DEPARTMENT OF CIVIL

ENGINEERING

CE8512
WATER AND WASTEWATER ANALYSIS LABORATORY

(REGULATION- 2017)

LABORATORY MANUAL

Name

Roll Number

Year&Semester
COURSE OBJECTIVE:

• To analyse the physical, chemical and biological characteristics of water and wastewater
• To quantify the dosage requirement for coagulation process
• To study the growth of micro-organism and its quantification
• To quantify the sludge

COURSE OUTCOME:

On the completion of the course, the students will be able to:

• Quantify the pollutant concentration in water and wastewater

• Suggest the type of treatment required and amount of dosage required for the treatment
• Examine the conditions for the growth of micro-organisms

SYLLABUS

WATER AND WASTE WATER ANALYSIS L T P C

CE8512
LABORATORY 0 0 4 2

LIST OF EXPERIMENTS:
1. Determination of pH, Turbidity and conductivity
2. Determination of Hardness
3. Determination of Alkalinity and Acidity
4. Determination of Chlorides
5. Determination of Phosphates and Sulphates
6. Determination of iron and fluoride
7. Determination of Optimum Coagulant dosage
8. Determination of residual chlorine and available chlorine in bleaching powder
9. Determination of Oil, and Grease
10. Determination of suspended, settleable, volatile and fixed solids
11. Determination Dissolved Oxygen and BOD for the given sample
12. Determination of COD for given sample
13. Determination of SVI of Biological sludge and microscopic examination
14. Determination of MPN index of given water sample

TOTAL: 60 PERIODS

2
Volumetric Analyses

By common usage, accurately calibrated glassware for precise measurements of volume

has become known as volumetric glassware. This group includes volumetric flasks,
volumetric pipettes, and accurately calibrated burettes. Less accurate types of glassware
including graduated cylinders and serological and measuring pipettes also have specific
uses in the analytical laboratory when exact volume is unnecessary.

3
Standards for Water and Wastewater
The term standard can be defined as certain rules, principles or measurements
established by the local or National/ International Authorities or legal agency and that
is applicable/compelled to implement and remain binding officially to almost all the
establishment of minimum standards of quality for public water supply is of
fundamental importance in achieving the certain ideas like water should be free from
pathogenic and harmful organisms, clear, palatable, free from undesirable taste and
odour, neither corrosive nor scale forming and free from minerals which could produce
undesirable physiological effects.
There are certain primary standards which are related to human health and
certain secondary standards which are related to protect human welfare. For water
quality monitoring study, three standards are of interest:
(a) Drinking water standards
(b) Industrial Effluent standards
(c) Sewage standards

Drinking Water Standards

SR. Drinking Water (IS: 10500 – 1991)

Parameters Units
NO. Desirable Maximum
1. Colour Hazen 5 25
units
2. Odour - Unobjectionable -
3. Taste - Agreeable -
4. Turbidity NTU 5 10
5. pH value - 6.5 to 8.5 No
relaxation
6. Total Hardness (as mg/L 300 600
CaCO3)
7. Iron mg/L 0.3 1.0
8. Chlorides mg/L 250 1000
9. Residual free Chlorine mg/L 0.2 -
10. Dissolved Solids mg/L 500 2000
11. Calcium mg/L 75 200
12. Copper mg/L 0.05 1.5
13. Manganese mg/L 0.1 0.3
14. Sulphate mg/L 200 400
15. Nitrate mg/L 50 No
relaxation
16. Fluoride mg/L 1.0 1.5

4
SR.NO. Drinking Water (IS: 10500 –
Parameters Units 1991)
Desirable Maximum
17. Phenolic compounds mg/L 0.001 0.002
18. Mercury mg/L 0.001 No
relaxation
19. Cadmium mg/L 0.01 No
relaxation
20. Selenium mg/L 0.01 No
relaxation
21. Arsenic mg/L 0.05 No
relaxation
22. Cyanide mg/L 0.05 No
relaxation
23. Lead mg/L 0.05 No
relaxation
24. Zinc mg/L 5 15
25. Anionic detergents mg/L 0.2 1.0
26. Chromium mg/L 0.05 No
relaxation
Polynuclear aromatic
27. mg/L - -
Hydrocarbons
28. Mineral oil mg/L 0.01 0.03
29. Pesticides mg/L Absent 0.001
Radioactive
materials Bq/L - 0.1
30.
(a) Alpha emitters Pci/L - 0.037
(b) Beta emitters
31. Alkalinity mg/L 200 600
32. Aluminium mg/L 0.03 0.2
33. Boron mg/L 1 5
Industrial Effluent Standards

SR. CPCB Permissible

Parameters Units
NO Limit
1. pH - 6.5 to 8.5
2. Temperature °C 40
3. Color (pt. co. Scale) Unit 100
4. Total Suspended Solids mg/L 100
5. Oil & Grease mg/L 10
6. Phenolic Compound mg/L 1.0
7. Cyanides mg/L 0.2
8. Fluorides mg/L 1.5
9 Sulphides mg/L 0.5
10. Ammonical Nitrogen mg/L 50

5
SR. CPCB Permissible
Parameters Units
NO Limit
11. Arsenic mg/L 0.2
12. Total Chromium mg/L 2.0
13. Haxavalent Chromium mg/L 0.1
14. Copper mg/L 2.0
15. Lead mg/L 0.1
16. Mercury mg/L 0.01
17. Nickel mg/L 3.0
18. Zinc mg/L 5.0
19. Cadmium mg/L 2.0
20. BOD (3 Days at 27 °C) mg/L 30
21. COD mg/L 100
22. Chlorides mg/L 600
23. Sulphates mg/L 1000
24. Total Dissolved Solids mg/L 2100
25. Insecticides/Pesticides - Absent
26. Sodium Absorption Ratio - 26
27. Selenium mg/L 0.05
28. Boron mg/L 2.0
29. Total Residual Chlorine mg/L 1.0
30. Percent Sodium % 60
90% Survival of
31 Bio Assay Test - fish
after 96 hours in
100% effluent
Sewage Standard

SR. CPCB Permissible Limit

Parameters Units
NO.
1 pH - 6.5 to 9.0
.
2. Total Suspended Solids mg/L Not More than 20
3. BOD mg/L Not More than 10
4. COD mg/L Not More than 50
5. NH4-N mg/L Not More than 5
6. N-Total mg/L Not More than 10
7. Total Coliform (MPN/100 Less than 100
ml)

6
 A LIST OF BASIC SAFETY RULES

1. When you handle chemicals wear eye protection (chemical splash goggles or full face
shield).
2. When you work with furnaces for heat treatment procedures or other thermally
activated equipment you should use special gloves to protect your hands.
3. Students should wear durable clothing that covers the arms, legs, torso and feet. (Note:
sandals, shorts, tank tops etc. have no place in the lab. Students inappropriately
dressed for lab, at the instructors discretion, be denied access)
4. To protect clothing from chemical damage or other dirt, wear a lab apron or lab coat.
Long hair should be tied back to keep it from coming into contact with lab chemicals or
flames.
5. In case of injury (cut, burn, fire etc.) notify the instructor immediately.
6. In case of a fire or imminently dangerous situation, notify everyone who may be
affected immediately; be sure the lab instructor is also notified.
7. If chemicals splash into someone's eyes act quickly and get them into the eye wash
station, do not wait for the instructor.
8. In case of a serious cut, stop blood flow using direct pressure using a clean towel,
notify the lab instructor immediately.
9. Eating, drinking and smoking are prohibited in the laboratory at all times.
10. Never work in the laboratory without proper supervision by an instructor.
11. Never carry out unauthorized experiments. Come to the laboratory prepared. If you are
unsure about what to do, please ask the instructor.
12. Always remember that HOT metal or ceramic pieces look exactly the same as COLD
pieces are careful what you touch.
13. Know the location and operation of :
➢ Fire Alarm Boxes
➢ Exit Doors
➢ Telephones

7
 LABARATORY CLASSES - INSTRUCTIONS TO STUDENTS

1. Students must attend the lab classes with ID cards and in the prescribed uniform.
2. Boys-shirts tucked in and wearing closed leather shoes. Girl’s students with cut shoes,
overcoat, and plait incite the coat. Girl’s students should not wear loose garments.
3. Students must check if the components, instruments and machinery are in working
condition before setting up the experiment.
4. Power supply to the experimental set up/ equipment/ machine must be switched on
only after the faculty checks and gives approval for doing the experiment. Students
must start to the experiment. Students must start doing the experiments only after
getting permissions from the faculty.
5. Any damage to any of the equipment/instrument/machine caused due to carelessness,
the cost will be fully recovered from the individual (or) group of students.
6. Students may contact the lab in charge immediately for any unexpected incidents and
emergency.
7. The apparatus used for the experiments must be cleaned and returned to the
technicians, safely without any damage.
8. Make sure, while leaving the lab after the stipulated time, that all the power
connections are switched off.
9. EVALUATIONS:
➢ All students should go through the lab manual for the experiment to be carried
out for that day and come fully prepared to complete the experiment within the
prescribed periods. Student should complete the lab record work within the
prescribed periods.
➢ Students must be fully aware of the core competencies to be gained by doing
experiment/exercise/programs.
➢ Students should complete the lab record work within the prescribed periods.
➢ The following aspects will be assessed during every exercise, in every lab class
and marks will be awarded accordingly:
➢ Preparedness, conducting experiment, observation, calculation, results, record
presentation, basic understanding and answering for viva questions.

8
 LIST OF EXPERIMENTS
PAGE
SL.NO. NAME OF THE EXPERIMENT
NO.
1. Determination of pH 13

2. Determination of Turbidity 16

3. Determination of Electrical Conductivity 19

4. Determination of Total Hardness 22

5. Determination of Acidity 25

6. Determination of Alkalinity 28

7. Determination of Chlorides 31

8. Determination of Phosphate 34

9. Determination of Sulphate 37

10. Determination of Iron 40

11. Determination of Fluorides 43

12. Determination of Optimum Coagulant Dosage 46

Determination of Residual Chlorine and Available
13. 49
Chlorine in Bleaching Powder
14. Determination of Oil and Grease 52
Determination of Total Suspended, Volatile, Fixed and
15. 55
Settleable solids
16. Determination of Dissolved Oxygen 59
Determination of Bio-Chemical Oxygen Demand (B.O.D
17. 62
test) for the given sample
Determination of Chemical Oxygen Demand (C.O.D test)
18. 68
for the given sample
19. Determination of MPN index for the given sample 71
Determination of SVI of Biological sludge and
20. 74
Microscopic examination

9
 INDEX

STAFF
EX.NO. DATE NAME OF THE EXPERIMENT MARKS
SIGNATURE

10

11

12

13

10
 STAFF
EX.NO. DATE NAME OF THE EXPERIMENT MARKS
SIGNATURE

14

15

16

17

18

19

20

11
TABULATION:

S.No Description of sample Temperature pH

12
 Ex.No.:
DETERMINATION OF pH
Date:

AIM:

To determine the pH of the given water / waste water sample.

APPARATUS & REAGENTS REQUIRED:

1. pH meter along with electrodes.

2. Buffer tablet of pH values 4 and 9.2
3. Thermometer.

PROCEDURE:

1. Calibrate the electrodes with two standard buffer solutions of pH 4.0 and 9.2
2. The sample temperature is determined at the same time and is entered into the
meter to allow for a temperature correction.
3. Rinse the electrode thoroughly with de-ionized distilled water and carefully wipe
with a tissue paper.
4. Dip the electrodes into the sample solution, swirl the solution and wait upto one
minute for steady reading. A pH meter reading within ± 0.1 pH unit will be adequate
for such work.
5. The reading is taken after the indicated value remains constant for about a minute.

ENVIRONMENTAL SIGNIFICANCE
pH (6.5 to 8.5) has no direct effect on health however a lower value below 4
will produce sour taste and higher value above 8.5 a bitter taste. Higher values of p1-I
have scale formation in water heating operators and also reduce the germicidal
potential of chlorine. High pH induces the formation of trihalomethanes which are
causing cancer in human beings.

pH below 6.5 starts corrosion in pipes, thereby releasing toxic metals such as
zinc, lead, cadmium & copper etc., According to BIS water for domestic consumption
should have pH between 6.5 to 8.5

Application of pH data in Environmental Engineering Practice

1. Determination of pH is one of the important objective in biological treatment, if the
pH goes below 5 due to excess accumulation of acids, the process is severely affected.
Shifting of pH beyond 5 to 10 upsets the aerobic treatment of the waste waters. In
these circumstances, the pH can be adjusted by addition of suitable acid or alkali to

13
 optimize the treatment of waste water.

2. Its range is of immense value for any chemical reaction. A chemical value shall be
highly effective at particular pH. Chemical coagulation; disinfection, water softening
and corrosion control are governed by pH adjustment.

3. Dewatering of sludges, oxidation of cyanides and reduction of hexa covalent

chromium in to trivalent chromium also need a favorable range 4. It is used in the
calculation of carbonate, bicarbonate, C02 calculation, stability index and acid- base
equilibrium.

RESULT:

The pH value of the given

1. Sample 1 = ______________________

2. Sample 2 = ______________________

3. Sample 3 = ______________________

14
TABULATION:

S.No Source of Sample Temperature of Sample (°C) Turbidity NTU

15
Ex.No.:

Date:
DETERMINATION OF TURBIDITY

AIM:

To determine the turbidity of given waste water/water sample using Nephelo

turbidity meter.

APPARATUS REQUIRED:

1. Nephelometric turbidimeter
2. Sample tubes

PROCEDURE:

1. Switch on the instrument and let the instrument warm for 15-20 minutes.
2. Insert the cell with distilled water into the cell holder. Cover the cell with light
shield.
3. Set the instrument at 100 on the scale with a 40 NTU standard suspension. In
this case, every division on the scale will be equal to 0.4 NTU turbidity.
4. The sample is thoroughly shaked and kept it for sometimes so the air bubbles
are eliminated
5. Take sample in Nephelometer sample tube and put the sample in sample
chamber and find out the value on the scale.
6. Dilute the sample with turbidity free water and again read the turbidity.

ENVIRONMENTAL SIGNIFICANCE
Turbidity is objectionable because of
a. Aesthetic considerations and
b. Engineering considerations
When turbid water in a small, transport container. such as drinking glass is help
up to the light, an aesthetically displeasing opaqueness or milky coloration is apparent.
The colloidal material which exerts turbidity provides adsorption sites for chemicals
that may be harmful or cause undesirable tastes and odours & for biological
organism that may be harmful. Disinfections of turbid water is difficult because of the
adsorptive characteristics of some colloids and because the solids may partially
shield organisms from disinfectant.
In natural water bodies, turbidity may impart a brown or other colour to water and
may interfere with light penetration and photosynthetic reaction in streams and lakes.
Turbidity increases the load on slow sand filters. The filter may go out of operation, if
excess turbidity exists.

16
Application of Turbidity Data in Environmental Engineering Practice:

Turbidity measurements of particular importance in the field of water supply. They

have limited use in the field of domestic and Industrial waste treatment.
1. Knowledge of the turbidity variation in raw water supplies along with other
information is useful to determine whether a supply repairs Special treatment by
chemical coagulation and filtration before it may be used for a public water supply.
2. Turbidity measurements are used to determine the effectivness of the treatment
produced with different chemicals and the dosages needed.
3. Turbidity measurements help to gauge the amount of chemicals needed from day-
today in the operation of water treatment works.
4. Measurement of turbidity is settled water prior to filtration is useful in controlling
chemical dosages so as to parent excessive loading or rapid sand filters.
5. Turbidity measurements of the filtered water are needed to check filter operation.
6. Turbidity measurements are useful to determine the optimum dosage of
coagulants to treat the domestic and Industrial wastes.
7. Turbidity determination is used to evaluate the performance of waste treatment
plants.

RESULT:

The Turbidity of given sample

1. Sample 1 = ______________________

2. Sample 2 = ______________________

3. Sample 3 = ______________________

17
TABULATION:

Conductivity
S.No Description of the sample Temperature
(mmhos/cm)

18
Ex.No.:

Date:
DETERMINATION OF ELECTRICAL CONDUCTIVITY

AIM:

To determine the electrical conductivity of given sample using conductivity meter.

APPARATUS REQUIRED:

1. Conductivity meter with measuring cell.

2. Beaker
3. Thermometer

REAGENT:

1. KCl 0.1N

PROCEDURE:

1. Calibrate the cell with standard 0.1N KCl solution of conductivity 14.12 mhos at
30°C.
2. Rinse the cell thoroughly with deionized distilled water and carefully wipe with a
tissue paper.
3. Dip the cell into the sample solution, swirl the solution and wait upto 1 minute for a
steady reading.
4. Note down the instrument reading and also temperature by a thermometer.

ENVIRONMENTAL SIGNIFICANCE
1. Electrical conductivity measurements are often employed to monitor desalination
plants.
2. It is useful to assess the source of pollution.
3. In coastal regions, conductivity data can be used to decide the extent of intrusion of
sea water into ground water.
4. Conductivity data is useful in determining the suitability of water and wastewater
for disposal on land. Irrigation waters up to 2 milli Siemens / cm conductance have
been found to be suitable for irrigation depending on soils and climatic
characteristics.

INFERENCE

The conductivity value gives us a rapid and inexpensive way of determining the
ionic strength of a solution. This is an easy measurement to make and relates closely to the
total dissolved solids content of water. The total dissolved solids are about seventy percent
of the conductivity. In the ground water, the ionisable salts are lesser and thereby the

19
conductivity is also lesser in nature. Water having more number of ionisable salts for
example sea water, is having high conductivity. The fresh water bodies only have a
minimum amount of salts and have moderate conductivity.

RESULT:

Conductivity value of given sample is

1. Sample 1 = ______________________

2. Sample 2 = ______________________

3. Sample 3 = ______________________

20
 TABULATION:

Burette solution : Std. EDTA Solution

Pipette solution : Given sample
Indicator : Erio-Chrome Black T
End point : Wine red to Steel Blue.

Volume of sample Burette reading ml Concordant value Volume of EDTA in

taken in ml Initial Final ml ml

CALCULATION:

Amount of hardness present in the given sample = (Volume of EDTA X 1000) / Volume of
sample.

21
Ex.No.:

Date:
DETERMINATION OF TOTAL HARDNESS

AIM:

To determine the Total hardness of the given sample.

APPARATUS REQUIRED:

1. Burette.
2. Pipette.
3. Conical Flask.
4. Standard Flask.
5. Beaker.

REAGENT:

1. Ammonia buffer solution

2. Eriochrome Black T indicator
3. Standard EDTA Solution 0.02N

PROCEDURE:

1. Take 20 ml of sample in conical flask.

2. Add 2 ml of ammonia buffer solution.
3. Add Eriochome Black T indicator followed by buffer solution and the solution
become wine red in colour.
4. Titrate the above solution against EDTA solution taken in the burette. The end
point is the appearance of blue in colour.

ENVIRONMENTAL SIGNIFICANCE:
Hard water has adverse action with soap since it allows less formation of leather. If hard
water is used in boilers, scaling problem occurs leading to the bursting of boilers, It makes food
tasteless. It affects the working of dyeing process. It is also precipitate protein of meat and
make tasteless.

Application of Hardness data in Environmental Engineering Practice

1. Hardness of water is important in determining the suitability of water for domestic and
industrial uses.
2. The relative amounts of calcium and magnesium hardness, carbonate and non- carbonate
hardness present in water are the factors while determining the most economical type of
softening process.
3. Determination of hardness serve as a basis for routine control of softening process.

22
RESULT:

Amount of total hardness present in given sample is ________________________mg/l.

23
TABULATION:

Phenolphthalein
Methyl orange indicator
indicator (burette
Sample Volume of the (burette reading, ml)
reading, ml)
details sample (ml)
NaOH NaOH
Initial Final Initial Final
used used

CALCULATION:

Mineral acidity due to mineral acids (as CaCO3, mg/L) = V1 x 1000

ml of sample taken

CO2 acidity due to CO2 (as CaCO3, mg/L) = V1 x 1000

ml of sample taken

Mineral acidity (mg/L) = CO2 acidity (mg/L) =

Total acidity as (CaCO3) = Mineral acidity + CO2 acidity

24
Ex.No.:

Date:
DETERMINATION OF ACIDITY

AIM:

To determine the Acidity of the given samples.

APPARATUS REQUIRED:

1. Conical flask.
2. Burette.
3. Pipette.
4. Measuring cylinder.

REAGENT:

1. Phenolphthaline Indicator.
2. Standard Sodium hydroxide (0.02N).
3. Methyl Orange Indicator
4. Sodium Thiosulphate (0.1N)
5. Carbon dioxide free distilled water

PROCEDURE:

1. The sample of 100 ml is pipette into the conical flask.

2. Add 1 drop of 0.1N sodium thiosulphate solution to remove the residual
chlorine if present.
3. Add 2 drops of Methyl orange and the sample turns pink
4. Proceed with titration with Std. Sodium Hydroxide solution until the colour
changes to yellow.
5. Note down the volume of NAOH added (V1)
6. Take another conical flask containing 100 ml of water sample, add 2 or 3 drops
of phenolphthalein.
7. Proceed with titration until the sample turns pink.
8. Note down the total volume of NaOH added (V2)

Environmental Significance:

1. Acidity interferes in the treatment of water (as in softening)

2. It corrodes pipes (zinc coating of G.I pipes got dissolved)
3. Aquatic life will be affected.
4. Waters contain mineral acidity are so unpalatable

25
5. Water having acidity more than 50 mg/L cannot be used in R.C.C works.

Application of acidity data in Environmental Engineering practice:

1. The amount of CO2 is an important factor in determining whether removal by aeration

or simple neutralization with lime or sodium hydroxide will be chosen as the
treatment method.
2. The size of equipment, chemical requirement, storage space and cost of treatment all
depend upon amount CO2 present.
3. Most industrial wastes containing mineral acidity must be neutralized before they are
subjected to biological treatment or direct discharge into water courses or sewers.

RESULT:

The total acidity of the given sample is ________________

26
TABULATION:

Phenolphthalein Methyl orange indicator

Sample Volume of the (burette reading, ml) (burette reading, ml)
details sample (ml) H2SO4 H2SO4
Initial Final Initial Final
used used

CALCULATIONS:

1. Phenolphthalein alkalinity (P) mg/L as CaCO3 =

V1 x Normality of H2SO4 x 1000 x 50
Volume of Sample taken
2. Total Alkalinity (T) mg/L as CaCO3 =
V2 x Normality of H2SO4 x 1000 x 50
Volume of Sample taken

27
Ex.No.:

Date:
DETERMINATION OF ALKALINITY

AIM:

To determine the Alkalinity of the given samples.

APPARATUS REQUIRED:

1. Conical flask.
2. Burette.
3. Pipette.
4. Measuring cylinder.

REAGENT:

1. Phenolphthaline Indicator.
2. Standard Sodium hydroxide (0.02N).
3. Methyl Orange Indicator
4. Sodium Thiosulphate (0.1N)
5. Carbon dioxide free distilled water

PROCEDURE:

1. The water sample of 100 ml is pipette into the conical flask.

2. Add 1 drop of 0.1N sodium thiosulphate solution to remove the residual chlorine if
present.
3. Add 2 drops of Methyl orange and the sample turns pink.
4. Run down 0.02N standard sulphuric acid till the solution turns to colour less.
5. Note down the volume of sulphuric acid added (V1).
6. Add 2 drops of methyl orange indicator the sample turns yellow.
7. Resume titration till the colour of the solution turns to pink.
8. Note down the total volume of sulphuric acid added (V2).
Environmental Significance:

1. Highly alkaline waters are usually unpalatable and consumers tend to seek other
supplies.
2. Chemically treated waters sometimes have rather high pH values which have met
with some objection on the part of consumers.
3. Large amount of alkalinity imparts a bitter taste to water.

28
Application of Alkalinity data in Environmental Engineering practice:

1. Chemical coagulation of water and wastewater: To neutralise acids produced

during flocculation, the sample should be alkaline otherwise further floc formation
slowly ceases (stops).
2. Water Softening: To find out the quantity of lime and soda-ash required for the
removal of hardness
3. Corrosion control
4. Effluents of wastewater: Wastewater containing excess alkalinity is not to be
discharged into natural water bodies or sewers.
Excess alkalinity in water is harmful for irrigation which leads to soil damage and
reduce crop yields. The desirable limit for consumption is 250 mg/L.

RESULT:

The Alkalinity of the given sample

1. Hydroxide alkalinity = ______________________

2. Carbonate alkalinity = ______________________

3. Bicarbonate alkalinity = ______________________

29
 TABULATION 1:
Burette solution : Silver Nitrate.
Pipette solution : Given sample.
Indicator : Potassium chromate.
End point : Yellow to brick red.
Titration 1( For Sample)

Volume of sample Burette reading ml Concordant value Volume of Ag NO3

taken in ml Initial Final ml in ml

TABULATION 2:
Burette solution : Silver Nitrate.
Pipette solution : Distilled water
Indicator : Potassium chromate.
End point : Yellow to brick red.
Titration 2( For Blank)

Volume of sample Burette reading ml Concordant value Volume of Ag NO3

taken in ml Initial Final ml in ml

CALCULATION:

Chloride in (mg/L) = (A - B) x Normality of AgNO3 x 35.46 x 1000

Volume of the sample taken

30
Ex.No.:

Date:
DETERMINATION OF CHLORIDES

AIM:

To determine the amount of chlorides present in the given sample.

APPARATUS REQUIRED:

1. Burette.
2. Pipette.
3. Conical Flask.
4. Beaker.

REAGENT:

1. Chloride free distilled water.

2. Standard Silver Nitrate (0.0141 N)
3. Potassium Chromate indicator
4. Standard Sodium Chloride (0.0141 N)

PROCEDURE:

1. Take 20 ml of sample in conical flask.

2. Add 1 ml of Potassium Chromate to get light yellow colour.
3. Titrate the sample against silver nitrate solution until the colour changes from
yellow to brick red.
4. Note the silver nitrate added (A).
5. For better accuracy, titrate distilled water in the same manner.
6. Note the volume of silver nitrate added for distilled water (B).

Environmental Significance of Chlorides

Chloride associated with sodium exerts salty taste, when its concentration is
more than 250 mg/1 .There is no known evidence that chloride- constitute any human
health hazard. For this reason, chlorides are generally limited to 250 mg/L in supplies
intended for public use. In many areas of world where water supplies are scarce, sources
containing as much as 2000mg/L are used for domestic purposes without the development
of adverse effect once the human system becomes adapted to the water.
It can also corrode concrete by extracting calcium in the form of calcide. Magnesium
chlorides in water generate hydrochloric acid after heating which is also highly corrosive in
nature and create problems in boilers.

31
Application of chlorides data in environmental engineering practice

1. Chlorides determination in natural waters is useful in the selection of water supplies for
human use.

2. Chlorides determination is used to determine the type of desalting operators to be used.

3. The chloride determination is used to control pumping of ground water from locations
where intrusion of sea water is a problem.

4. Chlorides interfere in the determination of COD a correction must be made on the basis
of the amount of chloride present.

RESULT:

Amount of Chlorides present in given sample is ________________________mg/l.

32
PREPARATION OF STANDARD CURVE

Standard
Ammonium Stannous Concentration
PO4 Distilled Display
Molybdate Chloride of new
solution water (ml) readings
(ml) (drops) solution (mg)
(ml)
0 25 1 2 0

5 20 1 2 0.05

10 15 1 2 0.10

15 10 1 2 0.15

20 5 1 2 0.20

25 0 1 2 0.25

CALCULATION:

Sample 1 =
Sample 2 =
Phosphate (mg/l) = (mg of PO4 x 1000) / ml of sample

Model graph:

Display Readings

Concentration of Phosphate (mg)

33
Ex.No.:

Date:
DETERMINATION OF PHOSPHATE

AIM:

To determine the phosphates in the given water sample by spectrophotometer.

APPARATUS

1. Spectrophotometer
2. Nessler tubes – 100 ml capacity

REAGENTS:

1. Standard Phosphate solution

2. Ammonium Molybdate solution
3. Strong acid reagent
4. Sodium Hydroxide (3N)
5. Phenolphthalein indicator
6. Stannous chloride

PROCEDURE:

1. Switch on the spectrophotometer and allow 20 minutes for warm up and set
410 nm by adjusting the wavelength knob.
2. For calibration of the instrument take distilled water in the cuvette holder and
place in the compartment on the light path and close the compartment.
3. Press the mode button to set transmittance mode and set 100 % T.
4. Again press the mode button to set it for absorbance to read 0.00.
5. Fill the prepared standard solutions in the cuvette holders and place in the
compartment.
6. Read the colour developed on the display and note down the peak value.
7. Take 25 ml of filtered and clear sample.
8. Add 1 ml of ammonium molybdate solution and 2 drops of stannous chloride
9. Measure the blue colour developed at 690 nm on a spectrophotometer using a
distilled water blank with the same chemicals.
10. Note down the readings of spectrophotometer after 5 minutes but before 12
minutes of the addition of the last reagent.
11. Find out the concentration of the phosphate with the help of the standard curve.

34
Environmental Significance of Chlorides

Small quantity of phosphorous in surface waters is necessary for biological life, but
excess of phosphorous promotes the abundant growth of nuisance algae
(eutrophication). Phosphorous can also interfere with water treatment processes,
concentration as low 0.2 mg/L interfere with chemical coagulation of turbid water. They
are used in small concentration to avoid corrosion in water mains, to remove iron and
manganese in micro quantities.

Application of Phosphorous data in Environmental Engineering practice:

1. It is used principally to control phosphorous in water systems for corrosion

prevention and n boilers for control of scale.
2. Phosphorous determinations are routine in the operation of wastewater treatment
plants and in stream pollution studies in many areas.
3. It is useful to assess fertility value of sludge.

RESULT

The amount of phosphates determined from the given sample is ________ mg/l.

35
TABULATION:

S. No. Standard solution Absorbance (nm) Sulphate concentration

(mg/l)
1 0
2 2
3 4
4 6
5 8
6 Waste water

CALCULATION:

Sulphate concentration :

1. For 2 ml

 0.3698 
   1000  2
 250   1000 = 59.17  60mg / l
50

2. For 4 ml

 0.3698 
   1000  4
 250   1000 = 118.33  120mg / l
50

3. For 6 ml

 0.3698 
   1000  6
 250   1000 = 177.50  180mg / l
50

36
Ex.No.:

Date:
DETERMINATION OF SULPHATE

AIM:

To determine the concentration of sulphate in the given water sample.

APPARATUS REQUIRED:

1. Spectrophotometer.
2. Measuring cylinder.
3. 50 ml glass beaker.

REAGENT:

1. Sodium sulphate
2. Barium Chloride
3. Sodium chloride – HCL reagents

PROCEDURE:

1. 5 number of 50 ml beaker are taken with sulphate solution of 2 ml, 5 ml, 6 ml,
8 ml & 10 ml.
2. Sodium chloride and Barium chloride are added with it of 10 ml in sample
beaker & blank.
3. It is make upto 50 ml by distilled water.
4. The spectrophotometer is calibrated of 420 nm.
5. The curve is plotted with those values.
6. 20 ml of sample is taken, 10 ml of barium chloride, 10 ml of sodium chloride
are added with the sample.
7. It is makeing up to 50 ml by distilled water.
8. The reading is noted & tabulated.The curve is plotted with the reading.

Environmental Significance of Sulphates:

Sulphates in natural waters in concentrations ranging from a few to thousand
mg/L.Excess Na2SO4 and MgSO4 should not be present in drinking waters as they cause
Cathartic action. Higher Concentration of Sodium Sulphate in water can cause malfunctioning
of the alimentary canal. So the recommended upper limit is 250m/l in water intended for
human consumption. In anaerobic decomposition of waste waters, Suiphates are reduced to
hydrogen Sulphide causing obnoxious odours and promote corrosion of sewers.Sulphates are
reduced to sulphide in sludge digesters and may upset the biological process, if the sulphide
concentration exceeds 200mg/L.

37
Application of Sulphate Data in Environmental Engineering Practice:
1. The sulphate content of natural waters is an important consideration in determining their
suitability for public and industrial water supplies.
2. The amount of sulphate in waste water is a factor of concern in determining the magnitude of
problems that can arise from reduction of sulphates to hydrogen sulphide.
3. A knowledge of the sulphate content of the sludge or waste fed to digestion units provides a
means of estimating the hydrogen sulphide content of the gas produced. From this information,
the design engineer can determine whether scrubbing facilities will be needed to remove
hydrogen sulphides and size of the units required.

RESULT:

The sulphate concentration in the given sample is ____ ____mg/l.

38
 TABULATION:

S. No. Standard solution Absorbance (nm) Iron concentration

(mg/l)
1 0
2 2
3 4
4 6
5 8
6 Waste water

CALCULATION :

1. Soluble Iron (Direct Determination without the Digestion Step)

mg of Fe/l = mg of Fe (in 100 ml of the final solution) / V

where v = Volume in ml of the sample used.

2.Total Iron (When the Digestion is Carried Out)

mg of Fe/l = [mg of Fe (in 100 ml of the final solution) x 100] / V1 x V2

where V1 = volume in ml of the sample used, and

V2 total volume in ml of digested solution used for Fe determination.

39
Ex.No.:

Date:
DETERMINATION OF IRON

AIM:

To determine the concentration of iron in the given water sample.

APPARATUS REQUIRED:

1. Spectrophotometer.
2. Measuring cylinder.
3. 50 ml glass beaker.

REAGENT:

1. Hydrochloric Acid
2. Hydroxylamine Solution
3. Ammonium Acetate Buffer Solution
4. Sodium Acetate Solution
5. 1.10 Phenanthroline Solution
6. Stock Iron Solution
7. Standard Iron Solutions
8. Di-isopropyl Ether

PROCEDURE:

1. Pipette out appropriate portions of standard iron solution into 125 ml

conical flasks to contain from 10 to 100 µg of Fe.
2. For the reagent blank, pipette out 10 ml of water to a separate conical flask.
Dilute the contents of each conical flask to about 50 ml by adding water.
3. To each flask, add 1 ml NH2 OH.HCI solution and 2 ml conc HCl. Add a few
boiling chips and boil the solution until the volume is reduced to about 20 ml.
4. Cool to room temperature and quantitatively transfer to 100 ml volumetric
flasks.
5. Add 10 ml ammonium acetate buffer solution first and add 10 ml, 1,10
phenanthroline solution to each flask.
6. Dilute to 100 ml with water and mix thoroughly and allow to stand for 10 to
15 min. Measure the absorbance of the iron complexes at 510 nm against the
reagent blank.
7. Construct a calibration curve by plotting absorbance values against
micrograms of iron in 100 ml of the final solution.

40
Environmental Significance of Iron:

1. Excess presence of iron in drinking water supplies is objectionable for a number

of reasons
2. Long time consumption of drinking water with a high concentration of iron lead
to liver diseases.
3. Iron rich water exposed to the air, becomes turbid and highly unacceptable from
the aesthetic view point.
4. Iron in excess of 0.3 mg/L causes stains to wash basin and steel containers. they
also form red spot on clothes.
5. Iron also promotes the growth of iron-bacteria which gives a rusty appearance
to waters.

Application of Iron data in Environmental Engineering practice:

1. Iron content of water is important in determining the suitability of water for

domestic and industrial purpose.
2. Determination of iron is useful to select the treatment unit and design of treatment
units.
3. The ratio of iron to manganese is a characteristic factor that determines the type of
treatment unit used, as well as the amount of organic matter present in the water.

RESULT:

The iron concentration in the given sample is ____ ____mg/l.

41
TABULATION:

S. No. Standard solution Absorbance (nm) Fluoride

concentration
(mg/l)
1 0
2 2
3 4
4 6
5 8
6 Waste water

42
Ex.No.:

Date:
DETERMINATION OF FLUORIDES

AIM:

To determine the amount of fluorides present in tne given water sample.

REAGENT:

1. Fluoride stock solution

2. Fluoride standard solution
3. Acid zirconyl-SPANDS reagent
4. References solution
5. Sodium arsenite solution

PROCEDURE:

1. Pipette 0.0, 0.5, 1.0, 2.0, 3.0, 4.0, 5.0, 6.0, and 7.0 ml fluoride standard solution
in to 50 ml nessler tubes and make up to the mark with distilled water.
2. Add exactly 10.0 ml acid-zriconyl-SPADNS reagent to each tube and mix well.
3. Set the spectrophotometer or filter photometer to zero absorbance using
reference solution at 570 mµ and measure the absorbance of the standards
immediately.
4. Plot the calibration curve
5. Place 50.0 ml of the sample or an aliquot diluted to 50.0 ml in a nessler tube. If
the sample contains any residual chlorine adds 1 drop of sodium arsnite
solution for each 0.1 mg Cl2 and mix well. Add exactly 10.0 ml of the acid-
zirconyl-SPANDS reagent and mix well. After setting the spectrophotometer to
zero-absobance with the reference solution, measure the absorbance of the
sample. Find out the mg fluoride of the sample equivalent to the observed
optical density from the calibration graph.

Environmental Significance of Fluoride:

Presence of large amounts of fluoride is associated with dental and skeletal fluorosis
(> 1.5 mg/L) and inadequate amounts with dental caries (> 1 mg/L)

Dental Fluorosis
In young children the diseases affects only on the teeth. This is known as dental
fluorosis. The teeth lose their shiny appearance and chalk-white patches develop on them. This
is known as mottled enamel and is an early sign of dental fluorisis. The white patches later
become yellow and turn brown or black.

43
Skeletal Fluorosis
In aged people the disease affects the bones, tendons and ligaments. This is known as
skeletal fluorosis. This is followed by pain and stiff of the back and later the joints of both limbs
and limitation of neck movements.

Genu Valgum
It was observed that this syndrome was most prevalent among people whose staple diet
was sorghum. Further studies have shown that diets based upon jower promote a higher
retention of ingested fluoride than their based on rice.

Application of fluoride data in Environmental Engineering Practice:

1. Fluoride of water is an important in determining the suitability of water from domestic and
industrial uses.
2. The size and design of Deflouridation units depends upon the level of fluorides present in the
water.

RESULT:

Amount of fluorides present in the given sample = ____ ____mg/l.

44
OBSERVATION:

Initial Turbidity Alum dosage Final Turbidity

Trial No. Efficiency %
in NTU in ml in NTU
1

FORMULA:

Efficiency of the Ferric chloride dosage = Initial turbidity - Final turbidity X 100

Initial turbidity

CALCULATION:

GRAPH:

Draw graph between Alum dosage (X-axis) and Turbidity (Y axis)

45
 Ex.No.:
DETERMINATION OF OPTIMUM COAGULANT DOSAGE
Date:

AIM:

To determine the optimum dosage of Coagulant dosage required for treating turbid
water.

APPARATUS:

1. Jar test apparatus

2. Glass beakers
3. Pipette
4. Nephelometer
REAGENTS:

1. Alum solution (Dissolving 1 gm of aluminium sulphate in 1 lit of distilled

water)

PROCEDURE:

1. Measure the initial turbidity of whole sample.

2. Measure 500 ml quantities of above wastewater sample into each of 6 beakers in
series.
3. Keep each beaker below each paddle and lower the paddles, such that each one is
about 1cm above the bottom.
4. Pipette 0 ml, 1 ml, 2 ml, 3 ml, 4 ml, and 5 ml of the Alum solution into the test
samples.
5. Immediately run the paddles at 100 – 120 rpm for 1-2 minute.
6. Reduce the speed to 20 rpm and run at this rate for 15 minutes.
7. Stop the machine, lift out the paddles and allow settling for 15 minutes.
8. Carefully take a small amount (about 100 ml) of settled waste water from top of
each beaker without disturbing the settled sediments.
9. Find the residual turbidity of the supernatant using Nephelometer.
10. Plot a graph with Alum dosage along x-axis and turbidity along y-axis.
11. The dosage of alum, which represents least turbidity, gives Optimum Coagulant
Dosage (O.C.D.).
12. Repeat steps 1–10 with higher dose of alum, if necessary.
Environmental Significance:

Excess dosage of alum may contribute excess aluminium in drinking water.

According to recent investigation aluminium is neurotoxic. Coagulation removes not only

46
turbidity, but also colour, micro-organisms, algae, phosphate, tasye and odour producing
substances.

Environmental Engineering applications:

1. This test is useful to identify various natural coagulants.

2. It is useful to estimate optimum coagulant dosage of coagulant required for raw
waters and wastewaters.

RESULT:

The Optimum coagulant dosage for the given sample = ____ ____.

47
TABULATION:

Volume of Burette reading

S.No Volume of Na2S2O3
sample taken Initial Final

CALCULATION:

Total available residual chlorine in the water sample =

Volume of Sodium thiosulphate ∗ N ∗ 35.45 ∗ 1000

𝑚𝑔 𝐶𝑙 𝑎𝑠 𝐶𝑙2/𝐿 =
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑡𝑎𝑘𝑒𝑛

48
 Ex.No.:
DETERMINATION OF RESIDUAL CHLORINE AND
Date: AVAILABLE CHLORINE IN BLEACHING POWDER
AIM:

To determine the amount of residual chlorine and available chlorine in

given sample.

APPARATUS:

1. Burette
2. Pipette
3. Measuring jar
4. Conical flask
PROCEDURE:

1. Concentrated Acetic Acid

2. Potassium Iodide crystals
3. Sodium thiosulphate (0.025N)
4. Starch indicator
PROCEDURE:

1. Take 5gm of fresh bleaching powder. Adding small quantity of water to it and
prepare fine paste. Add some more water, stir and allow to settle for a few
minutes. Dilute it with distilled water to make upto 1 litre and stopper the
container
2. Take 25 ml of the bleaching powder solution in a conical flask and add a pinch
of KI.
3. Add 5 ml Acetic acid and alow the reaction to complete.
4. Titrate the solution with standard Na2S2O3 solution untill the yellow colour of
liberated Iodine is almost faded out. (Pale Yellow color)
5. Add 1 ml of starch solution and titrate until the blue colour disappears.
6. Note down the quantity of solution thiosulphate added (V1).
7. Repeat the same procedure for distilled water.
8. Note down the volume of sodium thiosulphate added (V2)
Environmental Significance of Residual Chlorine:

Active chlorine (free and combined) should be determined at each stage in the
processing of drinking water and in the water mains in order to guarantee a
bacteriologically impeccable water. Active chlorine should be present in drinking water

49
within the range 0.1 to 0.2 mg/L. However, excessive chlorine content may give out bad
odour and may change even taste of waters. Further, chlorine is said to carcinogenous.

Application of Residual Chlorine data in Environmental Engineering practice:

1. Chlorine residuals determination is uded to control chlorination of domestic and

industrial wastewaters.
2. Determination of chlorine residual in water distribution is useful to find the source
of contamination or leakage points, so as to supply wholesome water to the
customer.

RESULT:

The amount of residual chlorine present in the given sample = ____ ____ mg/L

50
OBSERVATION
Temperature of measurement = ............................°C

Mass of evacuated flask = ..........................................g

Mass of evacuated flask + residue = .....................g

Mass of residue = ...........................................................mg

Volume of sample = ......................................................mL

CALCULATION

The amount of oil and grease in the sample can be calculated as,

Oil and Grease (mg/L) = (A - B) 1000/volume of the sample

where,

A = mass of evacuated flask and residue (g)

B = mass of evacuated flask (g)

51
Ex.No.:

Date:
DETERMINATION OF OIL AND GREASE

AIM:

To determine the quantity of oil and grease present in the given sample

APPARATUS REQUIRED:

1.Separatory funnel, 1L with TFE (Teflon) stopcock

2.Distilling flask, 125mL
3.Water bath
4. Filter paper, 110mm dia. (Whatman No. 40 or equivalent).
5.Weighing balance
6.Desiccators
7.Vacuum pump.
REAGENTS REQUIRED:

1. HCl
2. Trichlorotrifluosoethane (freon).

PROCEDURE

1. Collect about 1 litre of sample and mark sample level in bottle for latter determination
of sample volume. Add 5 ml of HCl to maintain pH level of 2. Transfer to a separating
funnel. Carefully rinse sample bottle with 30 ml trichlorotrifluoroethane and solvent
washing to separating funnel.
2. Shake vigorously for 2 minute.
3. Let layer separate out, drain solvent layer through a funnel containing solvent–
moistened filter paper into a clean, evacuated distilling flask. If a clear solvent layer
cannot be obtained, add 1g Na2SO4, if necessary.
4. Extract twice more with 30 ml solvent each time but first rinse sample container with
solvent. Combine extracts in evacuated distilling flask and mash filter paper with an
additional 10 ml to 20 ml solvent.
5. Distill solvent from distilling flask in a water bath at 70°C. Place flask on water bath at
70°C for 15 minute and draw air through it with an applied vacuum for final 1 minute
after the solvent has evaporated. If the residue contains visible water, add 2 ml
acetone evaporates on a water bath and repeat the addition and evaporation until all
visible water has been removed. Cool in a desiccators for 30 minute and weigh it.

52
Environmental Significance of Oil and Grease:
1. Oil and Grease in water can cause surface films and shoreline deposits leading to
environmental degradation and can induce human health risks when discharged in
surface or ground waters.
2. The presence of oil and grease in water bodies leads to the formation of oil layer,
which causes significant pollution problem such as reduction of light penetration
and photosynthesis. It further hinders oxygen transfer from atmosphere to water
medium and this leads to decreased amount of dissolved oxygen (DO) at the bottom
of the water and this adversely affects survival of aquatic life.
3. The effects of oil and grease in wastewater steam to include physical blockages in
sewers, pump, screens and filter distributor arms, and these consequently lead to
increase maintenance costs.

Application of Oil and Grease data in Environmental Engineering:

Oil and Grease may interfere with aerobic and anaerobic biological processes and
lead to decreased wastewater treatment efficiency. The limits are set in order to control
the amount of OG entering natural bodies of water or reservoirs through industrial
discharges, and also to limit the amount present in drinking water.

RESULT:
The quantity of oil and grease present in the given sample is....................................mg/L.

53
OBSERVATION:
S.No. Particulars Value

1 Volume of sample taken

Wt. of empty evaporating dish = W1 mg (For total
2
dissolved solids)
3 Wt. of dish after evaporation of sample = W2 mg

4 Total solids = (W2 – W1) mg

5 Wt. of dish after ignition in muffle furnace = W3 in mg

6 Fixed solids in mg = (W3 – W1) mg

Wt. of empty evaporating dish = W4 mg (For total
7
dissolved solids)
8 Wt. of dish after evaporation of filtrate = W5 mg

9 Total dissolved solids = (W5 – W4) mg

CALCULATION:

1. mg/l of total solids = total solids (mg) × 1000

ml of sample

2. mg/l of total fixed solids = total fixed solids (mg) × 1000

ml of sample

3. mg/l of total dissolved solids = total dissolved solids (mg) ×1000

ml of sample
4. mg/l of total suspended solids= mg/l of total solids – mg/l of total dissolved solids

5. mg/l total volatile solids= mg/l of total solids – mg/l of total fixed solids

6. Total settleable solids (ml/L) = (ml of solids x 1000) / ml of sample

54
Ex.No.:
DETERMINATION OF SUSPENDED, SETTLEABLE,
Date: VOLATILE AND FIXED SOLIDSLIDS IN WASTEWATER
AIM:

The aim of the experiments is to determine concentration of suspended,

volatile, fixed and settleable solids in wastewater.

APPARATUS:

1. Porcelain evaporating dishes of 150–200 ml capacity

2. Steam bath
3. Drying oven
4. Desiccators
5. Analytical balance or monopan balance
6. Filter paper (preferably of glass fibre)
7. Electric muffle furnace
8. Imhoff cone
PROCEDURE:

(a) Total solids

1. Ignite the clean evaporating dishes in the muffle furnace for 30 minutes at
550°C and cool in desiccators.
2. Note down the empty weight of the dish (W1).
3. Pour a measured portion (10 ml) of the well-mixed sample into the dish and
evaporate the contents by placing the dish on a steam bath.
4. Transfer the dish to an oven maintained at either 103–105°C or 179–181°C and
dry it for 1 hour.
5. Allow the dish to cool briefly in air before placing it, while still warm in
desiccators to complete cooling in a dry atmosphere.
6. Weigh the dish as soon as it has completely cooled (W2).
7. Weight of residue = (W2 – W1) mg.

(b) Total fixed solids

1. Keep the same dish used for determining total residue in a muffle furnace for
15 minutes at 550°C.
2. Allow the dish to partially cool in air until most of the heat has dissipated, then
transfer to a desiccators for final cooling in a dry atmosphere.
3. Weigh the dish as soon as it has cooled (W3).
4. Weight of total fixed residue = (W3 – W1) mg.

55
 (c) Total dissolved solids
1. Filter a measured portion of the mixed sample (10 ml) through a filter
paper and collect the filtrate in a previously prepared and weighed
evaporating dish.
2. Repeat the steps 3 to 6 outlined in total solids procedure.
3. Weight of dissolved solids = (W5 – W4) mg.
W4 = Weight of empty evaporating dish in mg.
W5= Weight of empty evaporating dish in mg + Residue left after evaporating
the filtrate in mg.

(d) Total Settleable solids

1. Gently fill the Imhoff cone with the thoroughly well mixed sample usually one
litre and allow it to settle.
2. After 4 minutes, gently rotate the cone between hands to ensure that all solids
adhering to the sides are loosened.
3. Allow the solids to settle for 15 minutes more, to make up for a total period of 1
hour.
4. Read the volume of the sludge which has settled in the apex.
5. Express the results in ml settleable solids per litre of sample per hour.

Environmental Significance of solids in water:

Suspended Solids: Suspended material may be objectionable in water for several reasons.
Biologically active suspended solids may include disease causing organisms as well as
organisms such as toxin producing strains of algae.
Fixed and volatile solids: The presence of high volatile solids indicates that the water may
have been polluted by domestic wastes or organic wastes. Well waters may have high
volatile solids due to lack of proper protection around well to prevent seepage of used
water.

Application of Solids data in Environmental Engineering practice:

Suspended Solids: Estimation of total suspended solids is useful to evaluate strength of
domestic wastewater and efficiency of treatment units.
Fixed and volatile solids: Helpful in assessing the amount biologically inert organic
matter, such as lignin in the case of wood-pulping waste liquors.
Settleable solids: Widely used in wastewater treatment plant operation to determine the
efficiency of sedimentation units.

56
RESULT:
The given water sample contains

1. Suspended solids = ____ ____mg/l.

2. Volatile solids = ____ ____mg/l.

3. Fixed solids = ____ ____mg/l.

4. Settleable solids = ____ ____mg/l.

57
TABULATION

Volume of Concordant
Burette Reading (ml) Volume of Sodium
S.No, the given burette reading
thio sulphate (ml)
sample (ml) Initial Final (ml)

CALCULATION:
1 ml of 0.025 N Sodium thiosulphate is equivalent to 0.2 mg of O2, since the volume of the
sample is 200 ml.

1 ml of Sodium thiosulphate is equivalent to

0.2 x 1000 mg/L = 1 mg/L

200

DO in (mg/l) = (V2 x N x 8 x 1000)

V1
V2 = Volume of Burette solution (ml)

V1 = Volume of Sample taken (ml)

N = Normality of Sodium Thiosulphate (N)

58
Ex.No.:
DETERMINATION OF DISSOLVED OXYGEN
Date:

AIM:

To determine the quantity of Dissolved oxygen present in the given sample.

APPARATUS REQUIRED:

1. BOD bottle (300ml)

2. Conical flask
3. Burette
4. Pipette
5. Measuring jar

REAGENTS REQUIRED:

1. Sodium Thiosulphate (0.025N)

2. Manganous Sulphate
3. Alkali- iodide azide reagent
4. Starch indicator
5. Conc. Sulphuric Acid

PROCEDURE

1. Take the BOD bottle and collect 300 ml of water sample into it.
2. Add 2 ml of each MnSO4 and 2 ml alkali iodide solution.
3. Place the stopper and shake the contents well by inverting the bottle. Keep the
bottle for sometimes to settle.
4. If no oxygen is present, the manganous ion reacts with hydroxide ion to form
white precipitate. If oxygen is present, it turns brown coloured manganous
oxide.
5. After shaking and allowing sufficient time for all oxygen to react, the chemical
precipitates are allowed to settle leaving clear liquid within the upper portion.
6. Add 2 ml of conc. H2SO4 and shake the bottle well to dissolve the precipitate.
7. Take 203 ml of sample from the BOD bottle and titrate it against Sodium
thiosulphate using starch as indicator. End point is change of color from blue
to colourless solution.

Environmental Significance of Dissolved Oxygen: Oxygen is poorly soluble in water.

Its solubility is about 14.6 mg/L for pure water at 0°C under normal atmospheric

59
pressure and it drops to 7 mg/L at 35°C. Aerobic bacteria survive when free oxygen is
available in plenty. End products of aerobiosis are stable and are not foul smelling.
While a minimum D.O of 4 to 5 mg/L is desirable for the survival of aquatic
life, higher values may cause corrosion of iron and steel.
Drinking water should be rich in D.O for good taste.

Application of Dissolved Oxygen data in Environmental Engineering Practice:

1. It is necessary to know D.O levels to assess quality of raw water and to keep a
check on stream pollution.
2. Oxygen is an important factor in the corrosion of iron and steel. D.O test is used to
control oxygen in boiler feed waters.
3. D.O test is used to evaluate the pollution strength of domestic and industrial
wastes.
4. Determination of D.O in wastewater is useful to identify the nature of biochemical
reactions whether it is aerobic or anaerobic.

RESULT

Amount of dissolved oxygen present in the given sample =____ ___ _ mg/L

60
CALCULATION: (for sample)

Initial D.O.

Sodium Thiosulphate Vs given sample

Volume of
Volume of Burette Reading (ml)
Concordant Sodium
the given
S.No, burette thio
soil sample
Initial Final reading (ml) sulphate
(ml)
(ml)

DO in (mg/l) = (V2 x N x 8 x 1000)

V1
V2 = Volume of Burette solution (ml)

V1 = Volume of Sample taken (ml)

N = Normality of Sodium Thiosulphate (N)

Final D.O:

Sodium Thiosulphate Vs given sample

Volume of
Volume of Burette Reading (ml)
Concordant Sodium
the given
S.No, burette thio
soil sample
Initial Final reading (ml) sulphate
(ml)
(ml)

DO in (mg/l) = (V2 x N x 8 x 1000)

V1

61
Ex.No.:
DETERMINATION OF BIO-CHEMICAL OXYGEN DEMAND
Date: (B.O.D test)

AIM:

To determine the Bio-Chemical Oxygen Demand in the given wastewater sample.

APPARATUS REQUIRED:

1. BOD incubator
2. BOD bottle (300ml)
3. Conical flask
4. Burette
5. Measuring jar

REAGENTS REQUIRED:

1. Sodium Thiosulphate (0.01N)

2. Manganese Sulphate
3. Alkali- iodide
4. Conc.H2SO4
5. Starch
6. Phosphate Buffer Solution
7. Magnesium Sulphate Solution
8. Calcium Chloride Solution
9. Ferric Chloride Solution
10. Manganese Sulphate Solution

SHORT PROCEDURE:

S.NO. CONTENT REAGENT

1 Burette solution Sodium Thiosulphate

2 Conical flask solution 50ml of prepared waste water sample

3 Additional solutions
4 Indicator
1 ml of Manganese Sulphate solution
is added, followed by 1 ml of Alkali-
Iodide. After 5 minutes add slowly 1
ml of Conc.Sulphuric Acid.
starch indicator

5 End point Disappearance of blue colour.

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CALCULATION: (for blank)

Initial D.O:

Sodium Thiosulphate Vs blank sample

Volume
Volume of Burette Reading (ml)
Concordant of
the given
burette Sodium
S.No, soil
reading thio
sample Initial Final
(ml) sulphate
(ml)
(ml)

DO in (mg/l) = (V2 x N x 8 x 1000)

V1
V2 = Volume of Burette solution (ml)

V1 = Volume of Sample taken (ml)

N = Normality of Sodium Thiosulphate (N)

Final D.O.

Sodium Thiosulphate Vs blank sample

Burette Reading (ml) Volume of

Volume of
Concordant Sodium
the given
S.No, burette thio
soil sample Initial Final reading (ml) sulphate
(ml)
(ml)

DO in (mg/l) = (V2 x N x 8 x 1000)

V1

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PROCEDURE

1. Distilled water is aerated for 4 hours to attain saturated Dissolved Oxygen

(DO) level. In distilled water 1 ml of each nutrient (Phosphate buffer,
Magnesium Sulphate, Calcium Chloride and Ferric Chloride) and 1 ml of pre
acclimatized seed per 1 litre of distilled water is added.
2. Two BOD bottles are taken. The wastewater sample 5 ml is taken in the BOD
bottles and then 245 ml of aerated water is filled. DO test is conducted for the
one BOD bottle sample by the following steps and initial DO is noted.
3. 1 ml of Manganese Sulphate solution is added, followed by 1 ml of Alkali –
Iodide – Azide reagent. Then the bottle is mixed twice and allowed to
precipitate settle for 5 minutes.
4. 1 ml of Conc. Sulphuric Acid is added slowly and mixed twice. 200 ml of
sample is taken and titrated against Sodium Thiosulphate solution with starch
indicator.
5. Disappearance of blue colour is taken as end point. Volume of Sodium thio
Sulphate consumed is noted.
6. Another bottle is placed in incubator at 20⁰ C. After 5 days DO test is
conducted and final DO is noted.

Environmental Significance of BOD

BOD is the principle test to give an idea of biodegradability of any sample and
strength of the waste. It is the basic criteria for control of stream pollution.

Efficiency of any treatment plant can be judged by considering influent BOD and
effluent BOD.

Ordinary domestic sewage may have a BOD of 200 mg/L. Any effluent to be
discharged into natural bodies of water should have BOD less than 30 mg/L. Drinking
water usually has a BOD less than 1 mg/L.

Advantages of BOD data in Environmental Engineering practice:

1. To determine strength of domestic and industrial sewage.

2. To measure the self purification capacity of streams and serves regulatory
authorities as a means of checking on the quality of effluents discharged to such
waters.
3. Useful in estimating population equivalent of any industrial waste.
4. It is the only parameter to give an idea of biodegradability of any sample.

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 TABULATION:

Sl Volume of Dilution Initial D.O Final D.O of Initial D.O Final D.O 5 days
No sample ratio of the the sample of the of the BOD at
(ml) sample (mg/l) blank blank 20°C
(mg/l) (mg/l) (mg/l) (mg/l)

BOD CALCULATION:

BOD5 (mg/l) = [(Initial DO – Final DO) x dilution factor]

Where

Dilution factor = Volume of diluted sample

Volume of waste water sample added

65
RESULT

BOD5 of given sample at 20oC in mg/l =________

66
OBSERVATIONS:
Sample Vs FAS
Volume of Burette Reading (ml)
the given
Concordant Volume of FAS
S.No, soil
Initial Final value consumed (ml)
sample
(ml)

Blank Vs FAS
Volume of Burette Reading (ml)
the given
Concordant Volume of FAS
S.No, soil
Initial Final value consumed (ml)
sample
(ml)

CALCULATION:
Total Chemical Oxygen Demand (mg/l) = (A−B × N × 8000) /V
Where,

A – Volume of Ferrous Ammonium Sulphate used for blank solution

B – Volume of Ferrous Ammonium Sulphate used for sample titration
N – Normality of Ferrous Ammonium Sulphate solution
V – Volume of wastewater sample taken

67
Ex.No.:
DETERMINATION OF CHEMICAL OXYGEN DEMAND (C.O.D
Date: test)
AIM:

To determine the Chemical Oxygen Demand in the wastewater sample.

APPARATUS REQUIRED:

1. COD Reactor
2. Burette with stand & Pipette
3. Measuring jar
4. Reflux apparatus
5. Beakers
6. Conical flask
7. Hot plate
REAGENTS REQUIRED:

1. Std. Potassium dichromate (0.25 N)

2. Sulphuric acid reagent (Con. H2SO4 + Ag2SO4)
3. Ferroin indicator solution
4. Std. Ferrous ammonium sulphate (0.1 N)
5. Mercuric Sulphate

SHORT PROCEDURE:

S.NO. CONTENT REAGENT

1 Burette solution
2 Conical flask solution
4 Salt
3 Additional solutions
4 Indicator
Std.Ferrous Ammonium sulphate
150 ml of prepared waste water
sample & 150 ml of prepared distilled
water sample(blank)
0.4 gm of Mercuric Sulphate crystal
10ml of more concentrated
dichromate solution with glass beads
and then add slowly 30 ml of H2SO4
containing Ag2SO4
Ferroin indicator.

5 End point Blue green to wine red.

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 PROCEDURE:

1. Place 0.4 g of H2SO4 in the reflux flask.

2. Add 20 ml of sample (or an aliquot diluted to 20 ml)
3. 10 ml of more concentrated dichromate solution are placed into flask
together with glass beads.
4. Add slowly 30 ml of H2SO4 containing Ag2SO4 and mix thoroughly.
5. Connect the flask to condenser. Mix the contents thoroughly before heating.
6. Reflux for a minimum period of 2 hours. Cool and wash down the condenser
with distilled water.
7. Dilute the sample to make up 150 ml and cool.
8. Titrate excess K2Cr2O7 with 0.1N Fe (NH4)2SO4 using ferroin indicator.
9. Sharp colour change from blue green to wine red indicates the end point.
10. Reflux the blank in the same manner using distilled water instead of sample.
Environmental Significance of COD:

1. BOD cannot be determined accurately when toxins are present and conditions are un favour
for the growth of microbes.
2. BOD test consumes more time i.e a minimum of 5 days where COD test is relatively faster
than BOD taking only 3hr for completion.
3. A BOD value close to COD indicates that the waste is highly biodegradable.

Application of COD data in Environmental Engineering practice:

1. COD test used extensively in the analysis of industrial wastes.
2. It is particularly valuable in survey system to determine and control losses in sewer system.
3. This test is widely used in place of BOD in the operation of treatment facilities because of the
speed with which the result can be obtained.
4. It is useful to assess the strength of waste which contains toxins and biological resultant and
organic substance.
5. The ratio of BOD to COD is useful to Access the amenability of waste for biological treatment.
6. The ratio of BOD to COD is greater than or equal to 0.8 indicates that the waste water are
highly amenable to biological treatment.

RESULT:

The COD of the given sample in mg/l is -----------------------

69
OBSERVATIONS:
Volume of sample (ml) showing positive result MPN index /
Sample
0.1 1 10 100 ml

70
Ex.No.:

Date:
DETERMINATION OF MPN INDEX

AIM:

To determine the Most Probable Number (MPN) (Viable count) of bacteria by

multiple – tube fermentation method.

APPARATUS REQUIRED:

1. Culture tubes
2. Autoclave
3. Incubator
4. Sterilized graduated pipettes
5. Nutrient – broth sample
6. Durham’s (tubes) vial
REAGENTS REQUIRED:
1. Lauryl tryptose broth
2. Brilliant green bile broth
3. Endo or Eosin methlene blue agar
4. Reagents for gram staining
PROCEDURE:

1. The 15 test tubes were thoroughly cleaned and boiled. Then the tubes were
sterilized after plugging them with non-absorbent cotton wool
2. The dilution was selected according to the expected coli form.
• 5 tubes of 10 ml double strength medium with 10 ml coli forms
• 5 tubes of 10 ml single strength medium with 1 ml sample.
• 5 tubes of 10 ml single strength medium with 0.10 ml sample.
3. The MPN fermentation tubes were inoculated with appropriate measured
quantities of water sample to be tested.
4. Appropriate quantity of Lauryl tryplose broth in each tube was added.

71
 5. One Durham’s vial was put inverted in each test tube. The top of the test tubes
was plugged with cotton plug.
6. All these tubes were placed in an incubator at 35 – 37oC for 48 hours.
7. After 48 hrs. the tubes were examined carefully. Those showing gas in the
Durham’s vial were recorded as positive.
8. The absence of gas formation at the end of 48 hrs of incubation was considered
as negative.
9. The results were interpreted by reference to the MPN Table.

Environmental Significance of MPN Index

1. The purpose of this test is to estimate the number of coliforms in water sample as
an index of the magnitude of biological contamination.
2. Each person discharges 100 to 400 billion coliform organisms per day, in addition
to other kinds of bacteria. Coliforms are harmless to man and are in fact useful in
destroying organic matter in biological waste treatment processes.
3. Pathogenic organisms present in wastes and polluted water are few, whereas
coliform are more numerous, more easily tested, and thus used as an indicator
organism.
4. The presence of coliform organisms are taken as an indication that pathogenic
organism may also present and absence is taken as an indication that the water is
free from disease producing organisms.

Application of MPN data in Environmental Engineering practice:

1. MPN determination is useful in the selection of water supplies for human needs.
2. It is useful to assess the degree of contamination of receiving waters due to
domestic sewage.
3. It is useful to find efficiency of disinfectant and treatment units efficiency in
pathogenic bacterial removal.

RESULT:
The MPN index / 100 ml in the given sample

72
CALCULATION:

73
Ex.No.:
DETERMINATION OF SVI OF BIOLOGICAL SLUDGE AND
Date: MICROSCOPIC EXAMIANTION

AIM:

To determine the Sludge Volume Index (SVI) in the given sample

APPARATUS REQUIRED:
1. 1 lit beaker
2. Stirrer rod
PROCEDURE:
1. Take 1 lit beaker with measurement.

2. Collect a gallon of sludge, mix gently, and pour into the beaker. Wait for settlement.

3. After 30 minutes, the sludge settles at bottom.

4. Record the volume to which the sludge settles.

Environmental Significance of SVI:

1. SVI indicates changes occurring in the activated sludge treatment process.
2. A high SVI may also indicate filamentous sludge bulking.

Applications of SVI data in Environmental Engineering practice:

1. SVI indicates the MLSS concentration in Secondary treatment units of wastewater
treatment plants.
2. F/M ratio in treatment plants is maintained with SVI parameter.

RESULT:
The SVI of given sample is = ____________________ml/g

74