ENVIRONMENTAL ENGINEERING

LABORATORY MANUAL
DEPARTMENT OF CIVIL ENGINEERING
SEM V
 CONTENT

Sr. No Name of the Experiment

1 Determination Of pH in Water

2 To determine chloride ion concentration in a water sample.

3 Determination of Dissolved oxygen

4 To Determine the Alkalinity in a Given Water Sample

5 Measurement of Noise level

6 To Determine optimum coagulant dose

7 To Determine residual chlorine in a water sample

8 To determine Hardness of Water

 Experiment 1

Aim: Determination Of pH in Water

Theory: The pH is one of the basic water and wastewater characteristics. It expresses the
intensity of acid or alkaline conditions by indicating the hydrogen ion activity. Some of the
processes in water quality engineering that require pH monitoring and control are the following:
disinfection, coagulation, softening, biological treatment etc. Natural waters usually have pH
values close to neutral. Figure 1 shows pH values of commonly used household products.

Apparatus: 1. pH meter 2. Beaker

Reagent: 1. Buffers Solutions of known pH value

Sample handling and preservation of sample is not practical. Because biological activity will
continue after a sample has been taken, changes may occur during handling and storage. The
characteristics of the water sample may change. To reduce the change in samples taken for the
determination of pH, keep samples at 4°C. Do not allow the samples to freeze. Analysis should
begin as soon as possible

Procedure: Three major steps are involved in the experiment. They are

1. Preparation of Reagents

2. Calibrating the Instrument

3. Testing of Sample

Steps: Perform calibration of the pH meter using standard pH solutions. The calibration
procedure would depend on the pH range of interest. In a clean dry 100 mL beaker take the
water sample and place it in a magnetic stirrer, insert the Teflon coated stirring bar and stir well.
Now place the electrode in the beaker containing the water sample and check for the reading in
the pH meter. Wait until you get a stable reading. Take the electrode from the water sample,
wash it with distilled water and then wipe gently with soft tissue.
Result

Sr. Source Of Sample Temperature PH

NO
 Experiment 2

Aim: To determine chloride ion concentration in a water sample.

Theory: Chloride in the form of chloride (Cl) ion is one of the major inorganic anions in water
and wastewater. The chloride concentration is higher in wastewater than in raw water because
sodium chloride is a common article of diet and passes unchanged through the digestive system
(Average estimate of excretion: 6 g of chlorides/person/day; additional chloride burden due to
human consumption on wastewater: 15 mg/L). Along the sea coast chloride may be present in
high concentration because of leakage of salt water into the sewage system. It also may be
increased by industrial process. In potable water, the salty taste produced by chloride
concentration is variable and depends on the chemical composition of water. Some waters
containing 250 mg/L Cl may have a detectable salty taste if sodium cation is present. On the
other hand, the typical salty taste may be absent in waters containing as much as 1000 mg/L
when the predominant cations are calcium and magnesium. In addition, a high chloride contents
may harm metallic pipes and structures as well as growing plants.

The measured chloride ions can be used to know salinity of different water sources. For brackish
water (or sea water or industrial brine solution), it is an important parameter and indicates the
extent of desalting of apparatus required. It also interferes with COD determination and thus it
requires a correction to be made on the basis of amount present or else a complexing agent, such
as HgSO4 can be added. Further, chloride ions are used as tracer ions in column studies to model
fate of different contaminants in soil and liquid media.

Procedure: The Mohr Method uses silver nitrate for titration (normality: 0.0141) (method
applicability: 0.15 to 10 mg/L chloride ions). This corresponds to 1 mL of 0.0141 equals to 1 mg
chloride in solution. The silver nitrate solution is standardized against standard chloride solution,
prepared from sodium chloride (NaCl). During the titration, chloride ion is precipitated as white
silver chloride (Eq.1): Ag+ +Cl<=>AgCl (Solubility product constant, Ksp=3×10-10) (1) the
indicator (potassium chromate) is added to visualize the endpoint, demonstrating presence of
excess silver ions. In the presence of excess silver ions, solubility product of silver chromate
exceeded and it forms a reddish-brown precipitate (Eq.2). This stage is taken as evidence that all
chloride ions have been consumed and only excess silver ions have reacted with chromate ions:
2Ag+ +CrO42-<=> Ag2CrO4 (Ksp=5×10-12) (1)

Apparatus: Burette, conical flask, pipette, measuring cylinder Reagents: Potassium chromate
indicator solution, standard silver nitrate titrant. 19 Steps:

1. Take 25 ml sample in a conical flask. Measure sample pH.

2. Add 1.0ml indicator solution,

3. Titrate with standard silver nitrate solution to pinkish yellow end point and note down volume
of titrant used. Also measure sample pH.

4. Calculate chloride ion concentration using

Eq.(3): Chloride Ion Concentration (mg/L) = (A×N ×35.45)*1000 / V sample (3) Where: A =
volume of titrant used, N is normality of silver nitrate (here we used N/71 or 0.0141 N), and
Vsample is volume of sample used (mL).

Result- The concentration of Chloride ion in Given Water Sample is _____________mg/L

.
 Experiment 3

Aim: Determination of Dissolved oxygen

Theory

All gases of the atmosphere are soluble in water to some degree. Oxygen is classified as poorly
soluble, and its solubility is affected both by atmospheric pressure, and physical and chemical
properties of water such as temperature, salinity, pollutants, etc. The solubility of atmospheric
oxygen in fresh waters ranges from 14.6 mg/L at 0o C to about 7 mg/L at 35o C under 1 atm. of
pressure. Most of the critical conditions related to dissolved-oxygen deficiency, both in natural
waters and biological wastewater treatment, occur during the warmer months when temperatures
are high and solubility of oxygen is at a minimum. The low solubility of oxygen is a major factor
limiting the purification capacity of natural waters. In aerobic biological treatment processes, the
limited solubility of oxygen is also of great importance, because it governs the rate at which
oxygen will be absorbed by the medium and therefore the cost of aeration. Hence, DO analysis is
a key test both in natural waters and water pollution control practice.

Equipment

The use of DO probes or electrodes which allow in-situ measurements to be made has become
standard practice in recent years. They are especially useful for taking DO profiles of reservoirs
and streams, for monitoring DO levels in aerobic biological wastewater treatment processes, and
for conducting BOD analyses. An inert metal such as gold or platinum serves as the cathode, and
silver is used for the anode. These are electrically connected with a potassium chloride solution,
and the cell is separated from the sample by means of a gas-permeable membrane, usually
polyethylene. The membrane shields the cathode and anode from contamination by interfering
liquids and solids. When a potential of about 0.5 to 0.8 volt is applied across the anode and
cathode, any oxygen which passes through the membrane will be reduced at the cathode, causing
a current to flow. The magnitude of the current produced is proportional to the amount of oxygen
in the sample. Dissolved-oxygen electrodes are very sensitive to temperature, and thus either
temperature measurements must be made along with dissolved-oxygen measurements so that a
correction can be applied, or else instruments which are equipped with a thermistor or other
device to compensate automatically for temperature changes must be used.

Procedure

Dissolved oxygen measurements using DO probe (i) Remove glass stopper of the BOD bottle,
and place DO probe into the sample. (ii) Switch on the stirrer of the DO probe. (iii) Read the DO
value in mg/L when the meter reading has stabilized.

Result

Sr. NO Source of Sample DO[mg/L]

 Experiment no. 4

AIM: To Determine the Alkalinity in a Given Water Sample

Theory: Alkalinity is a measure of the capability of water to absorb H+ ions without significant
change of pH. In other words, alkalinity is a measure of the acid buffering capacity of water. The
determination of alkalinity of water is necessary for controlling the corrosion, to calculate the
amount of lime and soda needed for water softening; in conditioning the boiler feed water, etc.
Alkalinity of a sample of water is due to the presence of OH – (hydroxide ion), HCO3–
(bicarbonate ion) and CO32–(carbonate ion) or the mixture of two ions present in water. The
possibility of OH– and HCO3 – ions together is not possible since they combine together to form
CO32–ions. The alkalinity due to different ions can be estimated separately by titration against
standard acid solution, using selective indicators like phenolphthalein and methyl orange.

1) OH– + H+H2O
ii) CO32– + H+HCO3–
iii) HCO3 – + H+ H2O + CO2
The neutralization reaction upto phenolphthalein end point shows the completion of
reactions (i) and (ii) (OH– and CO32–) and (CO3 2– and HCO3–) only. The amount of acid
used thus corresponds to complete neutralization of OH– plus half neutralization of CO32–
The titration of water sample using methyl orange indicator marks the completion of the
reactions (i), (ii) and (iii). The amount of acid used after phenolphthalein end point
corresponds to one half of normal carbonate and all the bicarbonates. Total amount of
acid used represent the total alkalinity due to all ions present in water sample. Apparatus:
Burette, pipette, conical flask, beakers, burette stand and clamp Chemicals: Dry Na2CO3,
concentrated 12(N) HCl, phenolphthalein and methyl orange indicator

Procedure: 1. Primary standard solution of Na2CO3 (0.1N) is provided.

2. Secondary standard solution of HCl and the water sample are provided.

3. Standardization of HCl solution by primary standard Na2CO3 solution– Pipette out 10 mL of

Na2CO3 solution in a conical flask, add 2 drops of methyl orange indicator, fill up the burette
with (N/10) HCl solution and titrate till the color of the solution changes from yellow to red.

4. Analysis of water sample i) Pipette 20 mL of the sample of water into a 100 mL conical flask
and 2 drops of phenolphthalein indicator was added and titrated against (N/10) HCl till the color
of the solution changes from pink to colorless. Corresponding burette reading indicates the
phenolphthalein end point (V1). ii) Again pipette out 20 mL of the water sample in a conical
flask, add 2 drops of methyl orange indicator. Color of the solution becomes yellow. Continue
the titration against the (N/10) HCl solution till the color changes to red. This burette reading
corresponds to the methyl orange end point (V2).

Observations and Calculations Table 1:- Standardization of HCl solution Strength of Na2CO3 solution (S1)
= 0.1(N)

Sr. No Vol. Of Burette Reading(Ml) Vol. Of HCl Mean

Na2CO3(V1)ml Required Volume of
HCl(V2)

1 10 Initial Final

2 10

3 10

Let, the strength of HCl = S2 As we know, V1S1=V2S2  S2=(V1S1/V2) (N)

Table 2:- Analysis of water using phenolphthalein indicator Strength of HCl solution (S2) = ____ (N)

Sr. No Vol. Of Water Burette Reading(Ml) Vol. Of HCl Mean Volume

Sample Required of
(V1)ml HCl(V4)mL

1 20 Initial Final

2 20
3 20

20 x S3 = V4 x S2 where S3 is the phenolphthalein alkalinity in water sample  S3 = (V4 x

S2 )/ 20

 Strength in terms of CaCO3 equivalent = S3 x Eq. Wt of CaCO3 = (V4S2 / 20) x 50 g/L = A

(say) g/L

 Phenolphthalein alkalinity (P) = A x 1000 mg/L

Table 3:- Analysis of water using methyl orange indicator

Sr. No Vol. Of Water Burette Reading(Ml) Vol. Of HCl Mean Volume

Sample Required of
(V1)ml HCl(V5)mL

1 20 Initial Final

2 20

3 20

 20 x S4 = V5 x S2 where, S4 is the methyl orange alkalinity in water sample S4 = (V5S2/20)

Strength in terms of CaCO3 equivalent = S4 x Eq. Wt. of CaCO3 = (V5S2/20) x 50 g/L = B

(say) g/L

 Methyl orange alkalinity (M) = B x 1000 mg/L

Discussions: i) Phenolphthalein alkalinity (P) = 0; that means the volume of acid used till the
completion of reaction (i) and (ii) is 0. This can only happen when both OH– and CO 32–ions are
not present in water. Alkalinity is present due to HCO 3– ion only which can be determined using
methyl orange indicator and called methyl orange alkalinity (M). ii) P = ½ M; indicates that only
CO32–ions are present. Using phenolphthalein indicator neutralization reaches uptoHCO3– but
using methyl orange indicator the complete neutralization of HCO3– takes place. iii) P > ½M;
implies OH– ions are also present along with CO 32–ions. Upto phenolphthalein alkalinity OH–
ions will be neutralized completely whereasCO32–will be neutralized uptoHCO3– ion. But using
methyl orange indicator HCO3– will be completely neutralized along with OH– and CO 32–. iv) P
< ½ M; indicates that beside CO32–ions HCO3– ions are also present. The volume of acid required
for the neutralization upto phenolphthalein end point correspond half neutralization of CO32–
(equation ii). Neutralization using methyl orange indicator corresponds to HCO3–obtained from
CO32–and HCO3– originally present in the water sample. v) P = M; indicates only OH– ions are
present.
 Experiment- 5

Aim- Measurement of Noise level

Procedure

Note: Make the measurements suggested below using A weighting and then C weighting. Record
all the data indicated by the Table headings below, including Source of Sound, Estimated
Distance from Meters, dB (A weighting), dB (C weighting), and your subjective judgments of
the loudness of the sounds (such as “very quiet”, “medium”, “loud”, “very loud”, etc.). Please
cover your ears for all sounds which could be potentially damaging.

Report: 1) Measure and record the sound pressure level (SPL) produced by the background
noise in the lab, along with the other data requested in the Table.

2) Measure and record the SPL produced when your lab partner screams at you as loudly as he or
she can. Try two or three difference distances from the sound level meter, e.g., 5 ft., 10 ft. and 15
ft. Note to the screamer: Do not scream so loudly that you damage your vocal folds! Note to the
listener: Cover your ears!

3) Measure and record the SPL produced when your lab partner speaks to you in a normal
fashion.

4) Measure and record the SPL produced by singing or playing various musical instruments (if
they are available) for two or three different distances from the sound level meter.

5) Have your partner try to sing (or play a musical instrument) a few notes in a scale (within an
octave) at what he or she considers to be the same loudness and record the actual sound levels
produced when this is attempted. (a) How large a variation typically occurs in the SPL from one
note to the next?

6) If anyone has a car parked nearby, it would be interesting to measure the SPL produced by
honking the horn, first when the sound level meter is relatively close to the horn, and then when
the meter is several feet away from the car.

7) Whistle as loudly as you can and measure the SPL (cover your ears).
8) Record the SPL in a place which you consider to be very quiet (possibly a room next door
where no one is present).

9) Turn up the volume of a stereo sound system (one will be set up in the lab) and record the SPL
produced under various conditions of your choice.

10) Measure the sound pressure levels produced by anything else which intrigues you. Use your
imagination, but keep in mind that you may look a bit suspicious walking around with a strange
instrument !!!!!Musical!Acoustics!Lab,!C.!Bertulani 4 taking readings now and then.

11) In general, what differences do you find between your measurements made with A and C
weighting? 12) Why do such differences exist? 13) Based upon the observations you have made
during this experiment, what types of situations have exposed your ears to the highest sound
levels during your life?

14) Do you think any of these situations were hazardous based upon the Table of Permissible
Noise Exposures?

Source of Sound Estimated SPL (dB) A SPL (dB) C Comments on

Distance from weighting weighting Subjective
Meter Loudness

Experiment No 6
 Aim
To determine the optimum coagulant dosage for clarifying the given sample of water by using
alum as the coagulant and performing the jar test experiment.

Principle
Coagulants are used in water treatment plants
to remove natural suspended and colloidal matter,
to remove material which do not settle in plain sedimentation, and

to assist in filtration.
Alum [Al2S(SO4)3. 18H2O] is the most widely used coagulant. When alum solution is added to
water, the molecules dissociate to yield SO 42- and Al3+. The +ve species combine with negatively
charged colloidal to neutralise part of the charge on the colloidal particle. Thus, agglomeration takes
place. Coagulation is a quite complex phenomenon and the coagulant should be distributed uniformly
throughout the solution. A flash mix accomplishes this.

Jar test is simple device used to determine this optimum coagulant dose required. The jar test,
device consists of a number of stirrers (4 to 6) provided with paddles. The paddles can be rotated
with varying speed with the help of a motor and regulator. Samples will be taken in jars or
beakers and varying dose of coagulant will be added simultaneously to all the jars. The paddles
will be rotated at 100 rpm for 1 minute and at 40 rpm for 20 to 30 minutes, corresponding to the
flash mixing and slow mixing in the flocculator of the treatment plant. After 30 minutes settling,
supernatant will be taken carefully from all the jars to measure turbidity. The dose, which gives
the least turbidity, is taken as the optimum coagulant dose.

Apparatus
1. Jar test apparatus
2. Glass beakers
3. Pipette
4. Nephelometer
5. pH meter

Reagents
1. Alum solution (1mL containing 10 mg of alum)
2. Lime
3. Acid/alkali

Procedure
1. Take 1-litre beakers and fill them with sample up to the mark.
2. Keep each beaker below each paddle and lower the paddles, such that each one is about
1cm above the bottom.
3. Find the pH of the sample and adjust it to 6 to 8.5.
4. Pipette 1, 2, 3, 4, 5, 6 mL of the alum solution into the test samples.
5. Immediately run the paddles at 100 rpm for 1 minute.
6. Reduce the speed to 30-40 rpm and run at this rate for 30 minutes.
7. Stop the machine, lift out the paddles and allow to settle for 30 minutes.
8. Find the residual turbidity of the supernatant using nephelometer.
9. Plot a graph with alum dosage along x-axis and turbidity along y-axis.
10. The dosage of alum, which represents least turbidity, gives Optimum Coagulant Dosage
(O.C.D.).
11. Repeat steps 1-10 with higher dose of alum, if necessary.

Observation

Result
Optimum coagulant dosage = ..........