appropriate protective equipment. Gloves, when working with hot materials.
6. If a fire occurs and is small enough to fight use the fire extinguisher in the lab.
a. Pull the pin.
b. Aim at the bottom of the flames. Remember to be level with the flames.
c. Squeeze the handle.
d. Sweep back and forth.
7. Report faulty equipment to the technical staff and professor immediately. Do not use
it until it is inspected and declared safe.
8. Dry wet hand and clothing before working with electricity.
9. Stop machinery or equipment capable of movement before cleaning or adjusting.
10. Be as careful for the safety of others as for yourself. Think before you act.
11. Always wash your hands before leaving the lab.
Department of Civil Engineering, TKMCE, Kollam Page iii

CONTENTS
Sl. No
Title Page No.
1. Turbidity 1
2. Conductivity 2
3. pH 4
4. Acidity 5
5. Alkalinity 7
6. Chlorides 9
7. Sulphates 10
8. Nitrates 12
9. Phosphates 14
10. Total Iron 15
11. Total hardness 16
12. Sodium and Potassium 19
13. Solids 21
14. Optimum coagulant dosage 23
15. Dissolved Oxygen 25
16. Biochemical Oxygen Demand 27
17. Chemical Oxygen Demand 29
18. Most Probable Number (MPN) 31
19. Available chlorine 33
20. Break point Chlorination 35
Department of Civil Engineering, TKMCE, Kollam Page iv

1. TURBIDITY
AIM
To determine the turbidity of the given water sample
APPARATUS/ REAGENTS
Nephelometer, Sample cells
Dilution water, Stock primary standard formazin suspension, Dilute turbidity suspensions
THEORY
Turbidity in water is caused by suspended and colloidal matter such as clay, silt, finely
divided organic and inorganic matter, and plankton and other microscopic organisms.
Turbidity is an expression of the optical property that causes light to be scattered and
absorbed rather than transmitted with no change in direction or flux level through the sample.
Turbidimeters with scattered-light detectors located at 90° to the incident beam are called
nephelometers. A standard reference suspension having reproducible light-scattering
properties is specified for nephelometer calibration.
PROCEDURE
1. Calibrate the Nephelometer using standard suspension.
2. Gently agitate the sample and wait until air bubbles disappear.
3. Pour the samples in the sample cell and determine the turbidity.
RESULT
Turbidity of sample = NTU
Department of Civil Engineering, TKMCE, Kollam Page 1

2. CONDUCTIVITY
AIM
To determine the specific conductance of the given water sample
APPARATUS/ REAGENTS
Water Quality Analyzer, Conductivity cell, Beakers

Standard KCl solution (0.01 N), Distilled water
THEORY
The conductivity of a solution is a measure of its ability to transport an electric charge, and
varies both with the number and type of ions in the solution. Conductivity (or indirectly
specific conductance) can be measured in a conductivity cell connected to a Wheatstone
bridge circuit. Such an arrangement allows measurement of the electrical resistance provided
by the cell. The mathematical formulation of conductivity is given below:
E = IR, where E is the voltage, I is current, and R is the resistance.
R = ρL/A, where ρ is the specific resistance in ohm.cm, L is the length and A is the area.
The reciprocal of ρ is the specific conductance of the solution k, i.e., k = 1/ρ (in mho/cm units
or Siemen/cm).
In practice, a conductivity cell is calibrated by determining the resistance (Rs) of a standard
solution and from this, the cell constant(C) is determined as C = ksRs,,whereks is the specific
conductance of the standard solution. Usually, 0.01 N KCl,with a specific conductance (ks) of
1.4 mS/cm at 25° C, is used as the standard solution for this calibration.Then, the specific
conductance of an unknown sample can be determined by measuring its resistance, R.
PROCEDURE
1. Switch on the instrument by keeping the conductivity cell (cell constant 1.00) in distilled
water.
2. Connect the terminals of temperature probe to the instrument and dip it in water.
3. Select the EC mode shown on the display and enter the cell constant of 1.00
(approximately).
4. Place the electrodes in standard solution of 0.01 N KCl and observe the specific
conductance on the mini-monitor. For, 0.01 N KCl solution, the specific conductance
should be 1.409 mS/cm.
5. Rinse the electrode in distilled water and keep it in the unknown sample and measure the
conductivity. It is customary to select 25oC for EC measurements.

OBSERVATIONS
Specific conductance of standard KCl solution = mS/cm
Specific conductance of sample = mS/cm
RESULT
Specific conductance of the sample = mS/cm

3. pH
AIM
To determine the pH of the given water sample
APPARATUS/ REAGENTS
pH meter, Buffer solutions (pH 4, 7, 9), Beakers
THEORY
pH value is a measure of hydrogen ion concentration and is the negative exponent of the
logarithm of the hydrogen ion concentration. The pH value of natural water is an important
index of acidity or alkalinity. The pH of water may be determined potentiometrically using a
pH meter, the principle of which is that hydrogen ion activity is dependent on the potential
difference between the glass and reference electrodes. The electrodes are to be standardized
using standard buffer solutions before each measurement.
PROCEDURE
1. Calibrate the electrode with two standard buffer solutions of known pH.
2. Rinse the electrode thoroughly with deionized distilled water and carefully wipe with
a tissue paper.
3. Dip the electrodes into the sample solution, swirl the solution and wait up to one
minute for steady reading.
RESULT
pH of the sample = .................................

4. ACIDITY
AIM
To determine the acidity of the given water sample
APPARATUS/REAGENTS
Burette, pipette, measuring cylinders, conical flasks
Sodium Hydroxide (0.02 N), Phenolphthalein Indicator, Methyl Orange Indicator
THEORY
Acidity of water is its quantitative capacity to react with a strong base to a designated pH.The
main sources of acidity in water are hydrogen ions of strong acids (mineral acidity) and ions
of weak acids(carbon dioxide acidity). Acidity of the sample can be measured by neutralizing
it with standard alkali. The mineral acidity of the sample can be calculated by titrating the
sample with strong base to a pH of 4.5 with methyl orange as the indicator. The carbon
dioxide acidity is measured by titrating the sample to pH 8.3 with phenolphthalein as the
indicator (as shown in the Figure), which is accepted as standard end point for titration of
total acidity. Hence it is obvious that carbon dioxide is the main cause of acidity for water
with pH greater than 4 and mineral acids are the main cause for water with pH less than 4.
PROCEDURE
1. Transfer 100 mL of sample into a conical flask.

2. Add 2 drops of methyl orange indicator and titrate it until the colour changes from
orange to pale yellow. Note the burette reading (V1).
3. Add 2 drops of phenolphthalein indicator to the sample and continue titration until the
colour changes to pink. Note the burette reading (V2).
OBSERVATIONS
Sample Vol. of Sample Vol. of NaOH consumed (mL)

No. (mL)
Methyl Orange end Phenolphthalein end
Initial
point (V1) point (V2)

CALCULATIONS
Volume of sample =
Volume of NaOH for Mineral Acidity (V1) =
Volume of NaOH for Total Acidity (V2) =
Normality of NaOH (N) =
𝑉1 ×𝑁×𝐸𝑞.𝑤𝑡 𝑜𝑓 𝐶𝑎𝐶𝑂3 ×1000
Mineral Acidity in mg/L as CaCO3 = 𝑉𝑜𝑙 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑡𝑎𝑘𝑒𝑛

Total Acidity in mg/L as CaCO3 = 𝑉𝑜𝑙 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑡𝑎𝑘𝑒𝑛
RESULTS
Mineral acidity of the sample = mg/L

Total acidity of the sample = mg/L
Carbon dioxide acidity of the sample = mg/L

5. ALKALINITY
AIM
To determine alkalinity of the given water sample
APPARATUS/ REAGENTS
Standard sulphuric acid (0.02 N), Phenolphthalein Indicator, Methyl Orange Indicator
THEORY
Alkalinity of water is its acid-neutralizing capacity. Alkalinity of many surface waters is

primarily a function of hydroxide (pH>10), carbonate (pH between 10 and 8.3) and
bicarbonate (pH between 8.3 and 4.5) concentration (Figure). Alkalinity is measured
volumetrically by titration with 0.02 N sulphuric acid and reported in terms of equivalent
CaCO3. For samples whose initial pH is above 8.3, the titration is made in two steps. In the
first step pH is lowered to 8.3, at which phenolphthalein indicator changes colour from pink
to colourless. Beyond the phenolphthalein end point, the bicarbonate reacts with the acid and
is converted to carbonic acid. The reaction is essentially complete when the pH has been
lowered to 4.5 where methyl orange indicator changes colour from yellow to orange.
OH- + H+ → H2O
CO32- + H+ → HCO3-
HCO3- + H+ → H2CO3
Figure : pH range of alkalinity

PROCEDURE
1. Transfer 100 mL sample into a conical flask.
2. Add 2 drops of phenolphthalein indicator and titrate until the colour changes from
pink to colourless. Note the burette reading (V1).
3. Add 2 drops of methyl orange indicator to the sample and continue titration until the
colour changes from yellow to orange. Note the burette reading. (V2).
4. The different types of alkalinity can be obtained from the table given below:
Hydroxide alkalinity Carbonate alkalinity Bicarbonate Concentration
Result of as CaCO3 as CaCO3 as CaCO3
Titration
P=0 0 0 T
P < T/2 0 2P T - 2P
P = T/2 0 2P 0
P > T/2 2P - T 2(T – P) 0
P=T T 0 0
OBSERVATIONS
Sample Vol. of Sample Vol. ofSulphuric acid consumed (mL)

No. (mL)
Phenolphthalein end Methyl Orange end
Initial
point (V1) point (V2)
CALCULATIONS
Vol. of sample =
Vol. of acid for phenolphthalein end point (V1) =
Vol. of acid for Methyl orange end point (V2) =
Normality of acid (N) =
Phenolphthalein alkalinity, P = 𝑉𝑜𝑙 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑡𝑎𝑘𝑒𝑛
Total Alkalinity, T = 𝑉𝑜𝑙 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑡𝑎𝑘𝑒𝑛
(OH)- Alkalinity =
(CO3)2- Alkalinity =
(HCO3)- Alkalinity =
RESULTS
Phenolphthalein Alkalinity as CaCO3 (mg/L) =
Total Alkalinity as CaCO3 (mg/L) =
(OH)- Alkalinity as CaCO3 (mg/L) =
(CO3)2- Alkalinity as CaCO3 (mg/L) =
(HCO3)- Alkalinity as CaCO3 (mg/L) =

6. CHLORIDES
AIM
To determine the chloride content of the given water sample
APPARATUS/ REAGENTS
Std. Silver Nitrate Soln. (0.014 N), Potassium chromate indicator
THEORY
Chlorides are determined by the Mohr’s Method. Silver nitrate solution (0.014 N) reacts with
the chloride ion in the sample resulting in the formation of white silver chloride precipitate.
Ag+ + Cl- → AgCl (s)
Once all the chloride ions have been depleted from the sample, Silver nitrate combines with
potassium chromate to form silver chromate, which is reddish brown.
PROCEDURE
1. Transfer 100 mL of sample into a conical flask.

2. Add 2-3 drops of potassium chromate indicator solution and titrate it against standard
silver nitrate solution until colour changes from pure yellow to reddish brown.
3. Note the burette reading (V1).
4. Repeat the procedure for blank solution and obtain the burette reading (V2).
OBSERVATIONS
Sample No. Vol. of Sample (mL) Burette Reading Vol. of AgNO3 (mL)
Initial Final
CALCULATION
Volume of sample =
Volume of AgNO3 for sample (V1) =
Volume of AgNO3 for blank (V2) =
Normality of AgNO3 (N) =
(V1−V2)x N x Eq.wt of 𝐶𝑙 − x 1000
Amount of Chlorides =
Vol.of Sample taken
RESULT
Chlorides in the sample =

7. SULPHATES
AIM
To determine the amount of sulphates in the given water sample
APPARATUS/ REAGENTS
Barium chloride solution, hydrochloric acid (2N)
Crucible, Digital balance, Hot air oven, Muffle furnace, Whatman filter paper (ashless),
Desiccators
THEORY
Sulphate iron present in a definite volume of the given solution is precipitated as barium
sulphate by adding barium chloride solution in the presence of dilute hydrochloric acid.
K2SO4 +BaCl2 → BaSO4 +2KCl
From the mass of BaSO4, the mass of sulphate in the whole of the given solution is calculated
knowing that 233.36g of BaSO4 contain 96g of sulphate.
PROCEDURE
1. Make the potassium sulphate solution to 100 ml and pipette 20 ml of the made up
solution into a 250ml beaker.
2. Add 2N hydrochloric acid and dilute to 100ml with distilled water.
3. Heat the solution to boiling and add a hot solution of 5% barium chloride drop wise
with constant stirring.
4. Boil for about 5 minutes. Cool the mixture and test the supernatant liquid for
complete precipitation by adding a few drops of barium chloride solution through the
sides of the beaker.
5. Cover the beaker with glass and keep the solution hot but not boiling for half an hour
in order to allow time for complete precipitation.
6. Decant the clear solution through an ashless filter paper and wash the precipitate with
small portion of hot water until the filtrate is free from chloride ions.
7. Transfer the precipitate completely into the filter and keep in an oven for drying.
8. Note down the weight of the filter paper. Calculate the mass of sulphate in the whole
of the given solution from the mass of barium sulphate, knowing that 233.36 g of
barium sulphate contains 96g of sulphates.

CALCULATION
Mass of filter paper (g) =a

Mass of filter paper + barium sulphate (g) =b
Mass of barium sulphate (g) = (b – a)
233.36 g of barium sulphate contains 96 g of sulphate
96 (𝑏−𝑎)
(b-a) g of barium sulphate contains = g of sulphate
233.36
96 (𝑏−𝑎)5
Mass of sulphate in the given sample = g of sulphate
233.36
RESULT
Mass of sulphate in the given solution = g

8. NITRATE
AIM
To determine the concentration of nitrates in the given water sample
APPARATUS/REAGENTS
Ion meter, Beakers

Standard nitrate solution
THEORY
In water and wastewater the forms of nitrogen of greatest interest are, in order of decreasing
oxidation state, nitrate, nitrite, ammonia, and organic nitrogen. Nitrate generally occurs in
trace quantities in surface water but may attain high levels in groundwater and in the effluent
of nitrifying biological treatment plants. It is an essential nutrient for many photosynthetic
autotrophs and in some cases has been identified as the growth-limiting nutrient. In excessive
amounts, it contributes to the illness known as methemoglobinemia in infants.
The NO3 ion electrode is a selective sensor that develops a potential across a thin, porous,
inert membrane that holds in place a water-immiscible liquid ion exchanger. The electrode
responds to NO3 ion activity between about 10–5 and 10–1 M (0.14 to 1400 mg/L NO3). The
lower limit of detection is determined by the small but finite solubility of the liquid ion
exchanger.
PROCEDURE
Preparation of calibration curve:

1. Transfer 10 mL of 1 mg/L NO3 standard to a 50 mL beaker, add 10 mL buffer, and
stir with a magnetic stirrer.
2. Immerse tips of electrodes and record millivolt reading when stable (after about 1
min).
3. Remove electrodes, rinse, and blot dry. Repeat for 10 mg/L NO3 and 50 mg/L
standards.
4. Plot potential measurements against NO3 concentration on semi-logarithmic graph
paper, with NO3 concentration on the logarithmic axis and potential (in millivolts) on
the linear axis (ordinate).
Measurement of sample:
1. Transfer 10 mL sample to a 50 mL beaker, add 10 mL buffer solution, and stir (for
about 1 min) with a magnetic stirrer.
2. Immerse electrode tips in sample and record potential reading when stable (after about
1 min). (Measure standards and samples at about the same temperature.)
3. Read concentration from calibration curve.

OBSERVATIONS
Calibration
Sample No. Concentration (mg/L) Electrode potential
Electrode potential of the sample = mV
RESULTS
Nitrate concentration in the given sample = mg/L

9. PHOSPHATE
AIM
To determine the concentration of phosphates in the given water sample
APPARATUS/REAGENTS
Pipette, flask, measuring cylinder, spectrophotometer
Ammonium molybdate, stannous chloride (SnCl2), and stock phosphate solution (50 ppm)
THEORY
Phosphate is primarily used in biological system as an energy conduit. In water, phosphate is

incorporated in organic matter. Phosphate can be determined by spectrophotometric method
at 690 nm. When ammonium molybdate reacts with phosphate in acidic condition
phosphomolybdic acid will be formed which upon reduction with SnCl2 yields abluecolour.
Arsenate and silicate may act as interference to this method as these ions have similar
characteristics as that of phosphate.
PROCEDURE
1. Prepare 100 mL standard solutions in the concentration range of 0.2 – 1.8 mg/L (0.2,
0.4, 0.6…).
2. Take 100 mL sample in a beaker.
3. Add 4 mL ammonium molybdate to each of the beakers.
4. Add 10 drops of SnCl2 to the beakers. Mix well and keep aside for 5 min for colour
development.
5. Measure the colour intensity in spectrophotometer at 690 nm and plot calibration
curve and find the phosphate concentration in the sample.
OBSERVATIONS
Sample No. Concentration (mg/L) Absorbance
Absorbance of unknown sample =
CALCULATIONS
Prepare the calibration curve and obtain the concentration of phosphates of unknown sample.
RESULTS
Concentration of phosphate in the sample = mg/L

10. TOTAL IRON

AIM
To determine the iron content of a water sample
APPARATUS/REAGENTS
Nesslers tube (100 mL), pipette, burette

DilHCl, potassium permanganate, potassium thiocyanate, Mohr’s salt (Ferrous ammonium
sulphate)
THEORY
Iron can be estimated in laboratory by colorimetric method. In this method ferrous form of
iron is converted to ferric form by reactionwith dil. HCl and potassium permanganate. This is
then allowed to react with potassium thiocyanate to form a brown coloured complex. The
intensity of the colour developed is proportional to the concentration of Iron.
PROCEDURE
1. Take 100 mL of sample in Nessler’s tube 1 and 100 mL of distilled water in Nessler’s
tube 2.
2. Add 1 mL dil. HCl to both the solutions
3. Add 2-3 drops of KMnO4 to both the tubes. The colourof the solutions changes to
purple.
4. Add 5 mL potassium thiocyanate to both the tubes and keep aside for 5 min.
5. Brown colouris developed in Nessler’s tube 1 whereas the solution in Nessler’s tube 2
remainscolourless.
6. Titrate the solution in Nessler’s tube 2 against Ferrous Ammonium Sulphate (FAS)
till the intensity of colour developed is same as that in Nesslers tube 1. Note the
volume of FAS used.
OBSERVATIONS
Sample No. Volume of sample (mL) Burette reading Volume of FAS used (mL)
Initial Final
CALCULATIONS
1 mL of FAS = 0.1 mg of Fe2+
RESULTS
Concentration of Iron = mg/L

11. TOTAL HARDNESS

AIM
To determine the total hardness, calcium and magnesium hardness of the given water
samples, by using Ethylene Diamine Tetra Acetic acid (EDTA) titrimetric method.
APPARATUS/REAGENTS
Burette, pipettes, measuring jars, beakers, erlenmeyer flasks.
Standard EDTA solution (0.01 M), Ammonia buffer solution, Eriochrome black-T indicator,
Muroxide indicator, Sodium hydroxide solution (1N NaOH)
THEORY
Hardness is caused by divalent metallic cations. Such ions are capable of reacting with soap
to form precipitate and with certain anions present in the water to form scale. The principal
hardness-causing cations are calcium, magnesium, strontium, ferrous and mangenous.
Aluminium and ferric ions are sometimes considered as contributing to the hardness of water.
However, their solubility is so limited at the pH values of natural waters that ionic
concentrations are negligible. The following table shows principal cations and anions
associated with them:
Cations causing hardness Ca2+ Mg2+ Sr2+ Fe2+ Mn2+

Anions HCO3- SO42- Cl- NO3- SiO32-
The hardness in water is derived largely from contact with soil and rock formations. The
ability to dissolve many substances in soil is gained when carbon dioxide is released by
bacterial action. Water is commonly classified in terms of the degree of hardness, as follows.
Degree of hardness Soft Moderately hard Hard Very hard

mg/l <75 75-150 150-300 >300
Hardness of water is an important consideration in determining the suitability of water for

domestic and industrial uses. Hard waters are less preferredby humans than soft waters.
Hardness is determined using EDTA titrimetric method. Eriochrome Black T (EBT), which is
used as the indicator, forms weak complex with divalent hardness causing ions at a pH >10.
During titration with EDTA, it disrupts the weak complex and form stable complex with
hardness causing ions.

PROCEDURE
a) Total Hardness:
1. Transfer 100 mL of water sample to a clean erlenmeyer flask and add 2 mL of
ammonia buffer solution and vigorously shake for about 10 to 20 seconds.
2. Add 2 drops of Eriochrome Black T indicator solution (or a pinch of the indicator
powder) to the solution and mix well.
3. Observe the change in colour (usually wine red colour appears) and titrate the mixture
against standard EDTA solution upto a point at which wine red colour changes to
blue.
b) Calcium Hardness
1. Transfer 100 mL of given water sample to a clean erlenmeyer flask and add 4 mL of
1N NaOH solution and a pinch of muroxide indicator.
2. Vigorously shake well for about 10 to 20 seconds and then titrate the pink coloured
mixture against standard EDTA solution until colour changes to purple.
OBSERVATIONS
Sample No.
Burette readings for total hardness Burette readings for calcium hardness
Volume consumed Volume consumed
Initial Final Initial Final
(mL) (mL)
T= mL C= mL

CALCULATIONS
T × Molarity of EDTA × Molecular weight of CaCO3 × 1000

Total Hardness =
Volume of Sample
C × Molarity of EDTA × Molecular weight of CaCO3 × 1000

Calcium Hardness =
Volume of Sample
Magnesium Hardness = Total Hardness − Calcium Hardness
Calcium Hardness × Molecular Weight of Ca

Concentration of Calcium =
Molecular Weight of CaCO3
Magnesium Hardness × Molecular Weight of Mg

Concentration of Magnesium =
Molecular Weight of CaCO3
RESULTS
Calcium hardness = mg/L as CaCO3
Magnesium hardness = mg/L as CaCO3
Total hardness = mg/L as CaCO3
Concentration of calcium = mg/L as Ca2+
Concentration of magnesium = mg/L as Mg2+

12. SODIUM AND POTASSIUM

AIM
To determine the concentration of Sodium and Potassium in water samples
APPARATUS/REAGENTS
Flame Photometer, beakers
NaCl, KCl
THEORY
Sodium is present in nearly all natural waters; relatively high concentrations may be found in
brines and hard water softened by sodium exchange process. Ratio of sodium to total cations
is important in agriculture and human pathology. Soil permeability can
beadverselyaffectedby a high sodium ratio. High pressure boilers require feed water with less
than 3 mg/L sodium to sustain efficient operation. Potassium ranks seventh among the
elements in order of abundance, yet its concentration in most drinking waters seldom reaches
20 kg/L. However, occasional brines contain more than 100 mg/L potassium.
Flame photometry is an elegant method of rapid analysis of sodium and potassium. These
chemical elements provide a flame of gas with a characteristic colouring at a wavelength of
589 and 766.5 nm for sodium and potassium respectively. A test solution is atomized and
blown into the gas burner and the intensity of colour lines of the spectrum isolated by filters
is measured by a photocell. This is a measure of the concentration of the element.
PROCEDURE
(i) Preparation of Stock Solutions

Sodium: 1000 ppm: Dissolve 2.5416 g NaCl in one litre of distilled water.
Potassium: 1000 ppm: Dissolve 1.886 g KCl in one litre of distilled water.
(ii) Calibration of the instrument and analysis of unknown samples
1. Select the appropriate filter (Na or K) from SET FLAME option.
2. Select the desired no. of standards and enter the concentration for both the ions and
run the calibration.
3. Start the analysis for unknown samples and aspire distilled water alternatively. Note
down the concentrations of ions.

OBSERVATIONS
Concentration of Sodium = mg/L
Concentration of Potassium = mg/L
RESULT
Concentration of Sodium = mg/L

Concentration of Potassium = mg/L

13. SOLIDS
AIM
To analyse the various types of solids in a given water sample
APPARATUS/REAGENTS
Crucible, Digital balance, Hot air oven, Muffle furnace, Whatman filter paper, Desiccators
THEORY
Solids refer to matter suspended or dissolved in water or wastewater. Water high in

suspended solids may be aesthetically unsatisfactory for such purposes as bathing. Water
with high dissolved solids tend to stain glass wares and has adverse impacts on irrigated
crops, plants and grasses.
‘‘Total solids’’ is the term applied to the material residue left in the vessel after evaporation
of a sample and its subsequent drying in an oven at a defined temperature. Total solids
includes ‘‘total suspended solids,’’ the portion of total solids retained by a filter, and ‘‘total
dissolved solids,’’ the portion that passes through the filter.
‘‘Fixed solids’’ is the term applied to the residue of total, suspended, or dissolved solids after
heating to dryness for a specified time at a specified temperature. The weight loss on ignition
is called ‘‘volatile solids.’’ Determinations of fixed and volatile solids do not distinguish
precisely between inorganic and organic matter because the loss on ignition is not confined to
organic matter. It includes losses due to decomposition or volatilization of some mineral
salts. ‘‘Settleable solids’’ is the term applied to the material settling out of suspension within
a defined period. It may include floating material.
PROCEDURE
Total Solids
1. Note down the empty weight of the dish (W1)

2. Pour 20 mL of well mixed sample into it and evaporate the water content at 103 to
105 oC in a hot air oven till it is completely dry.
3. After complete evaporation, take out the dish from the oven using tongs and cool it in
a desiccator to facilitate cooling in a dry atmosphere.
4. Weigh the dish as soon as it is completely cooled (W2)
Total Fixed solids
1. Keep the dish used for determining total residue in a muffle furnace for 30 minutes at
550 oC.
2. Cool the crucible in a desiccator and weigh it with the solids residue (W3).

Total Dissolved solids
1. Note down the empty weight of the dish (W4).

2. Filter 20 mL of sample through a filter paper and collect the filtrate in the dish.
3. Transfer the dish to a hot air oven maintained at 103 to 105 oC till it is completely dry.
4. After complete evaporation, take out the dish from the oven using tongs, cool it in a
dessicator and weigh it (W5).
OBSERVATIONS AND CALCULATIONS
1) Total Solids, Fixed solids, Volatile Solids

Volume of sample taken =
Weight of empty crucible (W1) =
Weight of crucible after heating in hot air oven (W2) =
Weight of crucible after heating in muffle furnace (W3) =
Total Solids (mg/L) = (W2- W1) x 106 / Vol. of sample =
Fixed solids (mg/L) = (W3- W1) x 106 / Vol. of sample =
Volatile solids (mg/L) = Total solids – fixed solids =
2) Vol. of filtered sample taken =
Weight of empty crucible (W4) =
Weight of crucible after heating in hot air oven (W5) =
Dissolved Solids (mg/L) = (W5- W4) x 106 / Vol. of sample =
Suspended solids (mg/L) = Total Solids – Dissolved solids =
RESULTS
Total Solids = mg/L
Total Suspended solids = mg/L
Total Dissolved solids = mg/L
Total Fixed solids = mg/L
Total Volatile Solids = mg/L

14. OPTIMUM COAGULANT DOSE

AIM
To determine the optimum coagulant dose to treat the given turbid water sample
APPARATUS/REAGENTS
Jar-test apparatus, Nephelometer, beakers of 1 L capacity, measuring jars.
Filter alum solution of known strength (1 mL = 10 mg of Alum), standard turbid solution (a

mixture of hydrazine sulphate and hexamethylene – tetramine) of turbidity 40 NTU (Nephelo
Turbidity Units)
THEORY
Coagulation – flocculation – sedimentation processes is commonly employed for removal of
colloidal solids from water. Filter alum is the best coagulant generally applicable in the water
treatment schemes to remove the turbid particles effectively. The various factors affecting the
removal of turbidity are: type and dosage of coagulant, nature and amount of turbid particles,
effectiveness of mixing of coagulant, pH, temperature, and alkalinity of water to be treated.
Therefore, it is essential to determine the optimum coagulant dose, which renders maximum
turbidity removal at lower dosage of coagulant. The “Jar Test Apparatus” (with 4 or 6 jar
capacity) is generally used to assess the optimum coagulant dose experimentally. Jar test
apparatus sequentially simulates rapid mixing, coagulation, flocculation, and sedimentation
processes adopted in water treatment technology.
PROCEDURE
1. Transfer approximately 1 L of turbid water sample into the six or four beakers of
1 L capacity (while drawing the sample, as far as possible do not collect the
floating and settleable solids).
2. Add predetermined amounts or dosage of filter alum solution into the respectively
marked beakers.
3. Place the beakers accordingly in the Jar Test Apparatus and switch on the
respective switches. Adjust the number of rotations of blades to around 60 to 80
rpm and after 2 minutes, reduce the speed to about 10 rpm and continue the same
upto 20 minutes. Intermittently, observe the formation of flocs in the beakers.
4. After 20 minutes, stop the motor, and allow the so formed flocs to settle by giving
a detention time of 30 minutes.
5. Determine the turbidity of the supernatant liquid using Nephelometer.

OBSERVATIONS
Initial turbidity of the given turbid water sample = NTU
Amount of alum Alum Final turbidity
Sample % Turbidity
solution added, dose, (after treatment),
No. removal
mL mg/L NTU
CALCULATIONS
Plot a graph between % turbidity removal vs alum dose and obtain the optimum coagulant
dose corresponding to maximum turbidity removal as shown in the Fig. below:
RESULTS
Optimum coagulant dose = mg/L.

15. DISSOLVED OXYGEN

AIM
To determine the Dissolved Oxygen (DO) content of a given water sample
APPARATUS/REAGENTS
BOD bottle, pipette, burette, erlenmeyer flask

Manganous sulphate, Alkali-iodide-azide reagent, Conc. H2SO4, Sodium thiosulphate
solution (0.025 N), starch solution
THEORY
Dissolved oxygen levels in natural and wastewaters depend on the physical, chemical, and
biochemical activities in the water body. DO of water is estimated using the Winkler’s
method (Iodometric titration). It is based on the addition of divalent manganese solution,
followed by strong alkali, to the sample in a glass-stoppered bottle. DO rapidly oxidizes an
equivalent amount of the dispersed divalent manganous hydroxide precipitate to hydroxides
of higher valency states. In the presence of iodide ions in an acidic solution, the oxidized
manganese reverts to the divalent state, with the liberation of iodine equivalent to the original
DO content. The iodine is then titrated with a standard solution of thiosulfate. The titration
end point can be detected visually, with a starch indicator.
Mn2+ + 2OH- +0.5O2 → MnO2 (brown hydrated precipitate) + H2O

Mn(OH)2 +0.5O2 → MnO2 +H2O
MnO2 +2I- + 4H+→ Mn2+ +I2 +2H2O
I2 +I- → I3–
In this method, the interference by nitrite may lead to erroneous results. Hence, modified
Winkler’s method is used in which the nitrite interference is overcome with use of sodium
azide (NaN3), which is incorporated in the alkali-KI reagent. When sulphuric acid is added,
following reactions happen:
NaN3 + H+→ HN3 + Na+

HN3 +NO2- + H+→ N2 +N2O+H2O
PROCEDURE
1. To the sample collected in a 300 mL bottle, add 2 mL MnSO4 solution, followed by 2

mL alkali-iodide-azide reagent. Mix thoroughly by inverting several times.
2. When precipitate has settled sufficiently (to approximately half the bottle volume),
add 2 mL conc. H2SO4. Restopper and mix by inverting several times until dissolution
is complete.
3. Transfer 203 mL of the sample to an Erlenmeyer flask and titrate with 0.025N
Sodium thiosulphate solution to a pale straw colour.

4. Add a few drops of starch solution and continue titration to first disappearance of blue
colour.
OBSERVATIONS
Sample No. Volume of Sample Burette reading Volume of sodium thiosuplhate used
(mL) (mL)
Initial Final
CALCULATIONS
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑖𝑜𝑠𝑢𝑙𝑝ℎ𝑎𝑡𝑒×𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦×𝐸𝑞.𝑊𝑡.𝑜𝑓 𝑜𝑥𝑦𝑔𝑒𝑛×1000
DO of the given sample =
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑢𝑠𝑒𝑑
RESULTS
The dissolved oxygen content of the given water sample = mg/L

16. BIOCHEMICAL OXYGEN DEMAND

AIM
To determine the BOD of a given wastewater sample
APPARATUS/REAGENTS
BOD bottle, BOD incubator, pipette, burette, erlenmeyer flask
Phosphate buffer, MgSO4 solution, CaCl2 solution, FeCl3.6H2O solution, MnSO4, Alkali-
iodide-azide reagent, Conc. H2SO4, Sodium thiosulphate solution (0.025 N), starch solution
THEORY
The biochemical oxygen demand (BOD) is an index of the biodegradable organics present in
wastewater samples. BOD determination is an empirical test in which standardized laboratory
procedures are used to determine the relative oxygen requirements of wastewaters, effluents
and polluted waters. The BOD concentration in most wastewaters exceeds the concentration
of dissolved oxygen (DO) available in an air-saturated sample. Therefore, it is necessary to
dilute the sample before incubation to bring the oxygen demand. Because bacterial growth
requires nutrients such as nitrogen, phosphorus, and trace metals, these are added to the
dilution water, which is buffered to ensure that the pH of the incubated sample remains in a
range suitable for bacterial growth. Complete stabilization of a sample may require a period
of incubation too long for practical purposes; therefore, the standard incubation period is
accepted as 5 days.
For determining the BOD of a wastewater sample, the initial DO of the diluted sample is
determined using Winkler’s method. The final DO of the sample after incubation for 5 days
at a specified temperature is measured. The BOD is computed as the difference between
initial and final DO.
PROCEDURE
Preparation of dilution water
1. Place desired volume of aerated water and add 1 mL each of phosphate buffer,
MgSO4, CaCl2, and FeCl3 solutions/L of water.
2. Seed the dilution water by adding 1 mL/L of the effluent or mixed liquor from a
biological treatment system processing the waste.
Preparation of sample
3. Make 2 sets of 5 dilutions of sample using the prepared dilution water (use the
following dilutions: 0.0 to 1.0% for strong industrial wastes, 1 to 5% for raw and
settled wastewater, 5 to 25% for biologically treated effluent, and 25 to 100% for
polluted river waters).
4. Determine the initial DO of one set of samples and blank (seeded dilution water)
5. Incubate the BOD bottles at 20°C ± 1°Cfor 5 days.

6. Determine the final DO of the incubated samples and blank.
OBSERVATIONS
Sample No. Dilution factor, p Initial DO (mg/L) Final DO (mg/L)
CALCULATIONS
(𝐷𝑂0 − 𝐷𝑂5 ) − 𝑓 × (𝐵0 − 𝐵5 )
𝐵𝑂𝐷5 =
𝑝
where BOD5 is the 5 day BOD

DO0 and DO5 are the Dissolved oxygen content of diluted sample at 0 and 5 day respectively
B0 and B5 are the Dissolved oxygen content of blank at 0 and 5 day respectively
F is the volume of seed in diluted sample/volume of seed in seed control
p is dilution factor
RESULTS
BOD of the given sample = mg/L

17. CHEMICAL OXYGEN DEMAND

AIM
To determine the COD of a given wastewater sample
APPARATUS/REAGENTS
Pipette, COD vials, COD digester, spectrophotometer
Digestion solution, sulphuric acid reagent, potassium hydrogen phthalate (KHP) solution
THEORY
Chemical oxygen demand (COD) is a measure of the oxygen equivalent of the materials
present in wastewater that are subject to oxidation by a strong chemical oxidant. The quantity
of oxidant consumed is expressed in terms of its oxygen equivalence. Because of its unique
chemical properties, the dichromate ion (Cr2O72–) is the specified oxidant. When a sample is
digested, the dichromate ion oxidizes COD material in the sample. This results in the change
of chromium from the hexavalent (VI) state to the trivalent (III) state. Both of these
chromium species are coloured and absorb in the visible region of the spectrum. The
dichromate ion (Cr2O7 2–) absorbs strongly in the 400-nm region, where the chromic ion
(Cr3+) absorption is much less. The chromic ion absorbs strongly in the 600-nm region, where
the dichromate has nearly zero absorption. For COD values between 100 and 900 mg/L,
increase in Cr3+ in the 600-nm region is determined. Higher values can be obtained by sample
dilution. COD values of 90 mg/L or less can be determined by following the decrease in
Cr2O7 2– at 420 nm.
PROCEDURE
1. Prepare five dilutions of KHP solutions in the required range (for calibration).
2. Place 2.5 mL each of the diluted KHP and samples for COD determination in the
COD vials and add precisely 1.5 mL digestion solution.
3. Carefully run 3.5mL sulphuric acid reagent down inside of vessel so an acid layer is
formed under the sample-digestion solution layer.
4. Tightly cap tubes or seal ampules, and invert each several times to mix completely.
5. Keep the vials in the COD digester preheated to 150°C and reflux for 2 h behind a
protective shield.
6. Cool sample to room temperature slowly to avoid precipitate formation.
7. Individually transfer each standard and sample to the sample cuvette and measure
absorption of each sample blank and standard at selected wavelength (420 nm or 600
nm). At 600 nm, use digested blank as the reference solution and at 420 nm, use
reagent water as the reference solution.

OBSERVATIONS
Calibration
Sample No. Concentration (mg/L) Absorbance
COD of Sample
Sample No. Absorbance
CALCULATIONS
Plot calibration curve and calculate the COD of the sample from the curve.
RESULTS
COD of the given sample = mg/L

18. MOST PROBABLE NUMBER (MPN)
AIM
To determine the most probable number in water samples using Multiple Tube Fermentation
Technique
APPARATUS/REAGENTS
Fermentation tubes, inoculum wire loops, durham vials, cotton plug, bacteriological
incubator, pipettes, other minor glass ware.
Lauryl Tryptose Broth, Brilliant green lactose bile broth
THEORY
Coliform group comprises of all facultative anaerobic, gram-negative, non-spore forming,

rod-shaped bacteria that ferment lactose with gas and acid formation within 48 hours at 350
C. The standard test for this group may be carried out either by Multiple Tube Fermentation
Technique (MTFT) or Membrane Filtration Technique (MFT). When MTFT is adopted,
results of the examination of replicate tubes and dilutions are reported in terms of Most
Probable Number (MPN) of organisms present, which is based on certain probability
formulas. The MTFT is applicable to the analysis of salt or brackish waters, muds, sediments
and sludges.
PROCEDURE
(i) Presumptive Test
1. Arrange fermentation tubes containing inverted durham vials in rows of five each in a
test tube rack. The number of rows and sample volumes selected depend upon the
quality and character of water to be examined. For potable water, use five 20 mL
portions, ten 10 mL portions or a single bottle of 100 mL portion; for non-potable
water, use five tubes of 10 mL, 1 mL and 0.1 mL each portion of water sample. For
10 mL portions, use fermentation tubes containing 10 mL double strength lauryl
tryptose broth and for 1 mL and 0.1 mL, use single strength medium.
2. Plug the tubes with cotton and incubate at 350 C ± 0.50 C for 24 ± 2 h. After the
incubation period, shake each tube gently and examine the production of acid or gas.
The tubes without gas formation are reincubated and reexamined at the end of 48 ±
3h.
3. Record the presence or absence of gas formation for each dilution. Production of gas
or acid within 48 ± 3h constitutes a positive presumption reaction. Submit all tubes
with a positive presumptive reaction to the confirmed phase.
(ii) Confirmed Test
1. Gently shake primary fermentation tubes showing gas formation and transfer one or
more loop full of medium using a sterile inoculum loop to the fermentation tubes
containing brilliant green lactose bile broth with inverted durham vials.

2. Incubate the inoculated tubes at 35 ± 0.50 C. Formation of gas in the inverted vial
within 48 ± 3h constitutes a positive confirmed test.
3. Calculate the MPN value from standard chart.
RESULT
The MPN of the given water sample = /100 mL.

19. AVAILABLE CHLORINE
AIM
To determine the percentage of available chlorine in the given bleaching powder sample by
iodometric method.
APPARATUS/REAGENTS
BOD bottles, measuring jars, burette, pipette, erlenmeyer flasks
Standard bleaching powder solution (1 mL of bleaching powder solution = 1 mg of bleaching

powder), Sodium thiosulphate solution (0.1 N), Concentrated acetic acid, Potassium iodide
crystals, Starch solution as indicator.
THEORY
The prime purpose of chlorinating public water supplies and wastewater effluents is to
prevent the spread of waterborne diseases. Chlorine is used in the form of free chlorine or as
hypochlorites. In either form, it acts as a potent oxidizing agent and often dissipates itself in
side reactions so rapidly that little disinfection is accomplished until amounts in excess of the
chlorine demand have been added. Bleaching powder (BP) is generally adopted as a
disinfecting agent because of its cost effectiveness and easiness in handling feeding devices.
An ordinary BP generally contains 25 to 35% of chlorine, which is a low level of availability
and also it loses 5 to 10% of chlorine every year. Hence, before using BP as disinfectant, the
chlorine available should be known. In India, calcium hypochlorite is most popularly used in
treatment practices.
Chlorine can be determined using iodometric method. Chlorine will liberate free iodine from
potassium iodide (KI) solutions at pH 8 or less. The liberated iodine is titrated with a standard
solution of sodium thiosulfate (Na2S2O3) with starch as the indicator. Titrate at pH 3 to 4
because the reaction is not stoichiometric at neutral pH due to partial oxidation of thiosulfate
to sulfate.
𝐶𝑙2 + 2𝐼− → 𝐼2 + 𝐶𝑙−
𝐼2 + 𝑆𝑡𝑎𝑟𝑐ℎ → 𝐵𝑙𝑢𝑒 𝑐𝑜𝑙𝑜𝑢𝑟
𝐼2 + 𝑆2 𝑂2− 2−
3 → 𝑆4 𝑂6 + 2𝐼
−
PROCEDURE
1. Transfer 100 mL of BP solution into a BOD bottle.
2. Add 5 mL of concentrated acetic acid and approximately 1 g of KI crystals, mix well
and stopper the bottle.
3. After a reaction time of 20 minutes, transfer the entire solution into an erlenmeyer
flask and add approximately 1 mL of starch solution.
4. Titrate the mixture against 0.1 N sodium thiosulphate solution until blue colour
completely disappears.
OBSERVATIONS
Sample No. Burette reading Volume consumed (mL)

Initial Final
CALCULATIONS
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑁𝑎2 𝑆2 𝑂3 × 𝑁 𝑜𝑓𝑁𝑎2 𝑆2 𝑂3 × 𝐸𝑞. 𝑤𝑡 𝑜𝑓 𝐶𝑙2 × 1000

𝐴𝑣𝑎𝑖𝑙𝑎𝑏𝑙𝑒 𝑐ℎ𝑙𝑜𝑟𝑖𝑛𝑒 =
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑢𝑠𝑒𝑑
𝐴𝑣𝑎𝑖𝑙𝑎𝑏𝑙𝑒 𝑐ℎ𝑙𝑜𝑟𝑖𝑛𝑒 𝑖𝑛 𝑚𝑔/𝐿

𝑃𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑎𝑣𝑎𝑖𝑙𝑎𝑏𝑙𝑒 𝑐ℎ𝑙𝑜𝑟𝑖𝑛𝑒 = × 100
1000
RESULTS
Available chlorine in bleaching powder = %
Available chlorine in bleaching powder solution = mg/L as Cl2

20. BREAKPOINT CHLORINATION
AIM
To determine the break-point chlorination and chlorine demand of the given polluted water
sample
APPARATUS/REAGENTS
BOD bottles, measuring jars, erlenmeyer flasks, burette, pipettes
Standard bleaching powder solution (strength: 1 ml of BP solution = 1 mg of BP), Sodium

thiosulphate solution (0.01 N), Potassium iodide crystals, Concentrated acetic acid, Starch
indicator.
THEORY
The chlorination of water supplies and polluted water serve primarily to destroy or deactivate
disease-producing microorganisms. A secondary benefit of chlorination is the overall
improvement in water quality resulting from the reaction of chlorine with ammonia, iron,
manganese, sulfide, and some organic substances. Usually, chlorine, hypochlorous acid, and
hypochlorite ion are referred to as free chlorine residuals, and the chloramines are called
combined chlorine residuals. The formation of HOCl over OCl- under an appropriate pH is
more effective for disinfection. The action of excess chlorine on water containing ammonia
merits special consideration. With mole ratios of Cl2 to NH3upto 1.1, both monochloramine
and dichloramine are formed. Chlorination of water to the extent that all the ammonia is
converted to N2 or higher oxidation state is referred to as break point chlorination. The break
point chlorination is required to obtain free chlorine residual for better disinfection if
ammonia is present in a water supply system. While free chlorine residuals have good
disinfecting powers; they are usually dissipated quickly in the distribution system. For this
reason, final treatment with ammonia is often practiced to convert free chlorine residuals to
longer lasting combined Cl2 residuals.
Chlorine demand of water is the difference between the amount of Cl2 applied and the
amount of free, combined, or total available chlorine remaining at the end of the contact
period. The Cl2 demand is different for different water and depends on the desired residual,
time of contact, pH, and temperature. Determination of the Cl2 demand of water or
wastewater is an important consideration in design. It serves as the basis for determining the
number and capacity of chlorinators required, the amount of Cl2 needed, the type of shipping
containers, and all appurtenances required for handling and storage.
For obtaining the chlorine demand of a sample, different dosages of bleaching powder are
added to the sample and the chlorine remaining in the solution after the reaction time is
determined using iodometric method. A graph is plotted between applied chlorine and
residual chlorine and the breakpoint chlorination can be obtained at point C of the curve as
shown in the Figure.

Figure: Schematic representation of Breakpoint Chlorination Curve

PROCEDURE
1. Transfer 100 ml of the given polluted sample into each of the BOD bottles of capacity
300 ml and add different dosages of bleaching powder solution of known strength
(i.e., 1 ml of BP solution = 1 mg of BP) to the respective marked bottles.
2. Mix thoroughly and after a contact time of 45 min, transfer the entire volume into an
erlenmeyer flask and analyse for residual chlorine present (i.e., amount of Cl2
remaining in the solution) iodometrically.
OBSERVATIONS
Sample Volume of BP solution added Volume consumed
Burette reading
No. (mL) (mL)
Initial Final
CALCULATIONS
a) Calculation of residual chlorine
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑁𝑎2 𝑆2 𝑂3 × 𝑁 𝑜𝑓𝑁𝑎2 𝑆2 𝑂3 × 𝐸𝑞. 𝑤𝑡 𝑜𝑓 𝐶𝑙2 × 1000

𝑅𝑒𝑠𝑖𝑑𝑢𝑎𝑙 𝑐ℎ𝑙𝑜𝑟𝑖𝑛𝑒 =
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑢𝑠𝑒𝑑

b) Calculation of applied chlorine data
y mL
BP stock solution Bottle with polluted

(x mg/L) water
Applied Cl2 in sample = (xy)/(100+y)
where x is the available chlorine in BP and y is the dosage of BP solution.
c) Determination of breakpoint chlorination
Volume of BP Residual Applied Chlorine

Sample Volume of
solution chlorine, chlorine, demand, Remarks
No. titrant, mL
added, y (mL) mg/L mg/L mg/L
Plot the breakpoint chlorination curve between applied chlorine and residual chlorine and
obtain a minimum chlorine demand.
Minimum chlorine demand = mg/L
RESULTS
The chlorine demand of the polluted water sample = mg/L

EE Lab Manual

Uploaded by

Document Information

Original Description:

Original Title

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

EE Lab Manual

Uploaded by

Copyright:

Available Formats

T.K.M.

DEPARTMENT OF CIVIL ENGINEERING

Department of Civil Engineering

The programme is targeted at developing the following abilities amongst students:

Department of Civil Engineering, TKMCE, Kollam Page i

Department of Civil Engineering

To equip the students in doing analysis of water and wastewater samples

Department of Civil Engineering, TKMCE, Kollam Page ii

1. Be regular and punctual to the laboratory sessions

Department of Civil Engineering, TKMCE, Kollam Page iii

Department of Civil Engineering, TKMCE, Kollam Page iv

To determine the turbidity of the given water sample

Nephelometer, Sample cells

Department of Civil Engineering, TKMCE, Kollam Page 1

To determine the specific conductance of the given water sample

Water Quality Analyzer, Conductivity cell, Beakers

Department of Civil Engineering, TKMCE, Kollam Page 2

Specific conductance of the sample = mS/cm

Department of Civil Engineering, TKMCE, Kollam Page 3

To determine the pH of the given water sample

pH meter, Buffer solutions (pH 4, 7, 9), Beakers

pH of the sample = .................................

Department of Civil Engineering, TKMCE, Kollam Page 4

To determine the acidity of the given water sample

Burette, pipette, measuring cylinders, conical flasks

Sodium Hydroxide (0.02 N), Phenolphthalein Indicator, Methyl Orange Indicator

1. Transfer 100 mL of sample into a conical flask.

Sample Vol. of Sample Vol. of NaOH consumed (mL)

Department of Civil Engineering, TKMCE, Kollam Page 5

𝑉2 ×𝑁×𝐸𝑞.𝑤𝑡 𝑜𝑓 𝐶𝑎𝐶𝑂3 ×1000

Mineral acidity of the sample = mg/L

Department of Civil Engineering, TKMCE, Kollam Page 6

Burette, pipette, measuring cylinders, conical flasks

Alkalinity of water is its acid-neutralizing capacity. Alkalinity of many surface waters is

Figure : pH range of alkalinity

Department of Civil Engineering, TKMCE, Kollam Page 7

Sample Vol. of Sample Vol. ofSulphuric acid consumed (mL)

Department of Civil Engineering, TKMCE, Kollam Page 8

To determine the chloride content of the given water sample

Burette, pipette, measuring cylinders, conical flasks

Std. Silver Nitrate Soln. (0.014 N), Potassium chromate indicator

Ag+ + Cl- → AgCl (s)

1. Transfer 100 mL of sample into a conical flask.

Chlorides in the sample =

Department of Civil Engineering, TKMCE, Kollam Page 9

To determine the amount of sulphates in the given water sample

Barium chloride solution, hydrochloric acid (2N)

K2SO4 +BaCl2 → BaSO4 +2KCl

Department of Civil Engineering, TKMCE, Kollam Page 10

Mass of filter paper (g) =a

Department of Civil Engineering, TKMCE, Kollam Page 11

To determine the concentration of nitrates in the given water sample

Ion meter, Beakers

Preparation of calibration curve:

Department of Civil Engineering, TKMCE, Kollam Page 12

Sample No. Concentration (mg/L) Electrode potential

Electrode potential of the sample = mV

Nitrate concentration in the given sample = mg/L

Department of Civil Engineering, TKMCE, Kollam Page 13

To determine the concentration of phosphates in the given water sample

Pipette, flask, measuring cylinder, spectrophotometer

Phosphate is primarily used in biological system as an energy conduit. In water, phosphate is