Environmental Engg Lab

LABORATORY MANUAL
ENVIRONMENTAL ENGINEERING
(BACHELOR OF TECHNOLOGY)
PREPARED BY
Mr. SHIVA SHANKAR Y (ASSISTANT PROFESSOR)
Mr. M.L. RATHORE (LAB ENGINEER)
DEPARTMENT OF CIVIL ENGINEERING
JAYPEE UNIVERSITY OF
ENGINEERING & TECHNOLOGY
A.B. ROAD RAGHOGARH-GUNA (M.P.)-473226 (INDIA)
Department of Civil Engineering, JUET Guna (M.P.): 1

DEPARTMENT OF CIVIL ENGINEERING, JUET
ENVIRONMENTAL ENGINEERING LAB
(COURSE CODE: 16B17CE471)
CONTENTS
Ex No Experiment Name Page No
1 pH, Turbidity, Electrical Conductivity 3–9

2 Acidity and Alkalinity 10– 13
3 Chlorides and Fluorides 14 – 16
4 Total Hardness, Calcium and Magnesium 17 – 19
5 Solids (total, suspended and dissolved) 20 – 25
6 Settleable solids (by Imhoff Cone) 26 – 27
7 Optimum coagulant dose (Jar Test) 28 – 29
8 Chlorine demand and Residual chlorine 30 – 31
9 Dissolved oxygen 32 – 34
10 Biochemical oxygen demand 35 – 37
11 Chemical oxygen demand (COD) 38 – 39
12 Gas liquid mass transfer characteristics (aeration apparatus) 40 – 43
13 Softening or demineralization of water (ion exchange 44 – 45
column)
14 Most probable number (MPN) 46 – 48
Demonstration Type Experiments
15 High volume sampler device (SPM, RPM, SO2 and NO2) 49 – 65
16 Batch sedimentation apparatus 66 – 67
17 Deep bed filtration set-up 68 – 71
-- References 72

EXPERIMENT NO.: 1(a)
NAME OF EXPERIMENT: pH
Aim: To determine pH of the given water samples.
Theory:
pH value denotes hydrogen ion concentration in the liquid and it is the measure of acidity or
alkalinity of the liquid. According to the law of mass action, in any liquid
Conc. of H ions × Conc. of OH ions/ Conc. of un-dissolved HOH molecules
= constant = 10-14
For convenience pH scale is taken from 0 to 14.
Principle:
pH of a liquid sample can be determined either by:
(i) Coloumetric method or use of indicators (ii) Electrometric method
Electrometric method of pH determination:
It is determined through a instrument by electrolysis and dissociation of H+ and OH- radical,

and the milivolts generated give on scale either by movement of analog pointer or digital
recording. Knowing pH value is a very important parameter for the analysis of wastewater and
its treatment. Certain chemicals and biological processes work only at a particular pH.
Apparatus:
1. pH-strips (papers),
2. pH meter,
3. thermometer
Reagents:
1) Distilled water
2) Standard buffer solutions: Standard buffer solutions having pH values of 4.0 and 9.2 are
readily available. Otherwise, they can be prepared easily by dissolving 1 pH tablet of
each buffer in distilled water and make up to 100 ml gives a standard solution of pH 4.0
and 9.2.

Procedure:
The pH of water can be found in the following manner.
1. Using pH-paper:
(i) Dip a wide-range (0-14) pH-strip (paper) into the solution whose pH to be found. The
color of the litmus paper changes to thick red for highly acidic waters to dark green for
highly alkaline waters and to any other color depending on the pH of the solution.
Compare the color of paper with the standard colours supplied. Note down the pH by
noting down the number corresponding to the matching color.
(ii) Select a suitable narrow-range pH-strip and compare the color by using the same
method with wide-range pH-strips. Note down the pH by comparing the changed color
with standard colours. Narrow-range pH-strips are normally available in the following
pH ranges: 2 to 4.5; 4 to 6.5; 6 to 9.5; 8.5 to 10.5; 10 to 12.
2. Using pH-meter:
(i) Switch on the pH meter for 15 minutes.
(ii) After washing and wiping the pH electrode and the temperature probe dip it in a
solution of pH 4.0 buffer. Change knob from standby to pH.
(iii) With the CAL knob set the pH value to 4.0
(iv) With a pH 9.2 buffer, set the pH value to 9.2 using the SLOPE knob.
(v) Repeat steps 2-3 till the pH meter is standardized with respect to both pH 4.0 and 9.2
(vi)Take the pH values of the different water samples with the pH meter.
SIGNIFICANCE:
1. Knowing pH value is very important parameter for analysis of water/wastewater and

its treatment, its suitability for domestic use and for irrigation. Certain chemical and
biological processes work only at a particular pH. pH of 6.5 to 8.5 has no direct
adverse effect on health. However a lower value below will produce sour taste and
higher value above 8.5 a bitter taste. Higher value of pH encourages the scale
formation in water heating systems and also reduces the germicidal potential of
chlorine. High pH induces the formation of tri-halo-methanes which are causing
cancer in human beings. According to BIS, water for domestic consumption should
have a pH between 6.5- 8.5.
2. Corrosion of water mains is the main the main problem associated with acidic
waters. Acidic/alkaline waters cannot be used for construction purposes also. If pH is
less, algae die, fish cannot reproduce and it causes acidity, corrosion, irritation of
mucous membranes, tuberculosis and other health problems in humans.
Observation Table:

S. Description of sample pH value
No. pH paper pH meter
Wide range Narrow range
Results and Conclusions:
Precautions:
EXPERIMENT NO.: 1(b)

NAME OF EXPERIMENT: TURBIDITY
Aim: To find out Turbidity of the given sample.
Principle:
When light is passed through a sample having suspended particles some of the light is scattered
by the particles. The scattering of the light is generally proportional to the turbidity. The
turbidity of sample is thus measured from the amount of light scattered by the sample taking a
reference with standard turbidity suspension.
Apparatus
1. Nephelometric Turbidity meter

2. Sample tubes
Reagents:
1. Dissolve 1 g of Hydrazine sulphate and dilute to 100 ml

2. Dissolve 10 g Hexametehylene Tetra amine and dilute to 100 ml
3. Mix 5 ml of each of the above solution (1 and 2) in a 100 ml volumetric flask and allow
standing for 24 hours at 25 ± 3°C and diluting to 1000 ml. This solution has a turbidity of
40 NTU.
4. This solution can be kept for about a month
Procedure:
1. Switch on Nephelometeric turbidity meter and wait for few minutes till it warms up.
2. 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.
3. Shake thoroughly the sample and keep it for sometime to eliminate the air bubbles.
4. Take sample in Nephelometer sample tube and put the sample in sample chamber and
find out the value on the scale.
5. Dilute the sample with turbidity free water and again read the turbidity.
Environmental significance:
1. Turbidity is objectionable because of aesthetic and engineering considerations. The
colloidal material exerts turbidity provides adsorption sites for chemical that may be
harmful. In natural waters, turbidity may impart a brown or other color to water and be

harmful. In natural waters, turbidity may impart a brown or other color to water and
may interfere with light penetration and photosynthetic reaction in streams and lakes.
2. Slow sand filters cannot function if raw water has excess turbidity. A rapid sand filter
may go out of function, if excess turbidity exists.
3. Knowing about turbidity variation in raw water supplies is useful to determine whether
a supply requires special treatment by chemical coagulation and filtration before it may
be used for a public water supply or not.
4. Turbidity measurement is used to find the efficiency of the treatment produced with
different chemicals and the dosages needed.
5. Turbidity measurement helps to gauge the amount of chemicals needed from day to
day in the treatment processes.
6. Turbidity measurements of the filtered water are needed to check the faulty filter
operation.
7. Measurement of turbidity in settled water prior to filtration is useful in controlling
chemical dosages so as to prevent excessive loading of repaid sand filters.
8. Often treated municipal waters also are found to contain excess turbidity. This may be
due to adding bleaching powder containing lot of impurities like clay or vacuum
prevailing in the water mains during the non-supply hours, that may suck the stagnated
(polluted) surface waters. As turbidity acts as a shield to protect the microorganisms,
bacterial population is found to be more in turbid waters.
Observation Table:
Sl No. Sample details Turbidity (NTU) Remarks
Precautions:

EXPERIMENT NO.: 1(c)
NAME OF EXPERIMENT: ELECTRICAL CONDUCTIVITY
Aim:
To determine the Conductivity of the given water samples.
Principle:
The electrical conductivity is a total parameter for dissolved, dissociated substances. Its value
depends on the concentration and degrees of dissociation of the ions as well as the
temperature and migration velocity of the ions in the electric field.
Apparatus: Conductivity Meter, Beakers, Thermometer.
Reagents: 0.1N KCl
Procedure:
1. Switch on the conductivity meter for 15 minutes.

2. Take out the conductivity cell dipped in distilled water, wash it with distilled water and
wipe it dry with a tissue paper.
3. Calibrate the cell with standard 0.1N KCl solution of conductivity 14.12 mmhos at 30°C.
4. Take out the conductivity cell, wash it thoroughly with distilled water and wipe it dry.
5. Dip the cell into the sample solution, swirl the solution and wait upto 1 minute for a
steady reading.
6. Note down the instrument reading and also temperature by a thermometer.
Significance:
1. Dissolved minerals, gases and organics may produce aesthetically displeasing colours,
taste and odours to water.
2. EC measurements are the basis to evaluate the performance of the processes of
desalination, demineralization, distillation and many process plants.
3. salinity and total dissolved solids can be estimated very quickly from conductivity.
4. If conductivity of a water sample is more than 2000µmhos/cm i.e. if TDS exceeds 2100
mg/1, it cannot be disposed off without treatment.
5. If TDS is more, water cannot be used for drinking as well as construction purposes. TDS
affects strength and solidity of concrete and palatability of food cooked. It also causes
gastro intestinal irritation.

Observation table:
S.No. Description of Temperature Conductivity Remarks

sample (mmhos)
1
2
3
4
5
Precautions:
1. The electrode must be dipped into the sample carefully lest it is broken.
2. If the ECL falls outside the range of the instrument, dilute the sample, with distilled
water and then estimate the EC.
3. Keep the electrode immersed in distilled water always and at the end of each
measurement wash it thoroughly with distilled water. Organic material coating, if any,
can be removed with alcohol or acetone followed by distilled water.

NAME OF EXPERIMENT: ACIDITY
Aim:
To determine acidity (base capacity) of the given water samples.
Principle:
The mineral acids present in the sample which are contributing mineral acidity can be
calculated by titrating or neutralizing samples with strong base NaOH to pH 4.3. The CO2 and
bicarbonates (carbonic acid) present and contribute CO2 acidity in the sample can be
neutralized completely by continuing the titration to p H 8.2
Apparatus:
1. Burette,
2. pipettes,
3. conical flask.
Reagent Required:
1. Standard sodium hydroxide (0.02N).

2. phenolphthalein indicator
3. Methyl orange indicator
4. Sodium thiosulfate (0.1N)
5. Carbon dioxide free distilled water.
Procedure:
1. Pipette out 100 ml of the given water sample into a conical flask.
2. Add 1 drop of 0.1N sodium thiosulfate solution to destroy any residual chlorine.
3. Add 2 drops of methyl orange indicator. The sample turns pink.
4. Titrate against 0.02N standard sodium hydroxide solution until pink color changes to
yellow.
5. Note down the volume of the NaOH added (V1).
6. Take another conical flask containing 100 ml of water sample, add 2 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 especially water softening.

2. It corrodes pipes.
3. Aquatic life will be affected.
4. Acidity present due to free CO 2 has no significance from public health view point.
However, waters containing mineral acidity (acidity due to H2SO4, HCL and HNO3) are
unacceptable.
5. Waters having an acidity of more than 50 mg/I cannot be used in R.C.C. works
Observation table:
Sl. Sample Sample Methyl Orange Indicator Phenolphthalein indicator

No details Volume Initial Final NaOH Mineral Initial Final NaOH CO2
(ml) Burette Burette Used Acidity Burette Burette Used Acidity
Reading reading (ml) (mg/l) Reading Reading (ml) (mg/l)
(ml) (ml) (ml) (ml)
Model Calculations:
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) = V2 X 1000/ml. of sample taken
Total acidity (as CaCO3) = Mineral acidity + CO2 acidity.
Results and conclusions:
Precautions:
1. Cleaned apparatus & glassware should be used for the preparation.
2. All the reagents should be prepared freshly and standardized.
3. To avoid loss of CO2, titration should be carried out quickly & vigorous shaking should be
avoided.

EXPERIMENT NO.: - 2(b)
NAME OF EXPERIMENT: ALKALINITY
Aim: To determine the Alkalinity of the given water samples.

Principle:
Alkalinity can be obtained by neutralizing OH-, CO3--- and HCO3- with standard H2SO4. Titration
to pH 8.3 or decolourization of phenolphthalein indicator will show complete neutralization of
OH- and ½ of CO3--, while to pH 4.4 or sharp change from yellow to pink of methyl orange
indicator will indicate total alkalinity i.e. OH-, CO3---, and HCO3-.
Apparatus:
1. Burette 2. Pipettes 3. Conical flask
Reagents:
1. Standard sulphuric acid (0.02 N)

2. Phenolphthalein indicator
3. Methyl Orange indicator
4. Carbon dioxide free distilled water
5. Sodium thiosulfate (0.1 N) (Optional)
Procedure:
1. Take 100 ml of the given water sample in a conical flask.

2. Add one drop of 0.1 N sodium thiosulfate solutions to remove the free residual chlorine
if present.
3. Add 2 drops of phenolphthalein indicator. The sample turns pink.
4. Run down 0.02 N standard sulphuric acid till the solution turns to colorless.
5. Note down the volume of H2SO4 added (V1).
6. Add 2 drops of methyl orange indicator the sample turns to yellow.
7. Resume titration till the color of the solution turns to pink.
8. Note down the total volume of H2SO4 added (V2).
Significance:
1. Highly alkaline water are usually unpalatable and consumer acceptance decreases.
Water having an alkalinity of less than 200 mg/l as CaCO3 is desirable for drinking.
2. Large amount of alkalinity imparts a bitter taste to water.

Observation table:
Serial Sample Sample Phenolphthalein indicator Methyl Orange Indicator

No. details Volume Initial Final H2SO4 Initial Final H2SO4
Burette Burette Used Burette Burette Used
Reading reading Reading Reading
(ml) (ml) (ml) (ml) (ml) (ml) (ml)
Value of P and T Alkalinity (mg/l) as CaCO3 due to

-
OH CO3-- HCO3-
P=0 0 0 T
P<T/2 0 2P T-2P
P=T/2 0 2P 0
P>T/2 2P-T 2T-2P 0
P=T T 0 0
Model Calculation:
1. Phenolphthalein alkalinity (P) (mg/l) as CaCO3

= V1 X normality of H2SO4X 1000X50/ Volume of sample taken
2. Total alkalinity (T) (mg/l) as CaCO3

= V2 X normality of H2SO4X 1000X50/ Volume of sample taken

Sample P T Alkalinity (mg/l) as CaCO3 due to
details OH- CO3-- HCO3-
Precautions:
1. The glass apparatus should be perfectly cleaned before the start of the experiment.
2. Since phenolphthalein and methyl orange indicators are used in determination of
alkalinity the end point of the titration should be observed carefully.
NAME OF EXPERIMENT : CHLORIDES
Aim:
To estimate the content of chlorides in the given water samples.
Principle:
The Mohr method for the determination of chloride in water is based upon the fact that in
solution containing chloride and chromate, silver reacts with all the chloride and precipitates
before the reaction with chromate begins. The appearance of the brick-red colour of the silver
chromate precipitate is the end-point of the titration.
Apparatus:
Burette, pipette and conical flask.
Reagents:
1. Chloride free distilled water.
2. Potassium chromate (K2CrO4) colour indicator
3. Standard silver nitrate solution (0.0141 N)
4. Standard sodium chloride solution (0.0141 N)
Procedure:
1. Take 100 ml of sample in conical flask.

2. Adjust the pH between 7.0 and 8.0 either with sulphuric acid or sodium hydroxide solution.
3. Add 1 ml of potassium chromate indicator to get light yellow colour.
4. Titrate with standard silver nitrate solution till the colour changes from yellow to brick-red.
5. Note the volume of silver nitrate added (A).
6. For better accuracy, titrate 100 ml of distilled water in the same way after adding 1 ml of
potassium chromate indicator to establish reagent blank.
7. Note the volume of silver nitrate added for distilled water (B).

Significance:
1. Analysis of a water sample is necessary to know whether the sample may be considered as
suitable for drinking, construction, hydro-testing and some industrial process or not.
2. Water containing chloride in excess of 250 mg/l is considered to be undesirable for drinking
purposes.
3. Chlorides are also corrosive and impart permanent hardness to water. Waters with chloride
in excess of 2000 mg/l are not recommended for many construction purposes also.
Observation table:
S. Sample details Volume of Observations Chlorides

NO. sample taken (mg/l)
(ml) Initial Final AgNO3
burette burette solution
reading reading used
(ml) (ml) (ml)
1.
2.
3.
Model Calculations:
Chlorides in (mg/l) = (A-B) X normality of AgNO3 X 35.46 X 1000/Volume of sample taken
Where
A = ml of AgNO3 required for sample
B = ml of AgNO3 required for blank
Precautions:
1. The whole apparatus should be washed with distilled water before the start of the
experiment.
2. The reaction mixture should be briskly shaken during the titration.
3. The end point of the reaction should be carefully observed.
4. The volume of the indicator should be same in all the titrations.
5. The pH of the sample should be adjusted to 7-8 range by adding acidic/basic solution to
the sample solution.

EXPERIMENT NO.: 3 (b)
NAME OF EXPERIMENT : FLUORIDE
Aim:
To determine the fluoride in the given water sample.
Principle:
The test is based on the fact that fluoride ion combines with zirconium ion to form a stable
complex ion, ZrF6 and this results in bleaching the reddish colour of zirconium and alizarin
combination. The decrease in intensity of colour is directly proportional to Fluoride
concentration.
Apparatus: Nessler tubes, 100 ml.
Reagents:
1. Standard sodium fluoride solution

2. Zirconium alizarin solution
3. Mixed acid solution
4. Acid zirconium alizarin reagent
5. Sodium thiosulphate solution
Procedure:
1. The sample should be free from chlorine, if chlorine present, it shall be dechlorinated
with a slight excess of sodium thiosulphate solution before use.
2. Take 0, 1, 2, 6, 8, 14 ml of standard sodium fluoride solution in six Nessler tubes.
3. Add 5 ml of acid zirconium reagent in each Nessler tube.
4. Similarly add 5 ml of acid zirconium reagent into the Nessler tubes containing 100 ml of
sample.
5. Mix thoroughly and compare the colours after standing for one hour exactly.
Significance:
1. During the formation of permanent teeth, fluoride combines with enamel of the teeth to
form strong, hard and durable teeth. As such many municipal water supplies are
supplemented with fluoride by addition of fluoride compounds. If fluoride is more than
1.5 mg/I it leads to discoloration of teeth called ‘’mottling’’. The white patches formed
later become yellow and turn brown or black. Fluoride in excess of 5 ppm, causes bone
Fluorosis and skeletal abnormalities.
2 Fluoride of water is an important in determining the suitability of water for domestic
and industrial use.
3. The size and design of defluoridation units depend on the level of fluoride present in
water. Excess Fluoride can be removed by defluoridation with activated charcoal or
Nalgonda technic using alum and lime.

Fluorides in given sample (mg/l) =………….

EXPERIMENT NO.: 4
NAME OF EXPERIMENT : HARDNESS
Aim:
To determine the total hardness, calcium and magnesium of the given water sample.
Theory:
Hardness in water is defined as soap consuming capacity of water. This is mainly due to
presence of calcium and magnesium ions in water. The hardness of water is taken as a measure
of Ca++ and Mg++ contents. The hardness is temporary and permanent. When water is boiled,
bicarbonates are decomposed to form carbonate ions and CO2 is driven off. Thus total hardness
is eliminated. The permanent hardness is not removed by boiling.
Hardness is total hardness of water which is determined by complex metric method using
EDTA. EDTA forms a complex with Ca++ and Mg++. The complexes exist at pH 8 to 10. The indicator
used is Eriochrome Black T. The color change with Eriochrome Black T is in the presence of Mg ++.
If Mg++ ions are not present in solution, they must be added.
Apparatus: Burette, Pipette, Conical flask and Beaker.
Reagents:
1. Buffer solution
2. Standard EDTA Solution 0.01 M
3. Eriochrome Black T indicator
4. Standard calcium solution
5. Murexide indicator
6. Sodium Hydroxide 2N
Procedure:
A. Total hardness:
(i) Take 100 ml of given water sample in a conical flask.
(ii) Add 2 ml of buffer solution.
(iii) Add 2 drops of Eriochrome Black T indicator. The color becomes wine red.
(iv) Titrate with standard EDTA solution till the color changes to blue.
(v) Note down the volume of EDTA solution used (A) ml.
(vi) Run a reagent blank if buffer is not checked properly. Note the volume of EDTA
required for blank (B) ml.
Calculations:
(A - B) x 1000
Total Hardness (mg/l) as CaCO3 = ----------------
ml of sample

B. Calcium hardness:
i. Take 25 ml of sample in conical flask.

ii. Add I ml NaOH to raise pH to 12 and a pinch of murexide indicator.
iii. Titrate with EDTA till pink colour changes to purple. Note the volume of EDTA used (A1).
Calculations:
A1 x 1000
Calcium Hardness (mg/l) as CaCO3 = ----------------
ml of sample
Where A1 = volume of EDTA used by sample.
C. Magnesium hardness:
Magnesium hardness = Total Hardness - Calcium Hardness
Significance:
1. Absolutely soft waters are tasteless (e.g. distilled water). On the other hand, hardness upto
600 mg/l can be relished if got acclimatized to.
2. Moderately hard water is preferred to soft water for drinking and irrigation purposes.
3. Hard waters form scales in hot water pipes and boilers.
4. Soft waters affects the human cardiovascular system and causes heart-attacks.
Observation and Results Table:
Sample details Vol. of Initial Final EDTA sol. Hardness

sample Burette burette Used
taken Reading reading (mg/l)
(ml) (ml) (ml) (ml)
Total
hardness
Calcium
hardness
Magnesium hardness

Precautions:
1. The glass wares namely burette, pipette, beakers should be rinsed only with the distilled
water.
2. All the solutions should be checked with care before used
3. Distilled water should be checked with care before use.
4. The same amount of indicator must be added each time.
5. The reaction mixture should be briskly shaken during the titration.
6. The end point should be observed carefully.
7. pH 10 should be maintained during the titration.

NAME OF EXPERIMENT : TOTAL SOLIDS
Aim:
To determine the total solids of the given water samples.
Principle:
Total solids are determined as the residue left after evaporation and drying of the unfiltered
sample.
Apparatus:
1. Evaporating dishes (Pyrex, porcelain or platinum)

2. Oven
3. Desiccators
4. Water bath
Procedure:
1. A clean porcelain dish is ignited in a muffle furnace and after partial cooling in the air; it is
cooled in a desiccator and weighed.
2. A 100 ml of well mixed sample (graduated cylinder is rinsed to ensure transfer of all
suspended matter) is placed in the dish and evaporated at 1000C on water bath, followed by
drying in oven at 1030C for 1 hour.
3. Dry to a constant weight at 1030C, cool in a desiccator and weigh.
Significance:
1. Total solids determination is used to assess the suitability of potential supply of water
for various uses.
2. The pH at stabilization depends on total solids also.
Observation Table
S. Sample details Volume of Initial wt. of Final weight Total solids

No. sample the dish of the dish (mg/l)
(ml) (mg) (mg)
1.
2.
3.
4.

Calculations:
(A-B) x 1000
Total solids (mg/l) = --------------------
V
A = Final weight of the dish in mg

B = Initial weight of the dish in mg
V = Volume of sample taken in ml
Total Solids (mg/l) = ………………………………..

NAME OF EXPERIMENT : TOTAL DISSOLVED SOLIDS
Aim:
To determine the total dissolved solids of the given water samples.
Principle:
Total dissolved solids are determined as the residue left after evaporation and drying of the
filtered sample.
Apparatus:
1. Evaporating dishes (Pyrex, porcelain or platinum)

2. Oven
3. Desiccators
4. Water bath
5. Whatman filter paper No. 44
Procedure:
1. A clean porcelain dish is ignited in a muffle furnace and after partial cooling in the air; it
is cooled in a desiccator and weighed.
2. A 100 ml of filtered sample is placed in the dish and evaporated at 100 0C on water bath,
followed by drying in oven at 1030C for 1 hour.
3. Dry to a constant weight at 1030C, cool in a desiccator and weigh.
Significance:
1. Many dissolved substances are undesirable in water. Dissolved minerals, gases and
organic constituents may produce aesthetically displeasing colour, taste and odour.
2. Estimation of total dissolved solids is useful to determine whether the water is suitable
for drinking purposes, agriculture and industrial processes or not.
3. High concentration of dissolved solids about 3000 mg/I may also produce distress in
livestock. In industries, the use of water with high amount to dissolved solids may lead
to scaling in boilers, corrosion and degraded quality of the product.
4. Water with higher solids content often has a laxative effect.
5. Refer to experiment on electrical conductivity (EC) also.

Observation Table
S. Sample details Volume of Initial wt. of Final weight Total

No. sample the dish of the dish dissolved
(ml) (mg) (mg) solids
(mg/l)
1.
2.
3.
4.
5.
6.
Calculations:
(A - B) x 1000
Total dissolved solids (mg/l) = --------------------
V
Where,
A = Final weight of the dish in mg
B = Initial weight of the dish in mg
V = Volume of sample taken in ml
Total Dissolved Solids (TDS) = ………………………… (mg/l)

EXPERIMENT NO.: 5 (c)
NAME OF EXPERIMENT : TOTAL SUSPENDED SOLIDS
Aim:
To determine the total suspended solids of the given water samples.
Principle:
Total suspended solids are determined as the residue left on gooch crucible or a glass fiber
after drying in oven.
Apparatus
1. Gooch crucible/glass fiber filter

2. Suction apparatus
3. Desiccator
Procedure :
1. A clean gooch crucible is ignited in a muffle furnace and after partial cooling in the air,
cool in a desiccator and weigh (W1).
2. Pour 100 ml of well mix sample on gooch crucible or glass fiber filter which is kept on
filter flask and apply suction.
3. Wash the gooch crucible with 100 ml of distilled water to remove all soluble salts.
4. Carefully remove the glass fiber filter paper or gooch crucible and dry in an oven at
1050C for one hour.
5. Cool in a desiccator and weigh (W2).
6. Ignite gooch crucible in a muffle furnace at 6000C for 15-20 minutes.
7. Cool the crucible partially in air until most of heat has been dissipated and then in a
dessicator and record final weigh (W3).
Significance:
1. Suspended solids may be objectionable in water for several reasons. It is aesthetically
displeasing and provides adsorption sites for chemical and biological agents.
2. Suspended organic solids which are degraded anaerobically may release obnoxious
odours.
3. Biologically active (live) suspended solids may include disease causing organisms.
4. The suspended solids parameter is used to measure the quality of wastewater Influent
and effluent and is useful in the analysis of polluted water.

Observation Table:
S. Sample details Volume of Initial wt. of Final weight solids

No. sample the dish of the dish (mg/l)
(ml) (mg) (mg)
1. Total suspended
2. solids
3.
1. Volatile suspended
2. solids
3.
Calculations:
(W2-W1) x 1000
Total suspended solids (mg/l) = -----------------------
ml of sample taken
(W2-W3) x 1000
Suspended volatile solids (mg/l) = ------------------------
ml of sample taken
Alternative:
Total suspended solids, mg/l = [Total solids, mg/l - Total dissolved solids] mg/l

EXPERIMENT NO.: 6
NAME OF EXPERIMENT: TOTAL SETTLEABLE SOLIDS
Aim:
To find out total settleable solids in the given water sample.
Principle:
The particles in suspension whose specific gravity greater than that of water will settle under
quiescent conditions.
Apparatus:
1. Imhoff cone
2. Holding device
Procedure:
1. Gently fill the imhoff cone with the thoroughly well mixed sample usually one liter and
allow it to settle.
2. After 45 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 ahs settled in the apex.
5. Express the results in ml settleable solids per liter of sample per hour (ml/l/hour).
Significance:
1. Determination of settleable solids is used extensively in the analysis of industrial waste

to determine the need for and design of plain settling tanks and in plants employing
biological treatment processes.
2. It is also used in wastewater treatment plant operation to determine the efficiency of
sedimentation units.
Observation and Results:
S. Sample details Volume of sample taken Total settleable

No. (ml) solids (ml/l/hour)
1.
2.
3.
4.
5.

Calculations:
ml of solids x 1000
Total settleable solids (ml/l) = ---------------------------
ml of sample
Results and Discussion:
Total settleable solids (ml/l/h) =
Precautions:
1. The imhoff cones must be cleaned with a strong soap and hot water using a brush.
2. Wetting the cone with water before use, helps in preventing adherence of the solids to
the sides.
3. The method is subjected to considerable in accuracy if the solids contain large
fragments.
4. The determination of total settleable solids should be carried out soon after sampling in
order to avoid errors through flocculation.

EXPERIMENT NO.: 7
NAME OF EXPERIMENT : JAR TEST
AIM:
To find the optimum amount of coagulant required to treat the turbid waters.
Principle:
Metal salts hydrolyse in presence of the natural alkalinity to form metal hydroxides. The
divalent cat ions can reduce the zeta potential, while the metal hydroxides are good absorbents
and hence remove the suspended particles by enmeshing them.
Apparatus:
1. Jar test apparatus

2. Pipettes
3. Beakers
4. Turbidity meter
5. pH meter
Reagents:
1. 1% Alum solution (dissolve 1.0 gram of alum in 100 ml distilled water).
Procedure:
1. Take 1 liter of sample into each of the 6 beakers.

2. Switch on the motor and adjust the speed of paddles to 100 rpm.
3. Add varying doses of alum solution i.e., 1 ml, 2 ml, 3ml, 4ml, or 6 ml to different beakers
simultaneously. (the doses varies with turbidity in water sample)
4. Allow flash mix (at 100 rpm) for 1 minute.
5. Reduce the speed of paddles to 40 rpm and continue mixing for 10 minutes.
6. Switch off the motor and allow 20 minutes for settling.
7. Collect the supernatant without disturbing the sediment and find the turbidity of each.
8. Draw the graph between Turbidity on Y- axis and alum dosage on X-axis.
9. Repeat the experiment with high doses of alum, if satisfactory results are not obtained.
10. Note the ideal (optimum) dose of the coagulant from graph (showing least turbidity) for
excellent flock formation.

Significance:
1. The test is useful for identification of natural coagulants like Nirmali seeds etc.
2. It is useful to estimate optimum dosage of coagulant required for raw waters and waste
waters.
3. If excess alum (aluminium sulphate) is used as a coagulant in water treatment plants,
aluminium may enter the municipal water and thus the human body. Excess aluminium,
if present in drinking water is highly toxic and causes acute abdominal pain and
‘dementia’. On the other hand if alum dosage is small, turbidity removal may not be
satisfactory.
Observation and calculations:
1. Raw water turbidity (NTU) = ……………………………

Sl No Sample details/ Dosage of Alum Dosage of Residual
jar no solution (ml) coagulant turbidity
(mg/l) (NTU)
1.
2.
3.
4.
5.
6.
Results and discussion:
Ideal dose of coagulant (mg/l) =

NAME OF EXPERIMENT: RESIDUAL CHLORINE
Aim:
To find out the amount of residual chlorine available in the given water sample.
Principle:
Orthotolidine is an aromatic organic compound that is oxidized in acid solution by chlorine,

chloramines and other oxidizing agents to produce a yellow coloured compound called
Holoquinone. Intensity of yellow colour of hydroquinone is proportional to the amount of
chlorine present.’
Apparatus:
Chloroscope
Reagents required:
Orthotolidone 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 the
comparator.
3. The colour which matches in both the cylinders directly gives the ‘residual chlorine’.
Significance:
1. Active chlorine should be present in drinking water within the range 0.1 to 0.2 mg/I.
However, excessive chlorine content may give out bad odour and may change even
taste of waters. Further, chlorine is said to be carcinogenic. Hence, except during
epidemics- super- chlorination is not to be done.
2. Determination of chlorine residuals is used universally in disinfection practice to control
addition of chlorine and ensure effective disinfection.
3. Chlorine in excess of 0.2 mg/ I is allergic to many humans, irritates eyes, nose and throat,
may damage skin, bleach hair and clothing and corrode pipes.
Amount of the residual chlorine (mg/l) = ……………………………………….

EXPERIMENT NO.: 8 (b)
NAME OF EXPERIMENT : Break Point Chlorination
Aim: To determine the optimum dose of bleaching powder and chlorine by Break Point
chlorination.
Apparatus:
1. Six beakers of I litre capacity
2. Stirrer
3. Chloroscope
Principle:
Chlorine combines with water to form hypochlorous and hydrochloric acid. Hypochlorous acid
dissociates to give the OCI‾ ion. Quantities of OCI‾ and HOCl depend on pH of the solution.
Hypochlorites also give the OCI‾ ions, HOCl rupture the cell membrane of microbes (disease
producing organism). These also react with the impurities like ammonia, oxidisable inorganic
matter likes ferrous ions, nitrites etc. to form chloramines and stable ions of the latter
respectively.
Procedure:
1. Take 1000 ml of water sample in six different beakers.

2. Add varying dose of bleaching powder to each beaker. This amount may be 2.0, 3.0, 4.0,
5.0 till 8.0 mg. (The dosage may be raised by 10 times in the case of polluted waters).
3. Stir the sample with a glass rod so that bleaching powder gets dissolved into water.
4. Necessary contact period of 20 minutes is given for bleaching powder to oxidize chloro-
organic compounds and form free available chlorine.
5. After the required contact period, the residual chlorine in each sample is determined.
6. The first beaker which gives the residual chlorine between 0.1 to 0.2 mg/l that will be
the required dose for disinfection.
Significance:
1. The residual chlorine of 0.1 to 0.2 mg/l is maintained in water distribution main in order
to prevent further contamination and supply the wholesome water to the consumer.
2. This test is useful to assess the quantity of bleaching powder.
Optimum dose of bleaching powder (mg/l) =

EXPERIMENT NO.: 9
NAME OF EXPERIMENT: Dissolved Oxygen
Aim:
To find the quantity of Dissolve Oxygen present in given water sample.
Principle:
The principle involved in the determination of DO is to bring about the oxidation of potassium
iodide to iodine with the dissolved oxygen present in the water sample after adding MnSO4,
KOH & KI, and the basic manganic oxide formed acts as an oxygen carrier to enable the
dissolved oxygen to take part in the reaction.
The liberated iodine is titrated against standard sodium thio-sulfate (hypo) solution using starch
as indicator. The blue color disappears to give indication of dissolve oxygen present originally.
MnSO4 + 2KOH → Mn(OH)2 + K2SO4

2 Mn(OH)2 + O2 → 2MnO(OH)2 Basic manganic oxide
MnO(OH)2 + H2SO4 → MnSO4 + 2H2O + [O]
2KI + H2SO4 + [O] → K2SO4 + H2O + I2
I2 + 2Na2S2O3 → Na2S4O6 + 2NaI
I2 + starch → Blue colored complex
Theory:
Determination of Dissolved Oxygen (DO) is important for drinking water. It is the indication of
purity of water. DO is needed for living organisms to maintain their biological processes. If DO is
less than the required limit, (6 to 7 mg/l) it is the indication of pollution due to sewage or
industrial waste. DO test is used to control the amount of oxygen in boiler feed water to
prevent corrosion. DO test helps to assess raw water quality and to keep a check on stream
pollution.
Oxygen is poorly soluble in water. The solubility of DO decreases with increase in concentration
of salt at 1 atm pressure. The solubility of oxygen of air in fresh water with low solid
concentration varies from 14.5 mg/l at 0°C to about 7.5 mg/l at 30°C. Iodometric (Winkler’s
method) are used for determining DO in water.
Apparatus
BOD bottles (capacity 300 ml), burette and pipettes

Reagents required:
1. Standard sodium thio-sulfate solution (N/50);

2. Potassium permanganate solution (N/10),
3. Potassium oxalate solution (2%);
4. Manganous sulfate solution (4.8%);
5. Alkaline potassium iodide;
6. Freshly prepared starch solution;
7. concentrated sulfuric acid
Procedure:
1. Take a glass stopered bottle of 300 ml capacity and fill it completely with water sample.
2. Add 0.9 ml conc. H2SO4 and 0.2 ml (4drops) KMnO4 solution with the help of a pipette.
The tip of pipette should dip below the liquid surface. Stopper the bottle and mix the
contents of the bottle by inverting it a few times. If the permanganate color is not
discharged within 5 minutes, add additional amount of KMnO4.
3. Add 0.5 ml of potassium oxalate solution, stopper and mix well. Add additional amount
of oxalate solution if the permanganate color is not discharged in 10 minutes.
4. Now add 2 ml of MnSO4 solution followed by 3 ml of alkaline KI solution. Stopper and
shake and allow the precipitate to settle.
5. Now add 1 ml of conc. H2SO4 solution and mix until the precipitate is completely
dissolved.
6. Measure 102.2 ml of this solution with a measuring cylinder in to a conical flask and
titrate slowly against N/50 hypo solution.
7. When the color of the solution is very light yellowish add 2 ml of freshly prepared starch
solution and continue the titration to the disappearance of the blue color and note
down the volume of hypo used.
8. Repeat the titration to get at least three readings and note down the volume of hypo
used.
Significance:
1. It is necessary to know DO levels to assess quality of raw water and to keep a check on
stream pollution. If DO is less than 4 mg/l. aquatic ecosystems would be badly affected.
2. DO test is necessary for all aerobic biological wastewater treatment processes to control
the rate of aeration.

Observation Table:
Total volume of the sample taken = 300ml

Volume of reagents added during = 0.9 ml H2SO4 + 0.2 ml KMnO4 + 0.5 ml
The preparation of iodine solution = K2C2O4 + 2 ml MnSO4 + 3 ml alkaline
KI = 6.6 ml
Volume of prepared solution (iodine) taken for titration = 102.2 ml
Average volume of N/50 hypo solution used in 3 readings = V ml
S. Volume of Volume of N/10 Hypo solution used in titration

No. sample taken Initial burette Reading Final burette Reading ml of hypo solution
(ml) (ml) (ml) used (ml)
Calculations:
6.6 ml of the reagents have been added under such conditions that approximately equal
volume of the sample is displaced. This dilutes the sample and so a correction factor is
needed.
N 1 V1 = N2 V2
(Oxygen solution) (Hypo solution)
N1 × 100 = 1/50 × V
N1 (normality of the sample with respect to DO) = (1/100) × (V/50) = 8V/5000 g/l =
1.6 × V mg/l
Volume of original sample that will be equivalent to 102.2 ml of the prepared solution is
given by:
Total = (volume of sample-volume displaced by reagents)/(total vol of sample) ×102.2

= (300- 6.6)/ (300) ×102.2 = 100 ml

Precautions:
1. After the addition of reagents in water sample taken inside BOD bottle check is done
and its removal is done if formed. Failing which the oxygen of air present inside the
bubble will also take part in the reaction and this will lead to high value of DO.
2. The reagents should be added inside the bottle with the help of pipette to avoid more
air contact.
3. Special care should be taken in sampling.
4. As for as possible, the sample should not be allowed to come in contact with air.

EXPERIMENT NO.: 10
NAME OF EXPERIMENT: Biological Oxygen Demand (BOD)
Aim:
To determine the Biological Oxygen Demand (BOD) of given water sample.
Principle:
The BOD is an empirical biological test. This BOD test may be considered as wet oxidation
procedure in which the living organisms serve as the medium for oxidation of the organic
matter to carbon-dioxide and water.
a b 3 Bacteria a 3
CnHaObNc + n+ --- - --- - ---- cO2 nCO2 + --- - --- c
4 2 4 2 2
X H2O + cNH3
On the basis of the above relationship, it is possible to interpret BOD data in terms of organic
matter as well as the amount of oxygen used during its oxidation.
Interference:
Undesirable oxygen consumption via nitrification can be prevented by addition of 1 ml of an N-

allyl thio-urea solution. Free chlorine present in some waste waters after chlorination reacts
with organic components within about 2 hours and does not interfere. Compounds which use
up oxygen without the presence of micro-organisms (e.g. iron (II), sulphite or sulphide ions) are
oxidized by leaving the original sample for 2 hours with occasional shaking. Lack of nutrient in
dilution water, lack of an acclimated seed organisms and the presence of toxic substances can
result in very low BOD values despite the presence of sufficient degradable organic materials. In
such cases, a series of measurements should be carried out at greater dilutions.
Reagents:
1. Distilled water
2. Phosphate buffer solution
3. Magnesium sulphate solution
4. Calcium chloride solution
5. Ferric chloride solution
6. Sodium thiosulphite solution

Procedure:
1. Place the desired volume of distilled water in a 5 liter flask. Aeration is done by bubbling
compressed air through water.
2. Add 1 ml of phosphate buffer, 1 ml of magnesium sulphate solution, 1 ml of calcium
chloride solution and 1 ml of ferric chloride solution for every liter of distilled water
(dilution water)
3. In the case of the waste waters which are not expected to have sufficient bacterial
population, add seed to the dilution water. Generally 2 ml of settled sewage is sufficient
for 1000 ml of dilution water.
4. Highly acidic or alkaline samples are to be neutralized to a pH of 7.
5. Add 2 or 3 ml of sodium thiosulphite solution to destroy residual chlorine if any.
6. Take the sample as follows:
Strong wastes: 0.1, 0.5, or 1 %
Settle domestic sewage: 1, 2.5 or 5%
Treated effluents: 5, 12.5 or 25%
River water 25 % to 100%
7. Dilute the sample with the distilled water and mix the contents well.
8. Take diluted sample into 2 BOD bottles.
9. Fill another two bottles with diluted (distilled) water alone.
10. Immediately find D.O. of a diluted waste water and diluted water (distilled water).
11. Incubate the other two BOD bottles at 200C for 5 days. They are to be tightly stoppered
to prevent any air entry into the bottles.
12. Determine D.O. content in the incubated bottles at the end of 5 days (120 hours).
Significance:
1. BOD test gives an idea of the biodegradability of any sample and strength of the waste.
2. Drinking water usually has a BOD of less than 1 mg/l and water is considered fairly upto
3 mg/l of BOD. When BOD value reaches 5 mg/l, the water is doubtful in purity.
Observations and results:
Sl Vol. of Dilution Initial Final D.O. Initial D.O. Final D.O. 5 days BOD
No sample ratio D.O. of of sample of blank of blank at 200C
sample mg/l mg/l mg/l (mg/l)
mg/l
1.
2.
3.
4.
5.

Calculations:
 Let initial D.O. of diluted sample = Do

 D.O. at the end of 5 days for the diluted sample = D5
 Initial D.O. of distilled water (blank) = Co
 D.O. at the end of 5 days for the distilled water blank (blank) = C5
 D.O. depletion of dilution water = Co-C5
 D.O. depletion of diluted sample = D o-D5
 D.O. depletion due to microbes = (D o-D5) – (Co-C5)
(Do-D5) x volume of bottle

 0
BOD at 20 C of the sample = --------------------------------- - (Co-C5)
ml sample

EXPERIMENT NO.: 11
NAME OF EXPERIMENT : Chemical Oxygen Demand (COD)
Aim:
To find out Chemical Oxygen Demand (COD) of given wastewater sample.
Principle:
The organic matter present in sample gets oxidized completely by K 2Cr2O7 in the presence of
H2SO4 to produce CO2 and H2O. The excess K2Cr2O7 remaining after the reaction is titrated with
Fe (NH4)2 (SO4)2. The dichromate consumed gives the O2 required to oxidation of the organic
matter.
Apparatus:
1. Reflux apparatus
2. Hot plate/ heating mantle
3. Burette
Reagents:
1. Standard potassium dichromate 0.25 N
2. Sulphuric acid with reagent (Conc. H2SO4 + Ag2SO4)
3. Standard ferrous ammonium sulphate 0.1 N
4. Ferroin indicator
5. Mercuric sulphate
Procedure:
1. Place 0.4 gm of HgSO4 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 beeds.
4. Add slowly 30 ml of H2SO4 containing Ag2SO4 and mix thoroughly.
5. Connect the flask to condenser. Mix the contents thoroughly before heating. Improper
mixing results in bumping and the sample may be blown out.
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 0.1 N Fe(NH4)2 SO4 using ferroin indicator, Sharp colour
change from blue green to wine red indicates the end point.
9. Reflux the blank in the same manner using distilled water instead of sample.

Significance:
1. COD test is widely used in the place of BOD in the operation of treatment facilities
because of the speed with which the results can be obtained.
2. The ratio of BOD to COD is useful to assess the amenability of waste for biological
treatment. Ratio of BOD to COD greater than or equal to 0.8 indicates that wastewaters
are highly amenable to the biological treatment.
Observations and results:
Sl No. Sample details Vol. of Initial Final Vol. of COD of the

sample burette burette Fe(NH4)2 (SO4)2 sample
taken reading reading added ( ml)
ml ml ml mg/l
1.
2.
3.
4.
5.
6.
Calculations:
Quantity of Fe (NH4)2 (SO4) added for blank = A ml
Quantity of Fe (NH4)2 (SO4) added for the sample = B ml
(A-B) x Normality Fe (NH4)2 (SO4) x 8 x 1000

COD = -------------------------------------------------------------
Quantity of sample (ml)
The COD of the given wastewater sample (mg/l) =

EXPERIMENT NO.: 12
NAME OF EXPERIMENT: Gas Liquid Mass Transfer Characteristics
(Aeration apparatus)
Aim:
To measure the rate of gas liquid mass transfer characteristics in a diffused bubble system and
to examine variables that influences the rate of mass transfer in Aeration set-up.
(i) To determine the mass transfer co efficient, kla.

(ii) To study the effect of stirrer speed and Temperature and liquid depth on k la.
Introduction:
Mass transfer between gas and liquid phases is commonly encountered in the environment
sector. In aerobic metabolism, oxygen acts as an electron acceptor for the catabolism. Since the
activated sludge process is designed to be substrate limiting, metabolism sets the rate of
oxygen demand. Dissolved oxygen concentration is one of the most important control variables
in any aerobic reactor. The purpose of the aeration system in an aerobic system is to provide
and transfer oxygen to the liquid at such a rate that it never becomes the limiting factor.
Theory:
Since oxygen has a low solubility in aqueous solution, and biological systems often has a high
demand for oxygen, an understanding of how oxygen is transferred to the liquid phase hence to
cells in reactor is crucial for successful design and analysis. Maintaining the design
concentration while organisms are consuming oxygen requires that oxygen be transferred
continuously into the reaction liquid.
OTR (Oxygen Transfer Rate) = dC/dt = kLa (C* - C)
Where,
kL = Oxygen Transfer Co-efficient (cm/h)
a = Gas Liquid interfacial area (cm2/cm3)
kL a = Volumetric Oxygen Transfer Co-efficient
C* = Saturated Dissolved Oxygen concentration
C = Actual dissolved oxygen concentration in the broth
OTR = Oxygen transfer rate (mg O2/L-h)
The mass transfer coefficient is a function of the mechanics of a particular reactor:its

dimensions and its operating parameters.
Two common ways to experimentally measure kLa in a fermentor are:
1) The static or gassing out method (used in this experiment), and

2) The dynamic method with growing culture.

dC/dt = (oxygen transfer rate – oxygen uptake rate)
Where,
C = dissolved oxygen concentration (mmol O2/L)
In case of static method where no bio mass is present, oxygen uptake rate is zero.
The saturation oxygen concentration in water (C*) varies with temperature. Values for C* are
given in the table bellow:-
Temperature T °(C) Solubility(Air, 1 atm) mg O2/L

mmol O2/L
0 0.456 14.62
6 0.389 12.48
10 0.355 11.33
15 0.322 10.3
20 0.288 9.24
25 0.263 8.42
30 0.242 7.75
35 0.228 7.29
40 0.215 6.90
Static method:
This experiment will focus on determining kLa by means of the static method. The static method
requires that no yeast be present in the broth. This drives our OUR (oxygen uptake rate) to zero
so that any measured changes in C are due to OTR (oxygen transfer rate).
dC/dt = (kLa) (C*-C)
Here the difference between the saturation dissolved oxygen concentration and the actual
concentration is the driving force behind any transfer of oxygen into solution.
Description:
The setup consists of an open water tank with variable speed stirrer. Air is supplied from air
pump provided to bottom of vessel. Flow of air is directly metered with the help of rotameter
and can be regulated by means of valve provided with rotameter. A heater with controller is
provided to maintain the desired temperature in the vessel. Three air diffusers of different type
are provided with the set up and are interchangeable.
1) Vessel
Material : Acrylic
OD : 300 mm
ID : 284 mm
Height : 380 mm

2) Air Pump : Capacity 15 LPM
3) Heater : Power 425 Watts
4) Rotameter : range 1.23 to 12.3 LPM of air
5) Air Diffuser : 3 No.
1) Sparger
2) Treble Air Stone
3) Single Air stone
Experimental Procedure:
1) Set the temperature of tank with the help controller.
2) Wait till the temperature of tank reaches ret value.
3) Set the RPM of stirrer to some desired value.
4) Deoxygenate the water in tank by chemical method as explained under “De oxygenation
of Water”.
5) When the DO reaches a steady value near 0%, start the air flow.
6) Measure the DO at regular intervals of time until DO reaches some steady-state value.
Effect of varing agitation speed on kLa
7) Repeat steps 3-6 at different stirrer speed.

8) Repeat steps 3-6 at different liquid heads.
9) Repeat steps 3-6 at different air flow rate.
10) Repeat steps 1-6 using other diffuser provided with the set up.
Observation and Calculations:
Data:
Volume of water = ---------------

Temperature of water = ------------
RPM of stirrer = -------------------
Saturation oxygen concentration, C* = ----------
Initial dissolved oxygen concentration, Co = -----------
Observation & calculation table:
S.No. Time(sec) Dissolved oxygen

(DO),mg/L In[(C*-Co)/( C*-C)]

Plot the graph of time vs In[(C*-Co)/( C*-C)], and find the slope of line.
Slope of graph = kLa, mass transfer co efficient (sec-1)
Calculate the oxygen transfer rate, R = kLa (C*-C)
S.No. Time(sec) R (mg O2/lit-sec)
Precautions & Maintenance Instructions:
1. The chemicals should be measured precisely.

2. Use DO meter carefully.
3. Clean the vessel with fresh water after experiment.

EXPERIMENT NO.: 13
NAME OF EXPERIMENT : Softening or Demineralization of Water

(Ion exchange column)
Aim:
To study the continuous softening or demineralization of water using two bed Ion-Exchange
Unit.
Introduction:
The most usual ion exchange material employed in water softening is a sulphonated styrene
based resin, supplied by the makers in the sodium form. This resin has a strong affinity for
calcium and magnesium ions, and will also remove ferrous ions after the more or less complete
removal of calcium and magnesium.
Softening can be carried out as a batch process by stirring a suspension of the resin in the
water for a period until equilibrium, or an acceptable level of hardness is reached.
Theory:
It is more convenient to operate a continuous flow process by passing the water slowly
downwards through a column of resin beads. The exchange reaction takes place rapidly enough
for the upper layers of the bed to approach exhaustion before the lower layers of the bed are
able to exchange ions. There is thus a zone of active exchange which moves down the column
until the resin at all depths becomes exhausted. The position at an intermediate stage can be
illustrated as below.
When the zone of active exchange reaches the bottom of the column, the emerging water
begins to show an increasing hardness. This is the breakthrough point, when it becomes
necessary to regenerate the resin with a strong sodium chloride solution.
A low cost, bench-mounted unit designed to demonstrate the use of ion-exchange resins for
either continuous water softening of demineralization. The equipment is designed to emulate
the industrial operation of such units, including monitoring ’break-through’ and regeneration
cycles.
Description:
The two vertical transparent tubes mounted on the backboard contain the respective cation
and anion resin. A manifold arrangement at the inlet and outlet to the tubes allows the flow
configuration to be changed to simulate the cycles involved in operation of a deionizer. Union
couplings permit the tubes to be removed from the manifolds and interchanged for
softening/demineralization experiments. Regenerant and test or wash solutions are contained
in independent sumps and delivered to the apparatus by pump. Effluent may be fed to a sump
tank and treated water collected in bottles for tests on hardness, conductivity or dissolved

solids. A conductivity meter connected to the outlet of second ion exchange bed gives a
continuous indication of the progress of demineralization. The apparatus is supplied with
typical commercial cation and anion resins.
Specifications:
Column (2 No.) = Material Borosilicate Glass/SS

(Anion &Cation) Dia 55mm, Length 500 mm approx.
Water tank = Material SS, Capacity 25 ltrs.
Feed circulation = FHP pump Tullu/Champion make
Flow Measurement = Rotameter
Piping = SS and PVC size ¼’’
Control panel comprising of:
Standard make on/off switch, mains indicator & fuse etc.
The whole set-up is mounted on a powder coated base plate.
Utilities Required:
Electricity Supply: 1 Phase, 220 V AC, 0.5 kW.

Bench Area: 1.2m × 1 m
Required Chemicals & Laboratory Glassware
1. Fill the column with ion exchange resin.

2. Fill the water tank with water.
3. Connect the power supply.
4. Start the water at any flow rate and check the conductivity of the inlet water.
5. Run the water at least half an hour and then check the conductivity if the conductivity
decreases means deionization occurs.
Observation and Calculation:
Initial conductivity of water = mS

Final conductivity of the water = mS
Flow rate water = LPH
(µS = micro Simens, it is an electronic unit)

EXPERIMENT NO.: 14
NAME OF EXPERIMENT : Most Probable Number (MPN)
Aim:
To determine MPN of coliforms of the given water samples.
Apparatus:
1. Auto clave
2. Hot air oven
3. Incubator
4. Durham Vial
5. Fermentation tubes
6. Inoculation loops (3 mm diameter of platinum wire) and
7. All other material used in standard plate count test.
Reagents:
1. Lauryl tryptose broth

2. Brilliant green bile broth
3. Endo or Eosin methelene blue agar
4. Reagents for gram staining.
Procedure:
Shake the water sample thoroughly before making dilutions or before inoculation.
(a) Presumptive test:

1. Select dilutions according to the expected coli firms.
2. Inoculate a series of MPN fermentation tube with appropriate measured quantities of
the water sample to be tested.
3. Add appropriate quantity of Lauryl tryptose broth in each tube.
4. Put one Durham’s vial inverted in each test tube. The top of the tubes is plugged with
cotton plug.
5. Place all these tubes in an incubator at 35-370C within 30 minutes.
6. After 24 hours examine the tubes carefully. Those showing gas in the Durham’s vials are
recorded as positive (=). If no gas has been formed, reincubate for another 24 hours
and at the end of 48 hours examine again.
7. Record the presence or absence of gas at each examination of the tubes regardless of
the amount.
8. Formation of the gas within 48±3 hours in any amount in inverted Durham’s vials are
recorded as positive (+). The absence of gas formation at the end of 48±3 hours of
incubation is considered as negative test.

(b) Confirmed test:
1. Prepare fermentation tubes with 10 ml brilliant green lactose bile broath and Durham’s
vials. The number of tubes to be prepared is equal to all positive tests in the
presumptive test.
2. Shake gently the fermentation tubes with positive results and transfer one loop or
loopful or medium to brilliant green lactose bile broath by using a sterile metal loop.
3. Incubate the tubes at 35-370C for 48±3 hours.
4. The formation of gas in any amount in the Durham’s vials of BGLB tubes at any time
within 48±3 hours constitutes a positive confirmed test.
(c) Completed test:
The completed test though not always necessary, is sometimes done to demonstrate with
certainly that organism showing positive results for the confirmed test are really members of
the coli form group.
1. Prepare endo or Eosin methylene blue (EMB) agar Petri plates. The number of the Petri
plates to be prepared is the same as that of tubes showing gas production in BGLB
medium.
2. Streak inoculums from the BGLB tubes on these plates in such a way that the colonies
after separation have a distance of 0.5 cm.
3. Incubate these plates at 370C ± 0.2 for 24 ± 2 hours.
4. Examine the plates for bacterial growth as colonies. Well isolated colonies with a dark
center (nucleated) are typical coli form colonies. They may have a metallic surface
sheen. The colonies that are pink or opaque and or not of coli form and are reported as
negative in the completed test.
5. Now inoculate as isolated coliform colony (avoid picking up a mixture) from each plate
into the tubes of Lauryl tryptose broth and record the gas production within 48 hours at
370C
Significance:
1. M.P.N. is the most probable number of coliform bacteria in 100ml of water. No water
sample should contain more than 10 MPN and the average of several values of MPN
should not be more than 1. It is a measure of the bacterial density of water and is a
measure of the population of pathogens in water. If MPN is more, the pathogens may
cause several water borne diseases such as typhoid, cholera, dysentery, fevers,
infectious hepatitis(jaundice), poliomyelitis, amoebeasis and gastro-entireties. Improper
disposal of domestic and municipal wastes pollutes water sources with MPN. MPN can
be removed by disinfection in water treatment plants. Strict precautions against back
syphonage and cross connections are required if amoebic cysts are not to be found in a
distribution system.
2. MPN determination is useful in the selection of water supplies for human needs.
3. It is useful to assess the degree of contamination of receiving waters by domestic
sewage.
4. It is useful to find efficiency of disinfectant and treatment units for bacterial removal.

Computing and Recording of MPN:
Record the number of positives findings of coli form group organism (presumptive, confirmed
and completed) resulting from multiple portion decimal dilution planting as the combination of
positives and compute in terms of the MPN.
Table: MPN Index For Various Combinations Of Positive Results In Fermentation Tube Tests

EXPERIMENT NO.: 15 (a)
NAME OF EXPERIMENT : Suspended Particulate Matter (SPM) and Respirable Particulate

Matter (RPM)
Aim:
To determine the suspended particulate matter (SPM), Respirable particulate matter (RPM) in
ambient air.
Filter selection and conditioning:
Glass micro fiber filters are particularly suitable for determination of particulates because of
their high retention efficiency combined with low pressure drop, high resistance to blocking
and low affinity for moisture. Three types of filters-GF/A. EPM-1000, and EPM -2000 are
available for Respirable Dust Sampler. The whatman GF/A glass fiber filter has been in use for
more than 20 years and can be used safely where trace element analysis is not required. What
man EPM-1000 or EPM-2000 spectra quality glass fiber filters containing very low levels of
contaminants are recommended for use where additional chemical analysis is anticipated.
Each filter should be visually inspected using a light table. Remove loose fibers with a
soft brush. Discard or return to the supplier the filters with pinholes and other defects such as
tears, creases or lumps.
Identification:
Assign a serial number to each filter. Stamp this number on two diagonally opposite corners –
one stamp on each side of the filter. Apply gentle pressure to avoid damage to the filter. EPM -
2000 comes numbered directly from the manufacturer.
Equilibration:
Equilibrate the filter in the conditioning environment for 24 hours before weighing it to
minimize errors in the weight; longer periods of equilibration will not affect accuracy. The
conditioning environment should average between 20 and 250C and not than ±30C with a
relative humidity (RH) less than 50 % without varying more than ±5 % RH. A convenient working
RH is 40 %.
Weighing:
Clean filters are usually processed in lots-that is, served at one time. Clean filters must not be
folded or creased prior to weighing or use. Before weighing the first filter, check the balance by
weighing a standard class-S weight of between 3 and 5 g. Record the actual and measured
weights the date and the operators initials.
Sampling Procedure:
Sampling is usually done at 1.5 m height. Ensure that the filter is parallel to the ground. To
obtain a representative sample, the sampler should not be placed under a tree near a wall or
other obstruction that would prevent free air flow from the ambient atmosphere.

During inclement weather (including high winds), move the entire sampler to a protected
location for servicing when practical ; before the new filter is installed, remove loose particles
from the inside surfaces of the sampler and the surfaces around the filter holder by wiping with
a clean cloth. Protect the clean installed filter when returning the sampler to the shelter.
Filter Installation:
To install a filter, use the following procedures:
1. Remove the dome of the sampler by loosening the four Knobs.
2. Center the filter with the left side up on the wire screen so that the packet forms an
airtight seal on the outer edge (1 cm) of the tilter when the faceplate is in position when
aligned correctly, the edges of the tilter will be parables both to the edges of the Screen
behind end to the faceplate gasket above it. Poorly aligned alters show uneven white
borders around the filter.
3. Tighten the four knobs just enough to prevent leakage when the filter is aligned and the
dome cover is in place. Excessive tightening may cause the filter to stick or permanently
damage the gasket.
Operational Checks:
Before connecting the instruments to the mains, see that all switches of instrument should be
in %% OFF position ‘‘. Now connect the instrument to the mains. Switch on the power with the
help of voltage stabilizer switch. The stabilizer voltage Output Should be in the range 230 a:15
VAC. Set the timer by removing the red needle to full scale i-e 24 hours and take back the
desired sampling time. Move the black needle to the extreme and clockwise or set to desired
sampling time. Rotate the flow controller knob. Now the blower will be on and it will draw ' the
sample through the filter and impinger tubes. Make flow rate measurement after a warm - up
time of at least 5 minutes. '
Adjustment of desired flow and operation:
Refer to the Calibration Graph and adjust the speed of the Blower motor to obtain the ∆P on
the manometer corresponding to the required flow rate. Let this flow-rate be Qi. ∆P is addition
of both side deviations in manometer in 'mm. However the actual flow through the alter paper
is expected to be reduced because of deposition of dust. Note down ∆P manometer again, just
before the end of the sampling and read corresponding flow rate from the calibration graph.
Let this reduced final flow rate be Qf. After the sampling is over, note down the ' sampling time
as indicated on the time totalizes.
Removing the Exposed Filter:
The following procedure should be used to remove the exposed filter:

1. Remove the dome and lift the exposed filter from the supporting screen by graphing it
gently at the ends, not at the corners.

2. Fold the filter length wise at the middle with the exposed side in; if the collected sample
is not centered On the filter (i.e. the unexposed body is not uniform around the alter).
Fold so that only deposit touches the deposit. An improperly folded filter, where
smudge marks from the deposit extend across the borders, is undesirable.
3. Check the fitter for signs of air leakage. Leakage may result from a worn faceplate
gasket or from an improperly installed gasket. If leakage signs are observed, void the
sample, determine the cause, and take corrosive actions before starting another
sampling period. Generally a gasket deteriorate slowly and thus the operator can decide
well in advance (by the increased fuzziness of the sample outline) to change the gasket
before a total failure occurs.
4. Inspect visually the gasket faces to see if glass fibers from the alter are being left behind
due to over tightening of the faceplate knob stud and consequent cutting of the tilter
along the gasket interface.
5. Check the exposed filter for physical damage that may have aired during or after
sampling. physical damage after sampling would not invalidate the samples if all pieces
of the tilter were put in the folder; however, sample losses due to leakages during the
sampling period or bosses of loose participates after sampling (e.g. loss when folding
the filter ) would invalidate the tilter, so mark much samples void before forwarding
them to tie laboratory.
6. Check the appearance of the participates. Any changes from normal colour for example
may indicate new emission sources or construction activity in the area. Note any change
on the field data forms along with any obvious reason for the change. Place the folder
filter into a plastic bag for storage/shipping.
Analysis of Samples:
Sample documentation and Inspection:
1. Remove the filter fodder from its shipping bag.

2. Record the tilter number on the sampler Geld data form and on the laboratory data log.
3. Examine the shipping envelope. If sample material has been dislodged from the filter,
recover as .much as possible by brushing it from the envelope on to the deposit on the
filter with a soft camels heir- brush.
4. Examine the filter; if Insects are embedded in the sample deposit, remove them with
Teflon-tipped tweezers, but disturb as little of the sample deposit as possible. If more
than 10 insects are observed refer the sample to the supervisor for a decision to accept
or reject it.
5. There is also the non-respirable (large particulate) fraction stored on a folded weighing
paper, which is handled in the same manner as the filter, steps 1 through 4, above.

Filter Equilibration:
1. Equilibrate the exposed filters In a conditioning environment for 24 hours; up to 48

hours may be needed for very damp filters.
2. Use an equilibration chamber with a saturated chemical solution to get an RH of less

than 50% at 20 degree C to 25 deg C. The chamber is recommended lieu of a controlled
temperature / humidity weighing room. An Air-conditioned room may be used for
equilibration if an RH of 50% that is constant within Asia and an air temperature that is
constant within +3 deg C are maintained while the tilters are equilibrating. A convenient
working RH is 40%. Keep a hygrometer in the room.
Gravimetric Analysis:
1. Weigh the exposed filters to the nearest milligram (mg) on the analytical balance within
30 sec removing them from the equilibration chamber.
2. Weigh the filter in the conditioning environment if practical, if not, be Sure that the
analytical balance is as close as possible to the conditioning chamber where it is
relatively free of air currents and where it is at or near the temperature of the chamber.
3. Record the weight in the laboratory data log and on the sampler field data form.
4. For the NRPM, the weighing papers with non - respirable fraction are weighed in the
same manner as the exposed filters.
Calculations of sample air volume and SPM and RPM concentration:
Calculate the air volume sampled, by applying the following formula:
V = ( Qi + Qf ) / 2) T------------------------------------ Eq. ( 1)
Where
V = STP- equivalent (25 deg. C. 1 atm) air Volume sampled, m3.

Qi = Initial air flow rate, m3 / min, STP.
Qf = Final air flow rates m3 main, STP.
T = Sampling period in minutes (from time totaliser )
SPM Calculation:
Calculate the SPM concentration by using the following equation
SPM (μg/m3) = (Wf - Wi) x 106

---------------- ------------------------------------Eq. (2)
V

Where
V = Volume of air sampled,m3

Wf = Weight of exposed filter, grams.
Wi = fare weight of tilters grams.
RPM Calculation:
1. Calculate the RPM concentration by using the Eq (2) as above, except substituting:
“RPM (µg/m3)'' in place of SPM (µg/m3)-
2. Calculate the (total) SPM Concentration by using Eq (2) again, except substituting:
“Wp + Wf '' in place of Wf, and “Wj + Wi” in place of Wi,
Where
Wp = Weight of material that was collected on the pan including: the 'weighing paper, gm.
Wj = Initial weight of the weighing paper, gm.
Record all original calculation in the data log book.
Method of sampling for gaseous pollutants:
Take the absorbing solution (as mentioned in the specific procedures) in each or the impinger
tubes. 'To adjust the individual flow rates through the impinger tubes connect inlet of one of
the impinger tubes to the Rota meter and outlet to (the of the four input connections of the
manifold. Adjust the required flow rate with the help of the respective restricted and then
lighten the screw to keep the flow rate constant. Let this initial flow rate be F1.
Follow the same procedure to adjust flows through the other impinger tubes. Measure the
individual flow rates again with the Rota meter just before the end of the experiment. Let that
flow rate be F2. Acer the sampling is over, note down the sampling time as indicated on the
localizer.
Calculation of volume of air sampled through the absorber (Impinger tube )

The volume of air sampled, V. is given by.
V (m3) = (F1 + F2) x T x10 -3 ------------------------------------------------------------ Eq (3)
Where
F1 = Initial flow rate at start of sampling. lpm
F2' = Final flow rate at end of sampling. lpm
T = Sampling time period, min.

NAME OF EXPERIMENT : Nitrogen Dioxide (NO2)
Aim:
Determination of Nitrogen Dioxide (NO2) in Ambient Air the suspended particulate matter in
ambient air
Principle and Applicability:
Nitrogen dioxide (NO2) is collected by bubbling air through a sodium hydroxide - sodium
arsenate solution to form a stable solution of sodium nitrite (NaNO2). The nitrate ion produced
during sampling is reacted it Phosphoric acid, aulphanilamide and N-1 (naphthyl)
ethylenediamine di-ydrochloride, to form an azo dye, and then determined colourimetrically.
The method is applicable to collection of 4 to 24 hours samples in the field and Subsequent
analysis in the laboratory.
Range and sensitivity:
The range of the analysis is 0.01 to 1.5 μg No2 / ml. A concentration 0.04 μg NO2/ml will
produce absorbency approximately 0.02 with 1 cm cells, and Beer's law is obeyed throughout
this range (0 to 0.1 absorbency unites). With 25 ml absorbing reagent and a sampling rate of 0.2
Lpm for 24 hours. The range of the method Is 3.5 to 180μg/m, (0.002 to 0.100 ppmv ) of
nitrogen dioxide.
Interference:
Nitric oxide (NO) Is a positive interferers. The presence NO can increase the NO2 response by 5
to 15 % of the NO2 sampled. The interference of sulphur dioxide (SO2) is eliminated by
converting it to sulphate ion with hydrogen peroxide before analysis.
Precision and Stability:
The relative standard deviations for sampling NO2 concentrations of 78, 105 and 328 gamma
are 3, 4 and zo/orespedively. Collected samples are stable for at least 6 weeks.
Apparatus:
1. Volumetric Flask - 50, 10Q, 200, 250, 50Q, 1000 ml.

2. Graduated Cylinder - 1,00Q ml.
3. Pipettes 1, 2, 5, 10, 15 ml. Volumetric, 2 ml graduated at Q. 1 ml. Intervals.
4. Test Tubes - Approximately 20 x 150 mm.
5. Spectrophotometer Capable of measuring absorbency at 540 nm.

Reagents:
1. Sodium Hydroxide - AR reagent grade.

2. Sodium Arsenate - AR reagent grade.
3. Absorbing reagent - Dissolve 4.0 gm sodium hydroxide in distilled water, add gm of
sodium arsenate and dilute to 1000 ml. with distilled water.
4. Sulphanilamide M. P of 165 to 167 deg C.
5. N (1- naphthyl) Ethylenediamine Dihydrochloride (NEDA) - Best grade available.
6. Hydrogen Peroxide - AR reagent grade 30 %.
7. Sodium Nitrites - Assay of 97% NaN01 or greater.
8. Phosphoric Acid - AR reagent graded--. 85% minimum.
9. Sulphanllamide Solution – Dissolve 20 gm sulphaqilamide in 700 ml distilled water. Add
with mixing 50 ml. concentrated phosphoric acid and dilute to 1.000 mf. This solution is
stable fpr one month if refrigerated.
10. NEDA Solution- Dissolve 0.5 gms of NEDA in 590 ml of distilled water. This solution is
stable for one month, if refrigerated and protected from light.
11. Hydrogen Peroxide Solution - Dilute 0.2 ml of book hydrogen peroxide to 250m1 with
distilled water. This solution may be used for one month, if preceded from light and
refrigerated.
12. Standard Nitrite Solution - Dissolve sufficient desiccated sodium nitrite and dilute with
distilled water to 1000 ml, so that a solution containing 1,000 gg Noz/ml, is obtained.
The amount of NaNO2 to be used is given by :
G = 100 x (1.500 / A)
Where
G =% amount of NaNO2. grams
1.500 = Gravimetric factor in converting No2 into NaNo2
A = Assay Percent
Analysis:
Replace any water lost by evaporation during sampling by adding distilled water tip 'to' the
calibration mark on the absorption tube. Pipette In . 1 ml of hydrogen peroxide solution, 10 ml
of Sulphanilamlde solution and 1..4 my NEO'A solution with thorough Su p mixing after the
addition of each reagent. Prepare a blank in the same manner using IQ my of unexposed
absolution ' reagent after IQ minute concur - development interval, measure the absorbable at
540 nm against the blank . Read μg No2 /mI from the calibration curve. Samples with an
absonance greater than 1.0 must be reanalyzed after ' diluting an aliquot (less than 10 ml) of
the colleted sample with unexposed absorbing reagent.

Calculation:
Calculate the concentration of nitrogen dioxide (NO2), using the following formula:
(NO2) (μg / m3) = (μg NO2/ml ) x 25

---------------------------
v x 0.82
25 = Volume of absorbing reagent used in sampling, ml.
v = volume of air sampled my earlier.
0.82 = empirical factor ' fir collection calculated by using Eq (3) as given efficiency
Calculate the concentration of nitrogen dioxide In units of ppm vol. by the formula: (NO 2) (
ppmv) = (NO2) (μg /m3) x 0.000532

EXPERIMENT NO.: 15 (c)
NAME OF EXPERIMENT : Sulfur Dioxide (SO2)
Aim:
Determination of Sulfur Dioxide Content of the Atmosphere (Tetrachloromercurate

Absorber/pararosaniline Method).
Principle of the Method:
1.1.1 Sulfur dioxide, in an air sample, is absorbed into a solution of potassium or sodium
tetrachloromercuratell-tEzM) by aspirating ' a ' measured air sample through unabsorbed
vessel. This procedure results in the formation of monochlorosulfonatomerarate (11) complex
(3), which resists oxidation by the oxygen in the air ( 1,2,3), Ethylenediamine-tetraacetic acid di-
sodium salt (EDTA) Is added to this solution to complex heavy metals that catalyze the oxidation
of the colleted Sulfur dioxide (4.5). Once this monochlorosulfonatomercurate complex is
formed, it is stable to strong oxidants (egg ozone, oxides of nitrogen and hydrogen peroxide)
(2). After sampling is completed, any ozone in the solution is allowed to decay (5). The liquid is
treated first with a solution of sulfuric acid to destroy the nitrite anion formed from the
absorption of oxides of nitrogen present in the atmosphere (6). It is then treated with solution
of formaldehyde and specially purified, acid- bleached pararosanline containing phosphoric acid
to control pH. Pararosanillne, formaldehyde and the biosulfite anion read to form the $
Intensely coloured Pararosanllinemethylsulfonic acid, which behaves as a two-color PH
indicators amid = 548 nm at ad 1.6 +.0.1, c = 47.7 x ' a 10 ). The E value assumes quantitative
production of the absorbing species. Re pH of the final solution is adjusted to 1.6 ± 0.1 by the
addition of a prescribed amount of 3M phosphoric acid to the pararosanlline reagent (5). This
technique is the basis of the reference method for the determination of sulfur dioxide by the
U.S. Environmental Protection Agency (7).
1.1.2 Two variations are given, differing only in the pH of the final solution. The variation
described above is designated Variation A and is the method of choice. It elves the highest
sensitivity. In Variation B, a larger quantity of phosphoric acid is added to yield a pH of 1.2±0.1
in the final solution. The wavelength of maximum absorbable under these conditions is 575 nm,
and the compound has a molar extinction of 37.0 x 103, assuming quantitative production of
absorbing Species.
Variation B is less sensitive, but has the advantage of a tower blank. It is PH dependent, and
may be more suitable with less expensive spectrophotometers.
2. 0 Range and Sensitivity:
2.1 Atmospheric sulfur dioxide concentrations are measurable by this technique in the range
from 10 ppbv to a few ppmv. Use smaller gas samples when analyzing higher concentrations (S
to 500 ppmv), found in special studies. A rapid redox reaction occurs between Hg (11) and the
sulfite ion if concentrations of th latter exceed 500 μg/ml (8). Collection efficiency falls off

rapidly below 100 pubs, and varies with the geometry of the absorber, the size of the gas
bubbles, and the contact time with the solution (9,10,11).
2.2 The lower limit of deletion of sulfur dioxide in 10 ml- of TCD is 0.3 μL (based on twice the
standard deviation representing a concentration of 10 ppbv (26 μg/m3) SO2 in an air sample Of
30 l-. One cannot extrapolate to lower values by taking larger volumes of air (e.g. 100 L at 3
qpbv). The method is only applicable to concentrations below 10 ppbv lf the absorption
efficiency of the particular System is determined.
2.3 Beer's Law is followed through the working range from 0.1 to 1.0 absorbance units (0 to 35
μg in 25 ML final solution).
3.0 Inferences:
3.1 The effects of the principal potential interferences (oxides of nitrogen, ozone and transition
metals (e.g. iron, manganese, and chromium) have been minimized or eliminated. The
interferences by oxides of nitrogen are eliminated by sulfuric acid (5,6), the ozone by time delay
(4), and the transition metals by EOTA and phosphoric acid (4,5). At least 60 pg of V (V) in 1.0 ml
of absorbing reagent cause no interference.
4.0 Precision and Accuracy:
The precision at the 95% confidence level is 4.6% (5).
5.0 Apparatus:
5.1 ABSORBER - Satisfactory absorbers are (a) the midget or standard fritted bubbterthe midget
impinger; (c) the Greenberg-smith impinger; and (d) the multiple jet bubbler (12).
5.2 AIR VOLUME MEASUREMENT- Re sample air volume must be measured within + 2%. See
Section 5 of Part I for details of air volume measurement. A critical orifice is recommended (13).
5.3 SPECTROPHOTOMETER OR COLORIMETER - The instrument must be suitable lot

measurement of color at 548 nm or 575 nm. With Variation A. reagent blank problems mar
result with Spectrophotometers or calorimeters having greater spectral band width than 16 nm.
The wavelength calibration of the Spectrophotometer should be verified.
6.0 Reagents:
6.1 PURITY OF CHEMICALS - All chemicals must be ACS analytical reagent grade. The
pararosaniline dye should meet the specifications described in 6.9.
6.2 WATER - Water must conform to the ASTM Standard for Reference ' Reagent Water Water.
Type 11. This can be produced either by distillation or a cartidged deionization system.
6.3 ABSORBING REAGENT 0.04 M POTASIUM TQ7XACI|LOROMERCURAW
(TCM), K2HgCI2- Dissolve 10.86 j mercuric chloride (CAUTION: Highly poisonous and corrosive.
If spilled on skin, flush off with water immediately): 5.96 g of potassium chloride and 0.066 g of

EDTA in water and bring to mark in a I-L volumetric flask, Sodium chloride, but potassium
chloride is usually available in purer form. The pie of this a reagent should be 4 ±1 ( 14). The
absorbing reagent is normally stable for six months, but if a precipitate forms, discards the
solution.
6.4 SULFAMIC ACID (0.6%)- Dissolve 0.6 g of sulfuric acid in 100 my Of water. This reagent can
be kept for 10 days if it is stored in a stoppered bottle.
6.5 BUFFER STOCK SOLUIRON (PH 4.7). In a 100 IML volumetric black, dissolve 13.61 g of
sodium acetate tri-hydrate in water. Add 5.7 ml of glacial acetic acid and dilute to volume with
water.
6.6 1.0N HYDROCHLORIC ACID. Dilute 83 ml of 12.1M acid (36% HCI) to 1 L.
6.7 3M PHOSPHORIC ACID (H3PO4) to IL. Dilute 83 ml of 12.1M acid (36% HCl) to 1L.
6.8 BUTANOL. 1-Butanol is required for the purification Of the pararosaniline dye. The butanes
should be checked for oxidants that can consume SO:. Check it by shaking 20 ml of 1-butanol
with 5 IML of 20% aqueous Kl. A yellow color in the alcohol phase indicates tine presence of
oxidant and the butanes must be redistilled from silver oxide.
6.9 PURIFIED PARAROSANILINE 0.2 % (NOMINAL) STOCK SOLUTION Pararosaniline dye needed
to ' ' prepare this reagent must meet the Following performance specifications. The dye must
have a wavelength of maximum absorbency of 540 nm when essayed in 0.1M sodium acetate-
acetic acid buffer the assonance of the reagent blank (section 7.3), which is temperature
sensitive (0.o1sA.wc), should not exceed 0.170 absorbency unit at 22*c; and the reagent should
give a calibration curve with a slope of 0.746 z 0.04 assonance units (μg SO2, mL) for a 1-cm
cell. Prepare a solution of the dye; weigh 0.200 g and completely dissolve by shaking with 100
my of 1N HCl In a 100 ml glass stoppered graduated cylinder. If the pararosaniline dye is
obtained in purified form as ozone solution, proceed to 6.9.5. Specially purified dye, 0.2% in 1N
HCI solution, is available from Eastman Kodam, J.T. Baker or Harleco.
6 .9.1 Dye Purification Procedure. The pararosaniline dye (PRA) is purified by extraction of
impurities into 1-butanol. In a 250 ml separating funnel shake 100 ml each of 1-butanol and 1 N
HCI and allow the layers to separate. Collect each layer separately. Add 0.1 g of pararosaniline
to 50 ml of the butanol-saturated acid and allow it to stand for several minutes. Add this acid
pararosaniline solution to 50 ml of acid-saturated 1-butanol in a 12S my separation funnel. The
impurities violet coloured, will be transferred to the phase. Save the lower (aqueous) phase and
extract again with 20 ML of 1-butanol. Repeat this procedure three times using 10 ml portions
of 1-butanol. If a violet color still appears in the l-butanol after 5 extractions, filter the aqueous
phase through a glass wool plug into a 50 ml volumetric flask and bring to volume IN HCI. The
final solution is nominally 0.2% pararosaniline in 1N HCI saturated with l-butanol.
6.9.2 1.0 M Sodium Acetate - Acetic Acid Buffer. Dissolve 57.3 my glacial acetic acid and 136 g
sodium acetate dehydrate in water and make up to the mark in a 1-L volumetric flask. .
6.9.3 Assay Procedure. The concentration of PRA need be assayed only once for each lot of dye
in the following manner: Dilute 1 my of the stock reagent (0.2%) to the mark in a 100-mL
volumetric flask with distilled water. Transfer a 5-mL aliquot to a 50 my volumetric flask. Add 5

ml if IM sodium acetate-acetic acid buffer, and dilute the mixture to 50 ml with water. After 1 h.
determine the assonance at 540 nm with a spectrophotometer.
6.9.4 Pararosaniline Reagent. To a 250-mL volumetric cask add 20 my of stock pararosaniline

reagent. Add an additional 0.2 ml of stock for each percent the stock assays below 100%. For
Variation A, add 25 ml of am H z PO4 and dilute to volume with water. For Variation B, add 2|0
ml of am HaPO4 and dilute to volume. These reagents are stable for at least 9 months.
6. 10 FORMALDEHYDE, 0.2%. Dilute 5 my of 37% formaldehyde to 1 L with water. Prepare daily.
6. 11 REAGENTS FOR STANDARDISATION.
6. I 1.1 Stock iodine Solution, 0.1 N. Place 12.7 g of iodine in a 250 ml beaker, add 40 gm. of
potassium iodide and 25 my of water. Stir until all the solid is dissolved, then dilute to 1 L with
water. If desired, prestandardized solutions of iodine can be purchased from laboratory supply
dealers. (a) Working Iodine Solution, 0.01N: Prepare approximately 0.01N iodine solution by
diluting 50 ml of the stock solution to 500 ml with distilled water.
6.11.1 Starch Indicator Solution. Triturate 0.4 g of soluble starch and 0.002 g of mercuric iodide
(preservative) with a little water and add t the paste slowly to 220 ml of boiling water. Continue
boiling until clear; cool and transfer to a glass stoppered bottle. If the Indicator solution is only
going to be kept for few days, omit the mercuric iodide.
6.11.2 Standard O.IN. Sodium Thiosulfate Solutlon. 2 Dissolve 25 g of sodium thiosulfate

(Na2S2O3 - 5 H2O) in IL of freshly boiled, cooked distilled water and add 0.1 g of sodium
carbonate to the solution. Allow the solution to stand for one day before standardizing. To
standardize accurately weigh 1.5 g of potassium iodate. primary standard grade, that was dried
at 180 C, and dilute to volume in a 500-mL volumetric flask. Into a 500-mL of the iodate
solution. Add 2 g of potassium iodide and 10 ml of a 1: 10 dilution of concentrated hydrochloric
acid. Stopper the flask. Acer 5 minutes, titrate with thiosulfate to a pale yellow color. Add 5 my
of starch indicator solution and complete the titration.
Normality of Thiosulfate = Wt. (grams KlO3) x 2.804

------------------------------------
ml of thiosulfate
Prestandardized solutions of sodium thiosulfate can be purchased from laboratory supply

dealers.
6 . 1 1 . 3 Standard Sulfite Solution.-Dissolve 0.400 g of sodium sulfite (Na2SO2) or 0.300 g of

sodium metabisulfite (Na2S2O3) in 500 (oil reagent quality de-aerated water. For a reagent
purity of 100% and no loss of sulfite in making up the solution, the respective So2 content of
this solution will be 406 μg/ml- (for Na2S2O3) and 404 μg/ml (Na2S2O5 as SO2) . In practice,
S02 concentration will be 0 to 10% below the theoretical value. If this level of uncertainty is
acceptable it is not necessary to standardize the sulfite solution. To minimize loss of Sulfite, the
diluted sulfite solution should be prepared immediately as indicated in 6.10.5. The actual
concentration of sulfite in the standard solution can be determined by adding excess iodine and
back-titrating with sodium thiosulfate that has been standardized by iodometric titration
against potassium iodate or dichromate (primary standard). Aqueous solutions of sulfite are

unstable due to air oxidation of of the Sulfite or loss of volatile SO2.
a) Back-titration is performed in the following manner: in to each of two 500 ml Erlenmeyer

flasks with ground glass stoppers pipette accurately 50 ml of the 0.01N iodine. Into flask A
(blank) add 25 ml of distilled water, and into flask B (sample) pipette 25 ml of the standard
sulfite solution. Stopper the casks and allow to read for 5 minutes. By means of a burette
containing standard 0.01N thiosulfate, titrate each flask, in turn, to pale yellow color. Then add
5 ml of starch solution and continue the titration to the disappearance of the blue color.
Calculate the concentration of sulfur dioxide in the standard solution as follows:
(X - Y) NZ
SO2 (μg/mI) = ----------------
S
Where:
X = number of mL for blank,

Y = number of mL for sample,
N = normality of thiosulfate solution,
Z = micro-equ|valent weight for SO2, 3.203 x 10*
S = sample volume taken in mL.
6.11. Dilute Sulfite Solution. Immediately after standardization of sulfite solution or

preparation of an acceptable unstandardized solutions pipette accurately 2 ml of the freshly
standardized solution into a 100 ml volumetric flask and bring to lark with 0.04M TCM. The
solution is stable for 30 days if stored at 5 C.
7.0 Procedure:
7.1.1 COLLECTION OF SAMPLE. Place 10 my of 0.04M TCM (20mL for sampling of long duration)
absorbing solution in a fidget impinges or 75 to 100 mL in a larger absorber. The sampling
probe-to-absorber linkage will depend on the installation. This should be kept as short and
direct as possible using glass or Teflon tubing. Care must be taken to avoid condensation in the
sample Inlet, which can occur when warm humid air is brought In to an air conditioned location.
After the absorber, a trap, such as a flask tightly packed with glass wont, should be placed to
prevent corrosion damage to downstream components from aerosolized TCM droplets, which
are highly corrosive. Provision must be made for the flow volume measurement farther
downstream of the absorber. The duration of sampling will depend on the concentration of
SO2. With midget impingers, rates of 0.5 to 2.5 L/min are satisfactory; with large absorbers the
rate can be 5 to 15 L/min.
Rates of sampling within the above ranges generally have absorption efficiency of 98% or
greater. For best result, rates and sampling tinge should be chosen to absorb 0.5 to 30 μg/ml-
of SO2. Shield tile absorber from direct sunlight by covering with a suitable wrapping. If the
sample must be stored for more than a day before analysis, keep it at S C, if possible.
7.1.2 CENTRIFUGATION. If a precipitate is observed, remove it by centrifugation.
7.1.3 ANALYSIS. Acer collection, transfer the sample quantitatively to a 25ml volumetric flask;
use about 5 ill of water for rinsing. Liquors may be taken, at this point, if the concentration or

volume of reagent is larger. If the sample has been freshly collected, decay analyses for 20 min
to allow any ozone present to decompose. For each set of determinations. prepare a reagent to
a 25-mL volumetric flask. To each flask add 1 ml 0.6% sulfuric acid and allow to read for 10 min
to destroy the nitrite from oxides of nitrogen. Accurately pipette in 2 ml of the 0.2%
formaldehyde, then 5mL of pararosanline reagent prescribed for Variation A or Variation B.
Start a laboratory timer that has been set for 30 min. bring all flasks to volume with freshly
boiled water. After the 30 min. determine the observances of the sample and of the blank at
the wavelength of maximum absorbency, 48 nm for Variation A or 575 nm for Variation B. Use
waer (not the reagent blank) in the reference cell. Do not allow the colored solution to stand in
sample absorbency cell; a film of dye will be deposited on the cell windows.
7.1.4 If the assonance of the sample solution ranges between 1.0 and 2.0, the sample can be
diluted 1: l with a million of the reagent blank and read within a few minutes. Solutions with
higher absorbency retire the diluted up to six-fold with the reagent blank in order to obtain of')
artists readings within 10% of the true assonance value.
7. 1.5 An automated procedure can be used as an alternative to manual addition of reagents

and calorimetric analysis (15).
8.0 Calibration and Standards:
8. 1 Accurately pipette graduated amounts of the diluted sulfite solution (such as ) 0, 1, 2, 3, 4,

and 5 mL) into a series of 25-ml volumetric flasks. Add sufficient 0.04M TCM to each flask to
bring the volume to approximately 10 mL. Then add the remaining reagents as described in the
procedure. For greatest precisian a constant temperature bath is preferred. The temperature of
calibration should not differ from the temperature of analysis by more than a few degrees.
8.2 The total observances of the solutions are plotted (as ordinates) against the total
micrograms of SO2. A linear relationship is obtained. The intercept with the vertical axis of the
line best little: the points usually is within 0.02 absorbency units of ''the blank (zero standard)
reading. Under these conditions the plot need be determined only once to evaluate the
calibration factor (reciprocal of the slope of the line). More accurate values of slope and
interceipt can be obtained by linear regression. This calibration factor can be used for
calculating results provided there are no radical changes in temperature of pH. At least one
control sample is recommended per series of determinations to ensure the reliability of this
factor.
8.3 ALTERNATIVE CALIBRATION PROCEDURE.
Permeation tubes containing liquefied sulfur dioxide are calibrated gravimetrically and .used to
prepare standard concentrations of sulfur dioxide in air (16-18). Sampling of these known
concentrations and subsequent analysis of collected samples give calibration curves that
simulate all of the operational conditions during the sampling and analytical procedure. Such
calibration curves include the important correction for collection efficiency at various
concentrations of sulfur dioxide. For details on the use of permeation tubes as calibration
sources see Section 3, Part 1.

9. Effects of Storage:
Solutions of monochlorosulfonatomtxrcura|e (11) are Sable towards the loss of SO2 when
stored at 5 C for 30 days. At 25 C toeless of SO2 ranges from 1-5% per day (3, 19, 20). These
losses of SO2 follow a first order reaction; the rate constant is independent of concentration.
For storage of samples under conditions where SO2 loss may be important, e.g., without
refrigeration correction factors must be applied. Alternatively, an increase In the Cl
concentration will improve the stability of the monochtorosulfonatomercurate (11) species
(3.19). This modification leads to some difficulties in sampling and a loss of sampling efficiency.
Thermoelectrically cooled enclosures for housing the absorber vessels during or after sampling
are commercially available from RAC, Division of Andersen samplers, Inc. Atlanta, ' Georgia.
Calculations:
Compute the concentrations of sulphur dioxide (SO2), in units of μg/m3 in the sample by using
the following formula:
(so2) (μg/m3) = (A - Ao ) x B
----------------
V
Where
A = the sample absorbable

Ao = the reagent blank absorbable
B = calibration factor, μg/ assonance
V = air sample volume m3 calculated using Eq (3) as given at the beginning of section 6.
The concentration of SO2 in units of ppm (Volume) is given by (SO2) (ppmv) = (SO2) (μg/m3) x
0.000382,
Where 0.000382 = the volume (mI) of 1 μgSO2 at STP (25 deg C. 101.3 kpa).

EXPERIMENT-16
Batch Sedimentation Apparatus
Aim:
1. To plot a graph between the height of interface (z) and time (θ) for slurries having five
different concentration of CaCO3.
2. To plot settling rate (dz/dθ)θ=0 vs initial concentration (C0).
Introduction:
The suspension of dilute slurry by gravity settling into a clear liquid and slurry of higher solid
concentration is known as sedimentation. The mechanism of sedimentation observed during a
batch settling set is shown in figure.
As sedimentation continues, the height of each zone varies as indicated in the figure. Both A
and D grow larger at the expense of B and ultimately zone B & C disappear and all the solids
appear in a D. This is known as critical settling point. The same zones shall be present in a
continuous thickner.
Batch sedimentation tests are used to determine the settling characteristics of a slurry/sludge.
The analysis is further used for the design of continuous thickner.
Theory:
For any batch sedimentation experiment, on slurry of known concentration, the height of a
liquid-solid interface is obtained as a function of time. Slopes of this curve at any point of time
represent settling velocities of the suspension at that time and are characteristics of specific
solid concentration.
Utilities Required:
1. Graduated Cylinders (1 m long, 50 mm dia.)
2. Stop watch
3. CaCO3 (Calcium Carbonate)
Prepare five samples of CaCO3 slurry in each cylinder. Mix the samples thoroughly before
starting the experiment so that homogeneous slurry is obtained in each case. Note the initial
height (z0). Start recording the time and interfacial height in each of the graduated cylinder
separately continue to take the record till height of interface stops any further. Note the final
height (z∞).

Observation Table & Calculation:
Concentration (C0, gm/L)
Time (θ) seconds Height of Interface z1 (cm)
Plot all the curves z vs θ. Find the slope of initial settling rates (dz/dθ)θ=0 for each concentration
(C0) and plot on a log-log graph.

EXPERIMENT NO.: 17
NAME OF EXPERIMENT: Deep Bed Filter Column
Aim:
To study the characteristics of a deep bed filter column using 50 to 150 mg/l kaolin suspension
in water.
Introduction:
Slow sand filters have been used to remove particles from drinking water since early 1800’s.
The particles that are captured on slow sand filters have been shown to significantly improve
filter performance.
Theory:
In slow sand filters with clean filter media, particles are initially removed by attaching to the
filter media. However, as the filter media begins to be covered with removed particles, particles
begin to attach to previously removed particles. If particle-particle interaction is more favorable
than particle-media interaction then particle removal efficiency increases as the media
becomes covered with particles. This improvement in filter performance with time is commonly
observed in slow sand filters and is referred to as filter “ripening”. Filter ripening often takes
several weeks to several months for new slow sand filters.
Filteration theory suggests that particle removal will be first order with respect to depth if filter
media is homogeneous. In equation from the relationship between particle concentration, C,
and depth can be expressed as:
dC/dz = -λC …………………………………(1)
Where, λ is the filter coefficient with units of [1/L]. Using appropriate limits
C0 0
 dC/C = -λ  dz ……………………………..(2)
C L
Where, L is the depth of the filter bed and C0 is the influent particle concentration and
integrating Eq (2) yields:
Ln C/C0 = -λL ………………………………(3)
Eq (3) can be used to evaluate the filter coefficient, λ.

Table 1: Typical values of filter co-efficient, λ
Filter Grain Size Particle Particle Size Approach Velocity λ

Medium (mm) Type ( µm) (cm/hr) (1/cm)
Calcium LR Ferric floc 10 500 0.1

Carbonate Grade
Calcium LR Ferric floc 10 1000 0.044
Carbonate Grade
Anthracite 0.77 Quartz 2-22 500 0.064
powder
Sand 0.54 Chlorella 5 500 0.34
Sand 0.647 Fuller’s 6 470 0.363
earth
Granular 0.594 Clay 4-40 500 0.102
carbon
Evaluation of Filter Performance:

Several measurement techniques could be used to characterize filter performance. Particle
concentrations could be measured using a particle counter, or measured indirectly using a
turbidimeter. If the particle suspension absorbed a significant amount of light, a
spectrophotometer could be used. A microscope could be used to count particles.
Turbidimeters measure the amount of light scatter caused by a suspension of particles. Because
absorption and scattering of light are influenced by both size and surface characteristics of the
suspended material, turbidity is not a direct quantitative measurement of the concentration of
suspended solids. In a turbidimeter the scattered light and the transmitted light is proportional
to the turbidity of the sample. The constant of proportionality is determined by measuring a
known standard.
1. Before the start of experiment, prepare a calibration curve using standard solutions of
kaolin in water ( 50 mg/L, 20 mg/L, 10 mg/L, 8 mg/L, 6 mg/L, 4 mg/L, 2 mg/L, 1 mg/L)
and measure the absorbance in terms of NTU in a turbid meter and plot the calibration
curve.
2. Prepare kaolin suspension in water in the range of 50 to 150 mg/L in the feed tank. Keep
the solution under constant stirring.
3. If the filter bed has been previously used, then using backwash mode use clean water to
wash the bed. Carefully observe the sand surface as you gradually increase the flow rate
from zero in backwash mode. Continue backwashing the filter to clean the sand until the
effluent turbidity is less than 0.5 NTU.
4. Obtain head loss (in cm) as a function of flow rate of pure clean water over a range of 1
to 25 m/hr using at least 5 data points. Use the rotameter to measure the flow rate..
5. Set the down flow rate to 5 m/hr.

6. Pump a clay suspension into the filter influent so that the influent concentration is in
the range of 50 to 150 mg/L. Measure the effluent turbidity and head loss as a function
of time for 30 minutes. Take turbidity measurements every 5 minutes and measure the
head loss.
7. Backwash the filter.
Data:
Tap No. Height (mm) Tap No. Height (mm)

1. 50 22. 470
2. 70 23. 490
3. 90 24. 510
4. 110 25. 530
5. 130 26. 550
6. 150 27. 570
7. 170 28. 590
8. 190 29. 610
9. 210 30. 630
10. 230 31. 650
11. 250 32. 670
12. 270 33. 690
13. 290 34. 710
14. 310 35. 730
15. 330 36. 750
16. 350 37. 770
17. 370 38. 790
18. 390 39. 8910
19. 410 40. 830
20. 430 41. 1150
21. 450
Filteration Parameters
Parameter Symbol Value Units
Column Diameter D 10 cm
Column Area A 78.5 cm2
Column Length L column 120 cm
Media depth L 135 cm
Bulk Density of Media Bulk density 145 kg/m3
Mass of Media Sandmass 11 kg
Influent Clay Concentration C0 In the range of 50 to Mg/L
300

Observation Table:
S. No. Time Concentration (mg/L) Pressure (mm of water column)

. h1 h2 h3 Upto h M1 M2 M3 Upto
41 M 41
1.
2.
3.
4.
Data Analysis:
1. Plot head loss vs. flow rate for a clean bed and estimate the hydraulic conductivity of
the sand.
2. Plot head loss at different depths.
3. Plot the fraction of influent particles remaining in the effluent vs. time and vs. depth for
each run on a single graph.
4. Plot head loss as a function of time foe each run on a single graph.
5. Calculate the filter coefficient (Eq (3)) for the filter with and without the filter aid.

REFERENCES
1. Muralikrishna, KVSG “Chemical analysis of water and soil”, Environmental protection
society, Kakinada, A.P., 1999.
2. Kotaiah, B. Kumara swamy, N “Environmental Engineering Lab Manual” Chartor
Publishing House, Anand, 1994.
3. Mathur, RP “Water and wastewater testing (A laboratory Manual)” New Chand & Bros
(Publishers) Roorkee, 1992.
4. Sudha Rani “Laboratory Manual on Engineering Chemistry” Dhanpat Rai Publishing
Company, 2001.
5. Bailey, JE and Ollis, DF “Bio chemical Engineering Fundamentals” 2nd Ed, Mc Graw –Hill,
1986.
6. Aiba, S, et al. “Biochemical Engineering” 2nd Ed. Academic Press, 1973.
7. Peavy, HS et al. “Environmental Engineering” Mcgraw-Hill, 1985.
8. Deory et al. “Laboratory scale equipment for the determination of kLa in Bio-reactors –
Bioprocess Engineering” pp. 73-75, Springer- Verlag, 1999.

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LABORATORY MANUAL

Mr. SHIVA SHANKAR Y (ASSISTANT PROFESSOR)

Mr. M.L. RATHORE (LAB ENGINEER)

DEPARTMENT OF CIVIL ENGINEERING

Department of Civil Engineering, JUET Guna (M.P.): 1

1 pH, Turbidity, Electrical Conductivity 3–9

Department of Civil Engineering, JUET Guna (M.P.): 2

Aim: To determine pH of the given water samples.

Conc. of H ions × Conc. of OH ions/ Conc. of un-dissolved HOH molecules

For convenience pH scale is taken from 0 to 14.

pH of a liquid sample can be determined either by:

(i) Coloumetric method or use of indicators (ii) Electrometric method

Electrometric method of pH determination:

It is determined through a instrument by electrolysis and dissociation of H+ and OH- radical,

Department of Civil Engineering, JUET Guna (M.P.): 3

The pH of water can be found in the following manner.

1. Knowing pH value is very important parameter for analysis of water/wastewater and

Department of Civil Engineering, JUET Guna (M.P.): 4

Results and Conclusions:

EXPERIMENT NO.: 1(b)

Department of Civil Engineering, JUET Guna (M.P.): 5

Aim: To find out Turbidity of the given sample.

1. Nephelometric Turbidity meter

1. Dissolve 1 g of Hydrazine sulphate and dilute to 100 ml

Department of Civil Engineering, JUET Guna (M.P.): 6

Sl No. Sample details Turbidity (NTU) Remarks

Results and Conclusions:

Department of Civil Engineering, JUET Guna (M.P.): 7

NAME OF EXPERIMENT: ELECTRICAL CONDUCTIVITY

Apparatus: Conductivity Meter, Beakers, Thermometer.

Reagents: 0.1N KCl

1. Switch on the conductivity meter for 15 minutes.

Department of Civil Engineering, JUET Guna (M.P.): 8

S.No. Description of Temperature Conductivity Remarks

Results and Conclusions:

Department of Civil Engineering, JUET Guna (M.P.): 9

NAME OF EXPERIMENT: ACIDITY

1. Standard sodium hydroxide (0.02N).

Department of Civil Engineering, JUET Guna (M.P.): 10

1. Acidity interferes in the treatment of water especially water softening.

Sl. Sample Sample Methyl Orange Indicator Phenolphthalein indicator

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

Results and conclusions:

Department of Civil Engineering, JUET Guna (M.P.): 11

NAME OF EXPERIMENT: ALKALINITY

Aim: To determine the Alkalinity of the given water samples.

1. Burette 2. Pipettes 3. Conical flask

1. Standard sulphuric acid (0.02 N)

1. Take 100 ml of the given water sample in a conical flask.

Department of Civil Engineering, JUET Guna (M.P.): 12

Serial Sample Sample Phenolphthalein indicator Methyl Orange Indicator

Value of P and T Alkalinity (mg/l) as CaCO3 due to

1. Phenolphthalein alkalinity (P) (mg/l) as CaCO3

2. Total alkalinity (T) (mg/l) as CaCO3

Results and Conclusions:

Burette, pipette and conical flask.

1. Chloride free distilled water.

2. Potassium chromate (K2CrO4) colour indicator

3. Standard silver nitrate solution (0.0141 N)

4. Standard sodium chloride solution (0.0141 N)

1. Take 100 ml of sample in conical flask.

Department of Civil Engineering, JUET Guna (M.P.): 14

S. Sample details Volume of Observations Chlorides