GUDLAVALLERU ENGINEERING COLLEGE WATER

AND WASTEWATER ENGINEERING LAB

GUDLAVALLERU ENGINEERING COLLEGE

SESHADRI RAO KNOWLEDGE VILLAGE:
GUDLAVALLERU

DEPARTMENT
OF
CIVIL ENGINEERING

III B.Tech - I Sem

2021– 22
 WATER AND WASTEWATER ENGINEERING LAB

Name : …………………………………………………………..

Regd. No :……………………………………………………………

Year & Semester: ………………………………………………………..

Academic Year : ……………………………………………………….

GUDLAVALLERU ENGINEERING COLLEGE

SESHADRI RAO KNOWLEDGE VILLAGE: GUDLAVALLERU
DEPARTMENT OF CIVIL ENGINEERING
 GUDLAVALLERU ENGINEERING COLLEGE
SHESHADRI RAO KNOWLEDGE VILLAGE
GUDLAVALLERU
DEPARTMENT OF CIVIL ENGINEERING

INDEX

SIGNATURE
SL DATE
NAME OF THE EXPERIMENT OF THE
NO
FACULTY
.

Determination and Estimation of Total ,Volatile , Dissolved ,

1
Suspended Solids

2 Determination of Chlorides

Determination of Optimum Coagulation Dose

3

Determination of Chlorine Demand

4

5 Estimation of settleable solids using Imhoff Cone

6 Determination of Dissolved Oxygen with D.O. Meter

7 Determination of B.O.D

8 Determination of C.O.D

9 Determination of Fluorides in water

10 Determination of Nitrates

11 Determination of Sulphates

Determination of Iron
12

Determination of Phosphorous
13
 1. Estimation of Total, Volatile, Settleable, Dissolved, Suspended Solids
Aim:
To determine the total solids, dissolved solids and settleable solids

Apparatus and equipment:

a. Electrically heated temperature controlled oven
b. Weighing balance
c. Evaporating dish
d. Pipettes
e. Measuring cylinder (100mL)
f. Muffle furnace
g. Whatmann filter paper (No. 42)

Introduction:
The term ‘solid’ refers to the matter either filterable or non-filterable that remains as residue upon
evaporation and subsequent drying at a defined temperature. Further categorization depends upon depends
upon the temperature employed for drying and ignition. Different forms of solids are defined on the basis of
method applied for their determination. Solids may affect water or effluent quality adversely in number of ways.
Water with high dissolved solids may include an unfavourable physiological reaction in the transient consumer
and generally are of inferior palatability. Highly mineralized waters are unsuitable for many industrial
applications. High suspended solids in waters may be aesthetically unsatisfactory for such purposes as bathing.
Analysis of total solids are important to decide upon the various unit operations and processes in physical and
biological wastewater treatment and to assess its performance evaluation. For assessing compliance with
regulatory agency, wastewater effluent limitations forvarious forms of solids act as indicating parameters.
A. Total solids
Principle
Residue left after the evaporation and subsequent drying in oven at specific temperature 103-105°C of a
known volume of sample are total solids. Total solids include “Total suspected solids” (TSS) and “Total
dissolved solids” (TDS). Whereas loss in weight on ignition of the same sample at 500°C, in which organic
matter is converted to CO2 volatilization of inorganic matter as much as consistent with complete oxidation of
organic matter, are volatile solids.
Sample collection, preservation and storage
The water samples may be collected in resistant glass or plastic bottle. Water has considerable solvent
property. There is possibility of increase in mineral content of sample, if water is collected and stored in non-
resistant glass bottle. The effect is pronounced with alkaline water. Exclude particles such as leaves, sticks, fish
and lump of feacal matter in the sample. Begin analysis as soon as possible due to impracticality of
preservation of sample.
Procedure
1. Take the empty weight of the thoroughly cleaned dish.(W1)
2. Take 20 ml of a well-mixed sample in the same dish.
3. Evaporate the sample to dryness at 103-105°C in hot air oven.(4-5h)
4. Cool in desiccator, weigh and record the reading (W2)
5. Take the same crucible and ignite the dish for 30 minutes in a muffle furnace maintainedat 550°C.
 6. Cool the dish in a desiccator and record final weight (W 3).
7. The concentration is to be calculated in percent by weight.
Procedure for dissolved solids
1. Take the empty weight of the dish (W4)
2. Take 25 ml of sample and filter it using Whatmann filter paper (No. 42) using the filtrationassembly.
3. Pour the filtrate into the dish and evaporate the sample to dryness at 103-105°C in hot air oven.
4. (4-5 h).
5. Cool in desiccator, weigh and record the reading (W5)
Procedure for settleable solids
1. Fill an Imhoff cone to the l-L mark with a well-mixed sample).
2. Settle for 45-min, gently agitate sample near the sides of the cone with a rod or by spinning,
settle 15 min longer, and record volume of settleable solids in the cone asmL/L.
3. If the settled matter contains pockets of liquid between large settled particles, estimate volume of
these and subtract from volume of settled solids.
4. The practical lower limit of measurement depends on sample composition and generally is in the
range of 0.1 to 1.0 mL/L. where a separation of settleable and floating materials occurs, do not
estimate the floating material as settleable matter.
5. Replicates usually are not required

Observation:

S.No Details Notations Weight(g)

1. Weight of empty crucible W1
2. Weight of crucible with water sample W2
after ovendrying.
3. Weight of crucible with water sample W3
after taking it from muffle furnace.
4. Weight of empty crucible W4
5. Weight of crucible with filtrate after W5
ovendrying.

Calculation:
Total solids (TS) = (W2-W1)/volume of sample
Total dissolved solids (TDS)= (W5-W4) /volume of sample
Total suspended solids (TSS) = TS-TDS
Total fixed solids (TFS) = (W3-W1) / volume of sample
Total volatile solids = (TVS) = TS- TFS =
Total Settleable solids =
Results:
The solids present in the given wastewater are reported below
• Total solids =
• Dissolved Solids =
• Suspended solids =
• Fixed solids =
• Volatile solids =
• Settleable solids =
•
Inference:

Water can be classified by the amount of TDS per litre:

• Fresh water < 1500 mg/l TDS
• Brackish water = 1500 to 5000 mg/l TDS
• Saline water > 5000 mg/l TDS
 2.Determination of Chlorides

Aim: To find the amount of chlorides present in the given water sample.

Apparatus Required: Burette, Conical flask, Pipette, Measuring jar.

Theory:

Chlorides are generally present in water in the form of Sodium Chloride (Common Salt) and may be due to
leaching of marine sedimentary deposits, pollution from the sea water, brine or industrial and domestic
waste etc. Chloride occurs in all natural waters in widely varying concentrations. The chloride content
normally increases as the mineral content increases. Upland and mountain supplies usually are quiet low in
chlorides, whereas river and ground waters usually have a considerable amount. Human excreta,
particularly the Urine contain chloride in an amount about equal to the chlorides consumed with food and
water. This amount average about 6gm of chlorides/person/day and increases the amount of Cl - in sewage
about 15mg/l above that of the carriage water.

Chlorides in reasonable concentrations are not harmful to humans. At concentrations above 250mg/l they
give a salty taste to water which is objectionable to many people. For this reason, the US Public Health
Service recommends that chlorides be limited to 250mg/l in supplies intended for public use. The sudden
increase of chlorides in water of low chloride concentration, is indicative of organic pollution. A high
chloride content also exerts a deleterious effects on metallic pipes and structures, as well as on agricultural
plants.

Principle:
Silver Nitrate react with chloride to form very slightly soluble white precipitate of AgCl. At the end point
when all the chlorides get precipitated free silver ions react with chromate to formreddish brown colour.

Reagents:
Silver Nitrate (0.014N), Potassium Chromate

Procedure:

• Take 20 ml o f water sample in a conical flask.

• Add 1-2 ml Potassium chromate indicator solution, then colour of the sample changes to yellow.
• Titrate the sample against 0.014N silver nitrate solution until the colour changes from yellow to brick
red
• Record the volume of silver nitrate used.
• Repeat the process until two successive consecutive readings.
Table:
Sl. No Volume of Burette Reading (ml) Volume of Silver
sample (ml) Nitrate used
Initial Reading (A) Final Reading
(A-B)(ml)
(B)

Calculation:

Chlorides, mg/l = ml of AgNo3 X Normality of AgNo3 X Eq.wt of chlorine X1000

ml of Sample

Result:
The amount of chlorides present in the given water sample is ----------

Inference:
 3.Determination of Optimum Coagulant dosage

Aim: To find out the optimum coagulant required to precipitate turbid particles present in the water.

Apparatus Required:
Jar test apparatus, Beakers – capacity 1000ml – 6nos, Turbidimeter, pH meter, Turbid water, pipettes,
Graduated measuring cylinder – 1000ml
Reagents: Coagulant (Alum solution)

Theory:
Chemical Coagulation is an important process applied extensively in water treatment practice, particularly
where surface supplies are involved. It is also used to some extent in domestic and industrial waste
treatment.

Chemical coagulation of water is performed for several reasons. The major ones are removal of i) turbidity,
organic and inorganic ii)colour, true, apparent iii) Harmful bacteria and other pathogens iv) algae and other
plankton organisms v) taste and odour producing substances and vi) Phosphates, which serve as nutrients
for growth of algae

Chemicals used for coagulation of water, sewage and industrial wastes react with water to form insoluble
hydroxide precipitates.

Much of the suspended matter in water, is colloidal in nature. This is particularly true of substance that
cause colour and turbidity. The colloidal matters are negatively charged, and for this reason, the salts of
trivalent metals, usually iron and aluminium are used to coagulate them.

The usual coagulants used for coagulation are Aluminium Sulphate, Chlorinated Copperas, Ferrous
sulphate and lime, Magnesium carbonate, Sodium Aluminate and Polyelectrolytes etc…

The reactions involved in chemical coagulation are essentially the same for both ferric and aluminium
sulphates (usually called filter alum). Filter alum [Al2(SO4)3.18H2O] is most widely used. The various
positive species which are formed may combine with negatively charged colloids to neutralize part of the
change on the colloidal particle
Principle:
Metal salts hydrolyze in the presence of the natural alkalinity to form metal hydroxides. The divalent cation
can reduce the zeta potential while the metal hydroxides are good absorbents and hence remove the
suspended particles by enmeshing them.
Procedure:
1. Take equal volume of sample in each jar.
2. Adjust the jars in such a way that moving paddles remain at the center of jars and merged in samples
3. Add increasing doses of coagulant of known strength to each jar (i.e., 2ml, 4ml, 6ml ……)
4. Now rotate the paddles with the help of driving unit at a constant speed of approximately 120 rpm for 2 to
3 mins
5. Reduce the speed to 40 to 60 rpm for a period of 30 mins
6. These jars are allowed to stand still for 15 mins.
7. Take the sample out of the beaker and test for turbidity in each trial
8. Plot the graph between dose of coagulant and turbidity
9. The least turbidity of the sample shows the Optimum dose of coagulant

Observations:

Volume of sample taken:

Jar ml of alum Dosage of pH Residual % Removal of

No added alum (mg/L) Turbidity Turbidity

Result:
The optimum dosage of coagulant required to remove turbidity in the given water sample is
_____________________mg/L
 4.DETERMINATION OF CHLORINE DEMAND

AIM: To find the residual chlorine available and chlorine demand in the given sample.

PRINCIPLE:
Ortholidine is an organic compound that is oxidized agents to produce a yellow colored
compound called "Holoquinone". Intensity of yellow color of Holoquinone is proportional to the
amount of chlorine present.

INTERFERENCE:
Oxidizing agents such as ferric compounds, manganic salts, nitrites etc.

APPARATUS:
Chloroscope.

REAGENT:
Orthotolidine reagent.

PROCEDURE:
1. Take the water sample under question into one of the cylinders of the comparator and
distilled water into the other.
2. Add 5 drops of Orthotolidine solution to both the cylinders and put them in thecomparator.
3. The color which matches in both the cylinders directly gives the residual chlorine.

OBSERVATION AND RESULTS:

Amount of residual chlorine (mg/l)=0.1mg/l

ENVIRONMENTAL SIGNIFICANCE:

 Chlorine residuals determination is used to control Chlorination of domestic and industrial

wastewaters.
 Active chlorine (free and combined) should be determined at each stage in the treatment
process of drinking water and in the water mains in order to guarantee a bacterologically
impeccable water.
 Active chlorine should be present in drinking water within the range of 0.1 to 0.2 mg/l.
However excessive chlorine content may give out bad odor and may change even taste of
water. Further chlorine is said to be earainogenous. Hence except during epidemic
'super chlorination' not to be done.

APPLICATION OF RESIDUAL CHLORINE DATA IN ENVIRONMENTAL

ENGINEERING PRACTICE:

1. Chlorine residual determination is said to control chlorination of domestic and industrialwaste

waters.
2. Determination of chlorine residuals is used universally in disinfection practice to control
addition of chlorine so as to ensure effective disinfection without taste.
3. 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 consumer.

RESULT:
Amount of residual chlorine (mg/l) is …………..
5. ESTIMATION OF SETTLEABLE SOLIDS USING IMHOFF CONE

AIM: To find out total settle able solids of the given sample

PRINCIPLE:
The particles in suspension whose specific gravity greater than that of water willsettle
under quiescent conditions.

APPARATUS:
1. Imhoff cone
2. Holding device

ENVIRONMENTAL SIGNIFICANCE:
Total solids measurements can be useful as an indicator of the effects of runoff from
construction, agricultural practices, logging activities, sewage treatment plant discharges, and
other sources. Total solids also affect water clarity. Higher solids decrease the passage of light
through water, thereby slowing more rapidly and hold more heat; this, in turn, might adversely
photosynthesis by aquatic plants. Water will heat up affect aquatic life that has adapted to a lower
temperature regime. As with turbidity, concentrations often increase sharply during rainfall,
especially in developed watersheds. They can also rise sharply during dry weather if earth
disturbing activities are occurring in or near the stream without erosion control practices in place.
Regular monitoring of total solids can help detect trends that might indicate increasing erosion in
developing watersheds. Total solids are related closely to stream flow and velocity and should be
correlated with these factors. Any change in total solids over time should be measured at the same
site at the same flow.
1. In the case of water:
Water with total solids generally is of inferior palatability and may induce an
unfavorable physiological reaction. It may be esthetically unsatisfactory for purposes such as
bathing. Total solids will be higher in highly mineralized waters, which result in unsuitability
for many industrial applications. It indicates effectiveness of sedimentation process and it
affects effectiveness of disinfection process in killing microorganisms. It is used to assess the
suitability of potential supply of water for various uses. In the case of water softening, amount
of total solids determine the type of softening procedure. Corrosion control is frequently
accomplished by the production of stabilized waters through pH adjustment. The pH
stabilization depends to some extent upon the total solids present as well as alkalinity and
temperature.
2. In the case of waste water:
Solids analyses are important in the control of biological and physical wastewater treatment
processes and for assessing compliance with regulatory agency wastewater effluent limitations
Although the waste water or sewage normally contains 99.9 percent of water and only 0.1 percent of
solids, but it is the solids that have the nuisance value. The amount of solids in wastewater is
frequently used to describe the strength of the water. The more solids present in a particular
wastewater, the stronger that wastewater will be. The environmental impacts of
solids in all forms have detrimental effects on quality since they cause putrefaction problems. If the
solids in wastewater are mostly organic, the impact on a treatment plant is greater than if the solids
are mostly inorganic.

PROCEDURE:
1. Gently fill the imhoff cone with the thoroughly well mixed sample usually 1 liter andallow it
to settle.
2. After 45 minutes gently rotate the cone between hands to ensure that all solidsadhering
to the sides are loosened.
3. Allow the solids to settle for 15 minutes more ,to make up for a total period 1 hour
4. Read the volume of the sludge which has settled in the apex.
5. Express the results in ml settle able solids per liter of sample per hour

CALCULATION:
Total Settle able Solids (mg\l) = ml of solids *1000
ml of sample

PRECAUTION:
1. The imhoff cone must be clean with a strong soap and hot water using the brush.
2. Wetting the cone with water before use helps in preventing adherence of solids to the
sides.
3. The method is subjected to considerable inaccuracy if the solids contain large
fragments.
4. The determination of total settle able solids should be carried out soon after samplingin
order to avoid errors through flocculation

OBSERVATIONS & RESULTS:

Sample details Volume of sample taken Total settle able solids

(ml) (ml\l\hr)

APPLICATIONS OF TOTAL SETTLEABLE SOLIDS DATA IN E.E. PRACTICE:

1. The settle able solids determination is used extensively in an analysis of industrialwaste

to determine the need for and design of plain settling tanks in plants employing
biological treatment process.
2. It is also widely used in waste water treatment plant operation to determine the
efficiency of sedimentation units.

RESULTS:
Total settleable solids =
6. DETERMINATION OF DISSOLVED OXYGEN WITH D.O. METER

AIM: To determine the DO value of given water sample.

INTRODUCTION:
The reagent MnSo4 reacts with the alkaline to form Mn(OH)2 (white precipitate).If
oxygen is present, it will oxidize Mn(OH)2 to MnO(OH)2 (brown precipitate).If H2SO4 is
added the brown precipitate is dissolved to form MnSo4which immediately reacts with KI
already added and liberates Iodine equivalent to the quantity of oxygen originally present in
the sample. The amount of iodine is estimated by titration against sodium thiosulphate
solution, using starch indictor.

EQUIPMENT AND REAGENTS:

1. Dissolved oxygen sampler
2.300ml glass stopper BOD bottle
3. Manganese sulphide
4. Alkaline Iodide Azide reagent
5. Sulphuricaci (H2So4)
6. Starch solution
7. Sodiumthiosulphate solution (0.025N)

ENVIRONMENTAL SIGNIFICANCE:
Drinking water should be rich in dissolved oxygen for good taste. DO test is used to
evaluate the pollution strength of domestic and industrial waste. Higher values of DO may
cause corrosion of Iron and Steel. Algae growth in water may release oxygen during its
photosynthesis and DO may even shoot upto 30 mg/L. Oxygen is poorly soluble in water. Its
solubility is about 14.6 for pure water at 0°C under normal atmospheric pressure and it
drops to 7 mg/l at 35°C. Higher temperature, biological impurities, Ammonia, Nitrates, ferrous
iron, chemicals such as hydrogen sulphide and organic matter reduce DO values. Aerobic
bacteria thrive when oxygen is available in plenty. Aerobic conditions do prevail when
sufficient DO is available within water. End products of aerobiosis are stable and are not foul
smelling. It is necessary to know DO levels to assess quality of raw water and to keep a check
on stream pollution. DO test is the basis for BOD test which is an important parameter to
evaluate organic pollution potential of a waste. DO test is necessary for all aerobic biological
wastewater treatment processes to control the rate of aeration.

PROCEDURE:
1. Take a glass stopper BOD bottles of known value and fill it with sample to avoid air
bubbles.
2. No air should be trapped in the bottle after stopper is placed.
3. Open the bottle and put 1ml of manganese sulphate and add 1ml of alkali Iodide Azide
using separate pipette.
4. Place he stopper and shake the bottle thoroughly until a brown precipitate formed.
5. Add 2ml of Conc.H2So4 to dissolved the precipitate.
6. Transfer gently the whole of known part of the water sample in a conical flask .
7. Put a few drops of starch indicator and titrate against sodium thiosulphate solution.
8. The end point is from initial blue to colour less.

PRECAUTIONS:
1. Disgard any subsequent return of colour
2. If the end point is overrun back titrate with biniodate (0.025) and effect the necessary
correction
3. Avoid air bubbles while stoppering the bottle

OBSERVATION AND CALCULATION:

DO in mg/ l = ml of Na2S2O3 used
V∗N∗weight of O2∗1000
=
200
DO=titrate value (V)*Normality of hypo(N)/50(V2/V2-2)

RESULT:
The Dissolved oxygen in he given water=
 7.DETERMINATION OF BIOLOGICAL OXYGEN DEMAND
AIM: Determination of Biological Oxygen Demand in the given water sample

INTRODUCTION:
Biological Oxygen Demand is defined as the amount of oxygen required by micro-
organisms while stabilizing biologically decomposable organic matter of water under aerobic
conditions. The BOD test is widely used to determine
1. The pollution load of waste water.
2. The degree of pollution in lakes, streams at any time and their self purification capacity.
3. Efficiency of waste water methods.

APPARATUS:
1. BOD bottles
2. Incubator
3. Conical flask
4. Analytical balance
5. Burette
6. Pipette

CHEMICALS AND REAGENTS:

1. Manganese Sulphate solution
2. Calcium Chloride
3. Ferric chloride
4. Starch Indicator
5. Sodium Thiosulphate
6. Alkaline Iodide Azide and Conc.H2SO4

PRINCIPLE:
1. MnSO4 is added to the water sample containing alkaline manganese hydroxide.
2. It is oxidized to basic manganese oxide but the dissolved oxygen present in the water
sample.
3. When H2SO4 is added, the basic manganese oxide liberates iodine which isequivalent
to the DO present in the sample.
4. The liberated iodine is titrated with a standard hypo solution using starch as an
indicator
MnSO4+2KOH→Mn(OH)2+k2So2
2Mn(OH)2+O2→2Mn(SO4)2(Basic Manganese Oxide)
MnO(OH)2+H 2SO4→Mn(SO4)2+3H2O
2MnSO 4+2KI→K2SO4+MnSO4+I2

ENVIRONMENTAL SIGNIFICANCE:
BOD is the principle test to give an idea of the biodegradability of any sample and
strength of the waste. Hence the amount of pollution can be easily measured by it. Efficiency of
any treatment plant can be judged by considering influent BOD and the effluent BOD and so
also the organic loading on the unit. Application of the test to organic
waste discharges allows calculation of the effect of the discharges on the oxygen resourcesof the
receiving water. Data from BOD tests are used for the development of engineering criteria for the
design of wastewater treatment plants. 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.
This is important parameter to assess the pollution of surface waters and ground waters where
contamination occurred due to disposal of domestic and industrial effluents. Drinking water
usually has a BOD of less than 1 mg/L. But, when BOD value reaches 5 mg/L, the water is
doubtful in purity. The determination of BOD is used in studies to measure the self-purification
capacity of streams and serves regulatory authorities as a means of checking on the quality of
effluents discharged to stream waters. The determination of the BOD of wastes is useful in the
design of treatment facilities. It is the only parameter, to give an idea of the biodegradability of
any sample and self
purification capacity of rivers and streams. The BOD test is among the most important method in
sanitary analysis to determine the polluting power, or strength of sewage, industrial wastes or
polluted water. It serves as a measure of the amount of clean diluting water required for the
successful disposal of sewage by dilution.

PROCEDURE:
1. Prepare 100 ml of Distilled water and is taken in 3 BOD bottles
2. 1BOD bottle is used for initial DO determination
3. Take 1ml of CaCl2 and FeCl3 and add to other two BOD bottles containing water
sample
4. Place 2BOD bottles in incubator at constant temperature of 20 ͦc
5. During incubation water is protected from air. This can be done by keeping the
bottles in incubator for 3 days or 5 days.
6. The DO is determined in two bottles after 3 or 5 days.
OBSERVATION:
For Initial Sl.No Sample Capacity Volume Burette reading ml. of D.O. in
D.O Details of BOD of titrant mg l
bottle for sample used
titration taken Initial Final
1.
2.

For Final 1.
D.O 2.

CALCULATIONS:
BOD=initial DO-final DO/50
Final DO=DO of water sample for 3days or 5 days

RESULT:
The BOD in the given water sample is………