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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

ACHARYA INSTITUTE OF TECHNOLOGY


(AFFILIATED TO V.T.U., BELGAUM)

DEPARTMENT OF CIVIL ENGINEERING

VII SEMESTER
06 CVL 77

ENVIRONMENTAL ENGINEERING
LABORATORY MANUAL

ACADEMIC YEAR: 2013 - 2014

NAME OF THE STUDENT:____________________________

UNIVERSITY SEAT NO. :____________________________

BATCH :____________________________

PREPARED FOR INTERNAL CIRCULATION ONLY

DEPARTMENT OF CIVIL ENGINEERING ACHARYA INSTITUTE OF TECHNOLOGY


ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

INSTRUCTIONS

1. This laboratory manual is ONLY for reference for those using the environmental
engineering laboratory.

2. Discussion after each experiment should be based on the following points:

(a) Limit prescribed for that constituent in drinking water standards.


(b) The suitability of the sample for drinking purpose with respect to that particular
constituent.

3. To Note:

(a) In water and wastewater analysis, the results are usually reported in terms of
mg/l of some particular ion, element or compound. It is most convenient to have
the standard titrating agent of such strength, that 1mL is equivalent to 1mg of
material being measured. Thus 1 litre of the standard solution is usually
equivalent to 1g of the standard substance.
(b) Rules listed by Worthing and Geffner are to be followed while plotting graphs.

4. Users may refer the following for writing the discussion after each experiment:

(a) “Standard Methods for the Examination of Water and Waste Water”, American
Public Health Association, 1015, 15th Street, N.W., Washington D.C., 2005.
(b) “Chemistry for Environmental Engineers”, Sawyer and McCarty, Tata Mc-Graw
Hill.
(c) “Manual of Standards of Quality for Drinking Water Supplies”, Indian Council
of Medical Research, New Delhi.
(d) “International Standards for Drinking Water” — World Health Organisation.
(e) “IS 2490 - 1981, IS 3306 - 1974, IS 3307 - 1977, IS 7968 - 1976, IS 2296 –
1974”, Bureau of Indian Standards, New Delhi.

DOS AND DONOT’S IN THE LABORATORY

1. Do thoroughly clean the glassware before and after use.


2. Do handle the glassware carefully.
3. Do not handle chemicals with bare hands.
4. Do not blow out the last drop from the pipette. When the liquid has drained out
completely, touch the tip of the pipette to the inner surface of the vessel.
5. Do not add water to acids. Do always add acid to water.
6. Do use large volumes of water, when a person is splashed with acid to prevent serious
burns.
7. Do weigh the articles in a balance only at room temperature.
8. Do use different pipette for different reagents.
9. Do not pipette out acids and other toxic reagents by mouth.
10. Do read the level of the curve (meniscus), in all volumetric glassware, with the eye at
approximately the same level as the curve of solution.

DEPARTMENT OF CIVIL ENGINEERING ACHARYA INSTITUTE OF TECHNOLOGY


ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

List of The Experiments Faculty


Signature

01 Determination of Solids in sewage: Total Solids, Suspended Solids,


Dissolved Solids, Volatile Solids, Fixed Solids and Settleable Solids.

Determination of Electrical Conductivity of water.


02
Determination of Chlorides and Sulphates.

Determination of Alkalinity.

03 Determination of Acidity.

Determination of pH.

Determination of Calcium and Magnesium Hardness.


04
Determination of Total Hardness.

Determination of Dissolved Oxygen.


05
Determination of BOD.

Determination of COD.
06
Determination of Percentage of Available Chlorine in Bleaching Powder.

07 Determination of Residual Chlorine for water.

Determination of Chlorine Demand for water.

Determination of Turbidity by Nephelometer.


08
Jar Test for Optimum Dosage of Alum.

Determination of Iron by Phenanthroline method.


09
Determination of Fluorides by SPADNS Method.
10

11 MPN Determination.

Determination of Nitrates by Spectrophotometer.


12

13 Determination of Sodium and Potassium by Flame Photometer.

Name & Signature of Faculty In-charge Head of the Department

DEPARTMENT OF CIVIL ENGINEERING ACHARYA INSTITUTE OF TECHNOLOGY


ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Preview

Concurrent with the evaluation of environmental engineering practice, analytical methods


have been developed to obtain the factual information required for the resolution and
solution of problems. Environmental engineering is perhaps most demanding in this
respect, for it requires the use of not only the conventional measuring devices employed by
engineers but, in addition many of the techniques and methods of measurement used by
chemists, physicists and some of those.

The objective of sampling is to collect representative sample. Representative sample by


means a sample in which relative proportions or concentration of all pertinent components
will be the same as in the material being sampled. Samples ought to be handled in such a
way that no significant changes in composition occur before the tests are made. The
sample volume shall optimal small enough that it can be transported and large enough for
analytical purposes. Grab samples are single collected at a specific spot at a site over a
short period of time. Composite samples provide a more representative sampling and can
be obtained by combining portions of multiple grab samples or by using specially designed
automatic sampling devices. Integrated samples are obtained by analyzing mixtures of grab
samples collected from different points simultaneously. The type of sample containers
used is also of utmost importance. Containers typically are made of plastic or glass, but
one material may be preferred over the other. Because of variability from analytical and
sampling procedures (i.e., population variability), a single sample is often insufficient to
reach any reasonable desired level of confidence. If an overall standard deviation (i.e. the
standard deviation of combined sampling and analysis) is known, the required number of
samples for water may be estimated.

Complete and unequivocal preservation of samples, whether domestic wastewater,


industrial wastes, or natural waters, is a practical impossibility because complete stability
for every constituent never can be achieved. At best, preservation techniques only retard
chemical and biological changes that inevitably continue after sample collection. If
immediate analysis is not possible, preferably store at 4°C. No single method of
preservation is entirely satisfactory; choose the preservative with due regard to the
determinations to be made.

STANDARDS FOR DRINKING WATER

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Experiment No.: 01 Date: ..../..../…...

SOLIDS IN WASTE WATER

Aim

Determination of Solids in sewage: Total Solids, Suspended Solids, Dissolved Solids,


Volatile Solids, Fixed Solids and Settleable Solids.
Apparatus
China dish of 150–200 ml capacity, Muffle furnace, hot air oven, digital balance, filter
paper, Imhoff cone, conical flask, Desiccators.

Theory

One of the most important characteristics of sewage is the solid content. Sewage
normally contains 99 % water and 1% solids. Solids test is an important parameter as it is
used in:

1. Design of biological units and water pollution control methods, which depend on the
concentration of organic solids.
2. In Grit chambers and sedimentation tank design which depends on the quantity of
inorganic and organic settleable solids respectively.
3. Dissolved inorganic solids are to be considered in the design of land treatment of
Sewage.

Classification of Sewage Solids:

Total solids: Analytically the total solids content of a wastewater is defined as all the
matter that remains as residue on evaporation at 103°C and subsequent drying. These
solids are very important as they indicate the strength of sewage and amount of treatment
required.

Total solids in wastewater exist in 3 forms:

Dissolved solids, Colloidal solids and Suspended solids.

Dissolved solids are those which remain dissolved in sewage just as salt in water and are
generally organic in nature causing putrefaction and thus increasing the strength of
sewage and creating nuisance if disposed off untreated. Colloidal solids are finely divided
solids remaining either in solution or in suspension.

Suspended solids are those, which are in suspension and are floating in sewage.

These are further classified into:

• Settleable solids, which settle down at the bottom of an Imhoff cone and are an
approximate measure of the quality of sludge that will be removed by sedimentation.

• Non settleable solids are those, colloidal in nature and can be removed by Chemical
treatment.

Fixed solids: Fixed solids are also called inorganic solids consisting of minerals and salts,
which include sand, gravel, debris, dissolved salts etc. They constitute about 55°/o of the
total solids and are not harmful in sewage treatment operations and require only
mechanical appliances such as screens for their removal.

Volatile solids: They are also called organic solids or ignited solids, consisting of organic
matter such as carbohydrates, fats, oils etc and constitute about 45% of the total solids
and commonly used in the analysis of wastewater sludge's to measure their biological
stability.

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Procedure

a] Total solids
1. Ignite the clean evaporating dishes in the muffle furnace for 30 minutes at 550°C and
cool in a desiccator.
2. Note down the empty weight of the dish (W1).
3. Pour a measured portion (50 to 100 ml) of the well-mixed sample into the dish and
evaporate the contents by placing the dish on a steam bath.
4. Transfer the dish to an oven maintained at either 103–105°C or 179–181°C and dry it
for 1 hour.
5. Allow the dish to cool briefly in air before placing it, while still warm in a desiccator to
complete cooling in a dry atmosphere.
6. Weigh the dish as soon as it has completely cooled (W2).
7. Weight of residue = WT = (W2 – W1) mg. [W2 and W1 should be expressed in mg.]

b] Total Fixed Solids

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

c] Total Dissolved Solids

1. Filter a measured portion of the mixed sample (50 or 100 ml) through a Whatmann
filter paper (No 44).
2. Heat and collect the filtrate in a previously prepared and weighed evaporating dish at
103 °C for 1 to 1.5 hours in a hot air oven and weigh the residue.
3. Allow the dish to cool briefly in air before placing it, while still warm in a desiccator to
complete cooling in a dry atmosphere.
4. Weigh the dish as soon as it has completely cooled (W5).
5. Weight of total dissolved solids = WD = (W5 – W4) mg.

Where,
W4 = Weight of empty evaporating dish in mg.
W5 = Weight of empty evaporating dish in mg + Residue left after evaporating the
filtrate in mg.

d] Total Suspended Solids = Ws = Total Solids – Total Dissolved Solids.

e] Total Volatile Solids = WV = Total Solids – Total Fixed Solids.

f] Settleable Solids (by volume) [WSS]

1. Fill an imhoff cone (lit capacity, graduated up to 40ml) to the litre mark with a
thoroughly mixed sample.
2. Allow to settle for 45 minutes.
3. Gently stir the sides of the cone with a rod a few times to ensure that all solids
adhering to the sides is loosened.
4. Allow to settle for further 15 minutes.
5. Record the volume of settleable matter in the cone as ml/l.

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Observations, Calculations and Results

Parameter Label Unit Result


Volume of sample taken V ml
Total solids
Weight of clean empty evaporating dish W1 mg
Weight of china dish after it has completely W2 mg
cooled with residue of sewage sample oven
dried at 103°C
Total Solids WT = W2 – W1 mg
Total Solids (per ml of sample) [WT x 103] / V mg/l

Total Fixed Solids


Weight of clean empty evaporating dish W3 mg
Total Fixed Solids WF = W3 – W1 mg
Total Fixed Solids (per ml of sample) [WF x 103] / V mg/l
Total Dissolved Solids
Weight of clean empty evaporating dish W4 mg
Weight of china dish after it has completely W5 mg
cooled with residue left after evaporating the
filtrate.
Total Dissolved Solids WD = W5 – W4 mg
Total Dissolved Solids (per ml of sample) [WD x 103] / V mg/l

Total Suspended Solids


Total Suspended Solids WS = WT – WD mg
= Total Solids – Total Dissolved Solids.
Total Suspended Solids (per ml of sample) [WS x 103] / V mg/l
Total Volatile Solids
Total Volatile Solids WV = WT – WF mg
= Total Solids – Total Fixed Solids.
Total Volatile Solids (per ml of sample) [WV x 103] / V mg/l
Total Settleable Solids
Settleable solids v ml

Settleable solids (per ml of sample) Wss = v/V ml/l

Conclusion

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Experiment No.: 02 Date: ..../..../…...

ELECTRICAL CONDUCTIVITY

Aim

To determine the Electrical Conductivity of water.

Apparatus

Self-contained conductance instruments: (Conductivity meter).


Thermometer, capable of being read to the nearest 0.1°C and covering the range 10-50°C.
Conductivity Cells:

Reagents

1] Conductivity water
2] Standard potassium chloride solution [0.01M KCl]

Theory

Conductivity is a measure of the capacity of water to pass an electrical current.


Conductivity in water is affected by the presence of inorganic dissolved solids such as
chloride, nitrate, sulfate, and phosphate anions (ions that carry a negative charge), or
sodium, magnesium, calcium, iron, and aluminum cations (ions that carry a positive
charge). A failing sewage system would raise the conductivity because of the presence of
chloride, phosphate, and nitrate; an oil spill would lower conductivity. The basic unit of
measurement of conductivity is the mho or siemens.

Procedure

1. Calibrate the cell with solution.


2. Rinse the cell thoroughly with deionized distilled water and carefully wipe with a
tissue paper.
3. Dip the cell into the sample solution, swirl the solution and wait upto 1 minute for
a steady reading.
4. Note down the instrument reading and also temperature by a thermometer.

Description of sample Temperature Conductivity

Conclusion/Result

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Experiment No.: 02 Date: ..../..../…...

DETERMINATION OF CHLORIDES IN WATER

Aim

To determine the chlorides in water by Mohr's method.


Apparatus
Burette, pipette, conical flask, measuring jar.

Reagents

1) 0.0141 N Silver nitrate (AgNO3)


2) Potassium chromate (K2Cr04) indicator

Theory

If water containing chlorides is titrated with silver nitrate solution, chlorides are
precipitated as white silver chloride. Potassium chromate is used as indicator, which
supplies chromate ions. As the concentration of chloride ions approaches extinction,
silver ion concentration increases to a level at which reddish brown precipitate of silver
chromate is formed indicating the end point.

NaCl + AgNO3 AgCl + NaNo3

2AgNO 3 + K2CrO4 AgCrO 4 + 2KNO3


(Reddish brown)

Procedure

1. Pipette out 50m1 of the given water sample into a clean conical flask.
2. Add 3 drops of Potassium chromate indicator. The solution turns yellow in colour.
3. Titrate this with 0.0141 N AgNO3 to a stable reddish brown or brick red precipitate.

Observations

Trial No Initial Reading Final reading Difference

Calculation

Chlorides = [(A-B) x N x 35.460 x 1000] / ml of sample = mg/l.

Where,
A = Volume of Silver nitrate consumed.
B = Blank Correction
N = Normality of AgNO3 (0.0141)

Conclusion/Result

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Experiment No.: 02 Date: ..../..../…...

SULPHATE
Aim
To determine the concentration of sulphate in water by Turbidimetric method.

Apparatus
Nephelometer, Magnetic stirrer, Stopwatch, Measuring spoon 0.2 to 0.3 ml capacity,
Nessler tubes

Reagents
Barium chloride: crystals, 20-30mesh, Standard sulphate solution, Buffer solution A
and Buffer solution B: (required when the sample sulphate (SO4--) is less than 10mg/L).

Sample collection, preservation and storage


In presence of organic matter certain bacteria may reduce SO4-- to S--. To avoid this, store
sample at 4°C.

Principle
The turbidimetric method of measuring sulphate is based upon the fact that Sulphate ion
is precipitated in an acetic acid medium with Barium chloride (BaCl2) so as to form
Barium sulphate (BaSO4) crystals of uniform size and that this tendency is enhanced in
presence of a sodium chloride—hydrochloric acid solution containing glycerol and other
organic compounds. The absorbance of the barium sulphate solution is measured by a
nephelometer or turbidimeter and the sulphate iron concentration, determined by
comparison of the reading with a standard curve.

Procedure
1. Take suitable volume of sample and dilute to 100mL into a 250 ml Erlenmeyer flask.
2. Add 20 ml buffer solution, mix well by placing on a magnetic stirrer.
3. Keep the flask constantly stirred with the help of stirrer. Add 1-spatula BaCl2 crystals
with stirring and begin timing immediately.
4. Continue stirring at constant speed exactly for 1 minute after addition of BaCl2
5. After stirring pour some of the solution into the absorption cell of the photometer, and
measure the turbidity at 30 second intervals for four minutes.
6. Usually maximum turbidity occurs within two minutes and the reading remains
constant thereafter for 3 to 10 minutes. So, take reading with maximum turbidity
occurring in within four minutes.
7. Prepare a calibration curve. The standards are prepared at 5 mg/l increments in the 0–
40 mg/l sulphate range and their turbidity or absorbance read alternatively using a
spectrophotometer at 420nm with a light path of 2.5 to 10 cm.
8. Absorbance versus sulphate concentration is plotted and a curve is obtained.
9. Finding the absorbance for a given sample, the concentration of sulphates in the
solution is determined with the help of calibration curve.

Observations
Sample Size Turbidity/ Absorbance
0 [BLANK]

Unknown Sample

Calculation

mg SO4--/l = {mg (SO4--) x 1000} / {ml of sample}

Conclusion/Result

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Experiment No.: 03 Date: ..../..../…...

ALKALINITY

Aim

To determine the alkalinity of water.


Apparatus
Burette, pipette, conical flask, measuring jar, volumetric flasks (1000ml, 200ml, 100ml)

Reagents

1. 0.02N H2SO4
2. Methyl orange indicator
3. Phenolphthalein indicator
4. Sodium thio sulphate 0.1 N

Theory

Alkalinity of a sample is a measure of its capacity to neutralize acids. It is mainly due to


the salts of weak acids and some times due to weak or strong bases, mainly due to
hydroxides, carbonates and bicarbonates. Highly alkaline water leads to embitterment and
causes deposition of precipitates in boiler tubes. Bicarbonates of calcium and magnesium
induce temporary hardness to water. Other forms of alkalinity include Hydroxide
alkalinity, Carbonate alkalinity and Bicarbonate alkalinity. Generally high alkalinity
waters are un-potable and may physiologically affect the consumers. It is a very
important parameter in corrosion control.

Procedure

Phenolphthalein Alkalinity

1. Take 25ml of sample (Water) in . a conical flask, add 2-3 drops of


phenolphthalein indicator.
2. Titrate the contents in the conical flask with 0.02N H 2 SO 4 . The end
point is pink to colorless.
3. Note the burette reading, which gives the volume of H 2 SO 4 Consumed.
Repeat till two concurrent values are obtained.

Observations

Trial No Initial Reading Final reading Difference

Calculation

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

P = [A × N × 50 × 1000] / ml of sample = mg/l as CaCO3

Where,
A = Volume of H 2 SO 4 consumed.
N = Normality of H2SO4 (0.02)

Result:

Procedure

Total Alkalinity

1. Take 25m1 of sample (Water) in a conical flask, add 2-3 drops of Methyl-orange
indicator.

2. Titrate the contents in the conical flask with 0.02N H2SO4. The end point is pale
yellow to pale pink.

3. Note the burette reading, which gives the volume of H2SO4.

4. Repeat until two concurrent values are obtained.

Observations

Trial No Initial Reading Final reading Difference

Calculation

T = [B ×N × 50 × 1000] / ml of sample= mg/l as CaCO3


Where,
B = Volume of H 2 SO 4 consumed.
N = Normality of H2SO4 (0.02)

Result:

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Experiment No.: 03 Date: ..../..../…...

DETERMINATION OF ACIDITY IN WATER

Aim

To determine the mineral acidity and total acidity of the given water sample.
Apparatus
Burette, pipette, conical flask, measuring jar.

Reagents

1. 0.02 N Sodium hydroxide (0.02 N NaOH)


2. Methyl orange indicator
3. Phenolphthalein indicator
4. Sodium thio sulphate 0.1 N

Theory

Acidity of a solution is a measure of its capacity to neutralize bases. Acidity is caused


due to the presence of mineral acids (Al2(S04)3, Fe2SO4), CO2, strong acids and weak
bases. This is caused mainly due to industrial wastes. Acidity of a sample is determined
by titrating against a strong solution of a base (alkali) such as NaOH. Types of Acidity
include Mineral acidity (partial acidity) and Total acidity.

Procedure

Mineral Acidity
1. Pipette out 25ml of the given water sample into a clean conical flask. Add
3 drops of methyl orange indicator to it. The solution becomes pink in colour.
2. Titrate this solution against 0.02 N NaOH solution taken in the burette till
the colour changes from pink to pale yellow.
3. Not e do wn t h e b ur et t e r e adi n g w hi ch i n di c at e s t he v ol u m e of N a OH
ru n d ow n (consumed). Repeat the experiment until at least 2 concurrent readings
are obtained.
4. The End Point is Pink to pale yellow.

Observation

Trial No Initial Reading Final reading Difference

Calculation
P = [A × N × 50 × 1000] / ml of sample = mg/l as CaCO3
Where,
A = Volume of NaOH consumed.
N = Normality of NaOH (0.02)

Result:

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Procedure

Total Acidity

5. Pipette out 25ml of the given water sample into a clean conical flask.

6. Add 3 drops of phenolphthalein indicator to it. The solution becomes colorless.

7. Titrate this solution against 0.02 N NaOH solution taken in the burette till the
colour changes to pink.

8. Note down the burette reading which indicates the volume of NaOH run down
(consumed).

9. The End Point is Colorless to pink.

10. Repeat the experiment until at least 2 concurrent readings are obtained.

Observations

Trial No Initial Reading Final reading Difference

Calculation

T = [B ×N × 50 × 1000] / ml of sample= mg/l as CaCO3


Where,
B = Volume of NaOH consumed.
N = Normality of NaOH (0.02)

Result:

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Experiment No.: 03 Date: ..../..../…...

pH

Aim

To determine the pH of the given water sample.


Apparatus
Burette, pH paper, pH meter, Glass Beaker, Buffer tablets.

Reagents

Standard Buffer solutions

Theory

pH is defined as the negative logarithm of hydrogen ion concentration or logarithm of


reciprocal of hydrogen ion concentration. Measurement of pH is one of the most
important and frequently needed tests in water and waste water engineering. Practically
every phase of water supply and wastewater treatment, for example acid base
neutralization, water softening, coagulation, disinfection and corrosion control is pH
dependent. pH of drinking water should be in the range of 6.5 to 8.5.

Procedure

1. By pH Paper Method

Tear off a piece of pH paper from the pH paper book. Dip this paper in a test
tube filled with the given water sample. Allow this paper to dry and
develop color. Compare the colour with the standard colour printed on the
cover of the pH paper book and record the pH. This method is an
approximate method only.

2. By pH meter Method (Electrometric method)

1) Check the inside of the electrode of the pH Meter to ascertain whether it contains
sufficient level of saturated KOH solution. The two electrodes are always
immersed in distilled water.

2) Set the temperature to 25°C (room temperature). Switch on the pH Meter and
allow the meter to warm up for about 15 minutes.

3) Take out the electrodes from the distilled water, rinse it and clean with a tissue
paper and immerse them in standard buffer solution of say pH 4. Press the knob to
adjust it to read pH position using the calibrating knob.

4) Repeat the procedure with the second buffer solution. If the meter shows the
correct reading directly, the instrument is calibrated

5) Place the electrodes in the given water sample and record the pH directly.

Observation

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Experiment No.: 04 Date : ..../..../…...

HARDNESS TEST

Aim

To determine the Total, Permanent and temporary hardness of given water sample.

Apparatus
Burette, pipette, conical flask.

Reagents

1. 0.01M EDTA (Ethylene Di-amine Tetra Acetic Acid)


2. Ammonia buffer solution
3. Eriochrome black-T indicator.

Theory

Hardness in water is defined as that property which prevents lathering of soaps. It is


caused clue to the presence of dissolved materials such as carbonates, bi-carbonates,
chlorides, nitrates and sulphates of calcium and magnesium.

Types of Hardness

1. Temporary hardness or Carbonate hardness


2. Permanent hardness or Non-carbonate hardness.

Temporary hardness in water is caused due to the presence of bicarbonates of calcium


and magnesium and boiling or addition of lime can easily remove this.

Permanent hardness is caused due to the presence of sulphates, chlorides and nitrates of
calcium and magnesium. This cannot be removed by boiling but requires special
treatment such as demineralization, ion exchange etc.

Hardness is expressed as mg/It on calcium carbonate scale. The desirable (permissible)


limit of total hardness in potable waters is 300mg/l and maximum permissible limit is 600
mg/l.

Principle

EDTA Titrimetric Method

A compound called Ethylene Di amine Tetra Acetic acid is made use of in this method.
In alkaline condition the Ca2+ and Mg2+ develops a wine red colour with eriochrome
black-T indicator. When EDTA is added as a titrant, the Calcium and Magnesium ions
get complexed resulting in a sharp change from wine red to blue, which indicates the end
point of the reaction.

Procedure

Total Hardness

1. Pipette out 25m1 of the given water sample into a conical flask.
2. Add 1m1 of ammonia buffer solution and 3 drops of Eriochrome black-T
indicator to it. The solution turns wine red in color.
3. Titrate this solution against 0.01 M EDTA taken in a burette till the color changes
from wine red to blue which indicates the end point.
4. Note down this burette reading.

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Observation

Trial No Initial Reading Final reading Difference

Permanent Hardness or Non Carbonate Hardness

1. Take about 50 ml of the given water sample, boil and cool it to remove temporary
hardness.
2. Transfer 25 ml of this solution into a clean conical flask.
3. Add l ml of ammonia buffer solution and 3 drops of Eriochrome black-T indicator
to it. The solution turns wine red in colour.
4. Titrate this solution against 0.01 M EDTA taken in a burette till the colour
changes from wine red to blue which indicates the end point.
5. Note down this burette reading which gives the volume of EDTA consumed.

Observation

Trial No Initial Reading Final reading Difference

Calculation

Total hardness = [A × B × 1000] / ml of sample = mg/l as CaCO3


Where,
A = Volume of EDTA consumed.
B = 1 (mg of CaCO3 equivalent to 1m1 of EDTA titrant)

Permanent hardness = [C × D × 1000] / ml of sample = mg/l as CaCO3


Where,
C = Volume of EDTA consumed for titrating the boiled and cooled sample.
D = 1 (mg of CaCO3 equivalent to 1m1 of EDTA titrant)

Temporary hardness = Total hardness - Permanent hardness

=…………-……….= ………… mg/l as CaCO3

Conclusion

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Experiment No.: 04 Date : ..../..../…...

HARDNESS TEST

Aim

To determine the Calcium-Magnesium hardness of given water sample.


Apparatus
Burette, pipette, conical flask.

Reagents

1. Std. EDTA (0.01 M)


2. 1 N NaOH solution
3. Muroxide indicator.

Significance

Small amounts of Ca combat corrosion of metal pipes by forming a protective coating


where as appreciable Ca content, On the other hand, forms scales in boilers, pipes,
utensils etc.

Principle

When EDTA is added to water containing both Ca2+ and Mg2+, it combines with Ca2+ in
preference to Mg2+. When the pH is sufficiently high (12 to 13), Mg2+ is largely
precipated as hydroxide and Ca2+ can be determined directly using EDTA.

Procedure

1. Pipette out 25m1 of water sample into a conical flask.


2. Add 2m1 of 1 N NaOH, followed by 2 to 3 drops of Muroxide indicator and
shake well. The solution turns pink in colour.
3. Titrate this solution against Std EDTA solution taken in a burette and discontinue
the titration when the colour changes from pink to purple.
4. Note down the volume of EDTA run down from the burette.

Observation

Trial No Initial Reading Final reading Difference

Calculation
Calcium Hardness = [A × B × 1000] / ml of sample = mg/l as CaCO3
Where,
A = Volume of EDTA consumed.
B = 1 (mg of CaCO3 equivalent to 1ml of EDTA titrant)

Magnesium Hardness = Total hardness - Calcium hardness = mg/l as CaCO3


Concentration of Ca or mg/l of Ca = {A × B × 400.8} / ml of sample.
Concentration of Mg or mg/l of Mg = 0.243 × Calcium hardness.

Result

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Experiment No.: 05 Date : ..../..../…...

DISSOLVED OXYGEN
Aim

To determine the Dissolved Oxygen content present in the given wastewater sample.

Apparatus
BOD bottles, burette, pipette, conical flask, measuring jar.

Reagents

1. Manganous sulphate solution


2. Alkali Iodide azide
3. Concentrated Sulphuric acid
4. Starch solution
5. 0.1N Stock Sodium-thio-sulphate solution
6. 0.025 N Sodium-thio-sulphate (Na2S203)

Principle (The Winkler method with Azide modification)

When MnS04 and alkali iodide azide are added to water containing DO, the oxygen
oxidizes Mn2+ to give a precipitate of Mn(OH)2. By the addition of H2SO4, free iodine is
liberated, which is converted to blue colour by the addition of starch.

Procedure
1. Fill up the BOD bottle with the given water sample up to the neck.
2. Add 2ml of MnSO4 and 2ml of alkali iodide azide solution to the BOD bottle.
Exclude the air bubbles and mix the contents of the bottle by inverting the bottle a
few times.
3. After the precipitate has settled to about 1/3rd the volume of the BOD bottle from
the bottom, add 2 ml of concentrated sulphuric acid. Once again mix the contents
gently till the suspension is completely dissolved and a uniform yellow colored
solution is obtained.
4. Take 203 ml of this solution in a conical flask and titrate with 0.025 N Na2S2O3 to
a pale straw color.
5. Add 1 ml of starch, which turns the solution blue in color. Continue the titration
till the blue color disappears. Note down the volume of Na2S203 consumed, which
gives the DO directly.
6. Hence the endpoint changes colour from Yellow to pale straw to blue to colorless.

Note

1 ml of 0.025 N Na2S203 is equivalent to 0.2 mg of oxygen.

Observation

Trial No Initial Reading Final reading Difference


1
2
3

DO in mg/L = (V x 0.2 x 1000 x N) / 200

Result

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Experiment No.: 05 Date: ..../..../…...

BIO-CHEMICAL OXYGEN DEMAND

Aim

To determine the 5 day Bio-Chemical oxygen demand (BOD5) of the given sewage
sample with 2% dilute solution.

Apparatus

BOD bottles, burette, pipette, conical flask, measuring jar.

Reagents

1. Magnesium sulphate solution


2. Alkali Iodide azide
3. Concentrated Sulphuric acid
4. Starch solution
5. 0.025 N Sodium-thio-sulphate (Na2S203)
6. Phosphate buffer
7. Calcium chloride
8. Ferric chloride

Theory

BOD is the amount of oxygen required to stabilize the organic matter present in
wastewater. The degree of magnitude of BOD depends on the amount of organic matter
present in the wastewater and temperature during the experiment. The rate of oxygen
demand or the process of stabilization on the organic matter is very high or rapid in the
initial stage i.e. 1-7 days. This is mainly due to the oxidation of carbonaceous matter
present in sewage. The oxidation of the rest is done due to nitrification. The time required
for complete oxidation is infinite, but it is limited to 20 days. For practical purpose the
period of oxidation is taken as 5 days. Then 70%-80% of oxidation will be completed
within first 5 days itself.

Principle

The standard test temperature is 20°C. This temperature is taken as the temperature of
natural water. There are 2 methods for determining the BOD.

1. Direct method: In this method BOD is directly calculated. This method is applicable
only for wastewater whose BOD value is < 7mg/l.

2. Dilution method: This test is made with various dilutions.

The following dilutions are suggested,


a. 0.1% to 7% - Strong trade waste
b. 1% to 5% - for raw or settled waste
c. 5% to 15% - for treated effluent
d. 25% to 100% - river water

Detailed Procedure

1. Place the desired volume of distilled water in a 5 litre flask (usually about 3 litres of
distilled water will be needed for each sample).
2. Add 1ml each of phosphate buffer, magnesium sulphate solution, calcium chloride
solution and ferric chloride solution for every litre of distilled water.
3. Seed the sample with 1–2 ml of settled domestic sewage.
4. Saturate the dilution water in the flask by aerating with a supply of clean compressed
air for at least 30 minutes.

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5. Highly alkaline or acidic samples should be neutralised to pH 7.


6. Destroy the chlorine residual in the sample by keeping the sample exposed to air for
1 to 2 hours or by adding a few ml of sodium sulphite solution.
7. Take the sample in the requisite concentrations as per dilution method
8. Add the required quantity of sample (calculate for 650 ml dilution water the required
quantity of sample for a particular concentration) into a 1000 ml measuring cylinder.
Add the dilution water up to the 650mL mark.
9. Mix the contents in the measuring cylinder.
10. Add this solution into two B.O.D. bottles, one for incubation and the other for
determination of initial dissolved oxygen in the mixture.
11. Prepare in the same manner for other concentrations and for all the other samples.
12. Lastly fill the dilution water alone into two B.O.D. bottles. Keep one for incubation
and the other for determination of initial dissolved oxygen.
13. Place the set of bottles to be incubated in a B.O.D. incubator for 5 days at 20°C. Care
should be taken to maintain the water seal over the bottles throughout the period of
incubation.
14. Determine the initial dissolved oxygen contents in the other set of bottles and note
down the results.
15. Determine the dissolved oxygen content in the incubated bottles at the end of
5 days and note down the results.
16. Calculate the B.O.D. of the given sample.

Overview of Procedure

1. Prepare the required dilution of the sewage sample.


(For 1% dilution 1/100 × 300= 3 ml of sewage is taken in the BOD bottle and diluted
to 300 ml with aerated distilled water).
2. Determine the DO of this sample, which is the zeroth day DO or initial DO.
3. In another BOD bottle, prepare the sample of same dilution as before. Keep this
sample in a BOD incubator at 20°C for determining the DO after 5 days to get D2
(final DO or DO after 5 days.)

Calculations

BOD5= (D1-D2)/P mg/l


D1= Zero day or initial DO (before incubation)
D2 = DO after 5 days (final or DO after incubation)
P = % dilution (1% = 1/100 = 0.01)

Observations for D1

Trial No Initial Reading Final reading Difference

Observations for D2

Trial No Initial Reading Final reading Difference

Result

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Experiment No.: 06 Date : ..../..../…...

CHEMICAL OXYGEN DEMAND

Aim

To determine the COD of the given sewage sample by Open Reflux method.
Apparatus
Reflux apparatus of capacity 500m1 with a condenser, Burner or hot plate, 250 or 500mL
Erlenmeyer flask with standard (24/40) tapered glass joints, Friedrich’s reflux condenser
(12 inch) with standard (24/40) tapered glass joints, Volumetric pipettes (10, 25, and
50ml capacity), Burette, 50ml with 0.1ml accuracy, Burette stand and clamp, Analytical
balance, accuracy 0.001gm, Spatula, Volumetric flasks (1000ml capacity), glass beads.

Reagents
0.25N Std Potassium-dichromate (0.04167 M), Conc. Sulphuric acid reagent, (0.25M)
Std Ferrous ammonium sulphate , Ferroin indicator, Mercuric sulphate crystals, analytical
grade and Standard Potassium hydrogen phthalate (KHP)

Principle
The organic matter gets oxidized completely by K2Cr2O7 in the presence of H2SO4 to
produce CO2 and H2O. The excess K2Cr2O7 remaining after the reaction is treated with
Ferrous Ammonium Sulphate .The dichromate consumed gives the oxygen required for
oxidation of the organic matter.

Procedure

Standardisation

Dilute 10 ml standard K2Cr2O7 to about 100 ml, add 30 ml conc.H2SO4, cool. Add 2
drops of ferroin indicator and titrate with FAS.

Estimation

Place 0.4 gm HgSO4 in a reflux flask. Add 20 m1 sample or an aliquot of sample diluted
to 20m1 with distilled water. Mix well and add glass beads followed by 10 m1 Std
K2Cr2O7. Add slowly 30 m1 H2SO4 containing Ag2SO4, mixing thoroughly. Connect the
flask to the condenser and mix the contents before heating. Reflux for a minimum period
of 2 hours, cool and wash down the condenser with distilled water. Dilute to about 150
m1, cool and titrate excess K2Cr2O7 with 0.1 N FAS using Ferroin indicator. Sharp colour
change from blue green to wine red indicates the end point. Reflux the blank in the same
manner using distilled water instead of the sample.

Calculation

COD (mg/l) = [ ( a – b) × 8000 × N ] / ml of sample.


Where a & b = ml of FAS for blank and sample respectively.
N = Normality of FAS (0.1 N )

Observation

Trial No Initial Reading Final reading Difference

Result

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Experiment No.: 07 Date : ..../..../…...

AVAILABLE CHLORINE
Aim
To determine the Percentage of Chlorine in Bleaching Powder.

Apparatus
Conical flask, burette, pipette, measuring jar, funnel.

Reagents
Bleaching powder, Potassium Iodide (KI), Glacial Acetic acid, Starch solution and 0.1 N
Sodium thio sulphate

Theory
Chlorine a strong oxidizing agent and a very effective disinfectant used for the
destruction of pathogenic bacteria. Chlorine is generally applied in the form of bleaching
powder for disinfection of water. Commercial bleaching powders generally contain 25 to
30% of available chlorine. This percentage is a very critical factor for effective
disinfection of water.

Procedure

1. Weigh 1gm of fresh bleaching powder and make it into a paste by adding a small
quantity of distilled water.
2. Add some more water, stir it and allow it to settle for a few minutes. Decant the
supernatant solution and dilute to 1000 ml with distilled water. This is called
chlorine water or standard chlorine solution
3. Pipette out 25 ml of this chlorine water into a conical flask. Add 1 pinch of KI
crystals and 5ml of glacial acetic acid. Wait for 15-20 minutes (contact period)
4. Titrate this solution with 0.025 N Sodium thio sulphate. The solution turns from
deep yellow to pale yellow.
5. Add 2 drops of starch solution. The solution becomes blue in color.
6. Continue the titration till the blue color just disappears. Note down the volume of
Sodium thio sulphate used.

Observation

Trial No Initial Reading Final reading Difference

Calculation
Percentage of chlorine in the given bleaching powder = [(V × N × 35.46 × 1000) / 25]

Note

Result

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ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Experiment No.: 07 Date : ..../..../…...

RESIDUAL CHLORINE

Aim

To determine the residual chlorine present in the given sample of water by Iodometric
method.
Apparatus
Conical flask, burette, pipette, measuring jar, funnel, beakers.

Reagents

0.1N Sodium thio sulphate, Glacial Acetic acid, KI solution and Starch solution indicator.

Principle

Chlorine present in water reacts with KI and iodine is liberated, when starch is used as
indicator, the presence of blue color produced indicates the presence of Iodine.

Procedure

1. Take 25m1 of water sample in a BOD bottle.


2. Add 1gm of KI crystals and 5ml of glacial acetic acid, Mix thoroughly. Wait for 15-20
minutes (contact period)
3. Titrate this solution with 0.025 N Sodium thio sulphate. The solution turns from deep
yellow to pale yellow.
4. Add 2 drops of starch solution. The solution becomes blue in color.
5. Continue the titration till the blue color turns colorless.

Sample collection, preservation and storage

Chlorine in aqueous solution is not stable, and the chlorine content of samples or
solutions, particularly weak solutions, will decrease rapidly. Exposure to sunlight or other
strong light or agitation will accelerate the reduction of chlorine. Therefore, chlorine
determination should be done immediately after sampling, avoiding excessive light and
agitation. The sample should not be stored for analyses of residual chlorine.

Observation

Trial No Initial Reading Final reading Difference

Calculation
Amount of residual chlorine = [V x N x 35.46 x 1000] / ml of sample = mg/l.
Where
V = volume of sodium thio sulphate run down.
N = Normality of sodium thio sulphate.

Result

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Experiment No.: 07 Date : ..../..../…...

CHLORINE DEMAND
Aim

To determine the chlorine demand of the given water sample.


Apparatus
BOD bottles, conical flask, burette, pipette, measuring jar, funnel, beakers.

Reagents
0.01N Sodium thio sulphate, KI solution, Glacial acetic acid and Starch solution

Theory

Chlorine is used as a disinfectant in water. The chlorine demand of water is the difference
between the amount of chlorine applied and the amount of free chlorine left after the
contact period as residue. The optimum dose of chlorine for given water is therefore
generally determined experimentally by adding varying amounts of chlorine to the given
sample and observing the residual chlorine left after a contact period of about 20 minutes.
The dose, which leaves a residual of 0.2 mg/l, is then selected. This total dose minus the
free residual will automatically represent the chlorine demand of water.

Procedure

1. Take 6 clean BOD bottles and add 200m1 of homogenous water sample to each.
2. Add 0, 2, 4, 6, 8 ml of chlorinated water (known strength) to each bottle respectively.
3. Put stopper and Shake well. Allow it to remain so for about 20 minutes. Chlorine
reacts with the organic matter and oxidizes it and also kills the bacteria present in the
sample
4. After contact period, add 1gm KI and 5ml glacial acetic acid to each of these bottles.
5. Titrate this solution with 0.025 N Sodium thio sulphate. The solution turns from deep
yellow to pale yellow.
6. Add 2 to 3 drops starch indicator. The appearance of blue color indicates the presence
of chlorine.
7. To estimate the amount of chlorine left in the sample as residue, it can be titrated
against 0.01 N Na2S203 till the end point is reached, which is indicated by the
disappearance of blue color.
8. The chlorine demand is given by the difference between the applied Chlorine and the
residual chlorine after the contact period.

Observations for Residual Chlorine

Trial No Initial Reading Final reading Difference

Calculation
Sl.No BOD ml of chlorine mg of chlorine Residual Chlorine
bottle No added added to 1000 chlorine Demand [mg/l]
ml [mg/l]

Result

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Experiment No.: 08 Date : ..../..../…...

TURBIDITY
Aim

To determine the turbidity of the given sample by Nephelo turbiditymeter.

Apparatus

Nephelo turbiditymeter.

Reagents

Standard stock solution for Nephelo turbidity test

Sample collection, preservation and storage

Determine turbidity on the day the sample is taken. It storage is unavoidable, store the
samples in dark for up to 24 hr. Prolonged storage before measurement is not
recommended because irreversible changes in turbidity may occur. All samples should be
shaken vigorously before examination.

Theory

Suspension of particles in water interfering with the passage of light is called turbidity.
Turbid water is undesirable from aesthetic point of view in drinking water supplies and
may also affect products in industries. It also causes a number of problems in water
treatment plants. The permissible limits for drinking water is 5 to 10 ppm, measured on a
silica scale

Principle

When light is passed through a sample having suspended particles, some light is scattered
by the particles. The scattering of light is proportional to the turbidity.

Procedure

1. Switch on the Nephelo Meter and wait for 10 to 15 minutes for the instrument to warm
up.
2. Fill up the sample holder with distilled water, place it in the instrument & Close the
cover. Using the zero adjustment knob, adjust the reading to show zero.
3. Take out the distilled water sample and fill up the holder with the standard solution of
500 NTU from the already prepared standard stock solution. Place it in the instrument
and close the cover. Turn on the range switch to 1000 and adjust the instrument to read
50 (500 NTU) using the calibrating knob. Repeat the procedure with other standard
solutions to calibrate the instrument.
4. To know the turbidity of the given unknown sample, Keep it in the instrument and
record the turbidity reading directly in NTU.

Note

Linear dilution of 1000 NTU (Stock solution)

Strength Dilution

1000 NTU Direct


800 NTU 80m1 of 1000 NTU (stock) solution + 20m1 of distilled water

Result

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Experiment No.: 08 Date : ..../..../…...

JAR TEST EXPERIMENT


Aim
To determine the optimum dosage of the coagulant alum to treat turbid water.

Apparatus
Glass beakers, Jar test apparatus, Nephelometer, Pipette, pH meter.

Reagents
Alum

Theory

The public water supplies consists of very fine particles of clay, silt etc which are present
in a finely divided state and it is not possible to detain them in primary sedimentation
tanks unless they are designed for longer detention periods. The other way to remove
them is to increase their size so that they become settleable, by adding certain chemicals
called coagulants, which react with impurities in water and convert them into settleable
size. Some common coagulants used are Alum, Sodium aluminate, ferric chloride,
copperas, chlorinated copperas, ferric sulphate etc.

Procedure

1. Prepare standard solution of coagulant say 1% solution, by dissolving 5gm of alum in


distilled water and making upto 500m1.
The strength of the solution = 1% (1m1 = 10mg)
2. Take 1-litre beakers and fill them with sample up to the mark.
3. Keep each beaker below each paddle and lower the paddles, such that each one is
about 1cm above the bottom.
4. Find the pH of the sample and adjust it to 6 to 8.5.
5. Pipette 1, 2, 3, 4, 5, 6 ml of the alum solution into the test samples, i.e. the dosage is
10, 20, 30, 40, 50 and 60mg respectively.
6. Immediately run the paddles at 100 rpm for 1 minute.
7. Reduce the speed to 30–40 rpm and run at this rate for 30 minutes.
8. Stop the machine, lift out the paddles and allow to settle for 30 minutes.
9. Find the residual turbidity of the supernatant using nephelometer.
10. Plot a graph with alum dosage along x-axis and turbidity along y-axis.
11. The dosage of alum, which represents least turbidity, gives Optimum Coagulant
Dosage..
12. Repeat steps 1–10 with higher dose of alum, if necessary.

Note
Strength of solution. 1 gm = 100m1

Observation

Jar ml of mg of Concentration
Description of
No coagulant coagulant mg/l
the sample added added

Conclusion

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Experiment No.: 09 Date : ..../..../…...

IRON

Aim

To determine the concentration of iron in the given water sample by Phenanthroline


method.

Apparatus
Nessler's tubes (100 ml), Conical flasks, Pipettes, Colorimeter.

Reagents

Conc. HCl acid, Hydroxylamine hydrochloride solution, Ammonium acetate buffer


solution, 1, 10-Phenanthroline solution, Stock Fe soln. and Std Fe soln. (1ml = 1 mg Fe).

Principle

In the Phenanthroline method, the ferric form of iron is reduced to ferrous form by
boiling with hydrochloric acid and hydroxylamine hydrochloride. The reduced iron
chelates with 1,10 phenanthroline at pH 3.2 - 33 to form a complex of orange-red color.
The intensity of color is proportional to the concentration of iron and obeys Beer's law.

Procedure

1. Pipette 10, 20, 30 and 50m1 of standard iron solution into 100m1 conical flask
2. Add l ml of Hydroxyl amine hydrochloride solution and 1m1 of sodium acetate
solution to each flask.
3. Dilute each to about 75m1 with distilled water and Add 2ml of 1,10-phenanthroline
solution to each flask.
4. Make up the contents of each flask exactly to 100m1 by adding distilled water and
allow atleast 10-15 minutes for maximum color development.
5. For visual comparison pour the solution in 1.00 m1 Nessler tubes and keep them in a
stand. Mix the sample thoroughly and measure 50ml into a conical flask
8. Add 2 ml of concentrated HCl and 1 ml of Folderol amine solution and a few glass
beads. Boil the contents to half of the volume for dissolution of all the iron
9. Cool the flask to room temperature and transfer the solution to a 100 m1 Nessler tube
10. Add 10m1 of Ammonium acetate buffer solution and 2m1 Phenanthroline solution
and dilute to 100m1 mark with distilled water. If the sample contains interference of
heavy metals add 10m1 of Phenanthroline instead of 2m1
11. Mix thoroughly and allow atleast 10-15 minutes for maximum color development
12. For visual comparison, match the color of sample with that of the standards prepared
in steps 1-6 above
13. The matching color standard will give the concentration of iron in the sample

For photometric measurement, use light path at 510nm. Read standards against distilled
water set at zero absorbance and plot a calibration curve, including a blank. If samples
are coloured or turbid, carry a second set of samples through all steps of the procedure
without adding Phenanthroline.

Comments

Environmental Significance

Long time consumption of drinking water with a high concentration of iron can lead to
liver diseases. Iron rich water exposed to the air becomes turbid and highly unacceptable
from the aesthetic view point.

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Experiment No.: 10 Date : ..../..../…...

FLUORIDE

Aim

To determine the concentration of fluoride for a given water sample by Colorimetric


method (SPADNS method).

Apparatus
Distillation apparatus, Colorimetric, Nessler tubes [capacity-100ml], Pipette

Reagents

1. Stock sodium fluoride solution


2. Standard sodium fluoride solution
3. Zirconium alizarin solution
4. Mixed acid solution
5. Acid zirconium alizarin reagent
6. Sodium thio sulphate solution

Sample collection, preservation and storage

Polyethylene bottles are preferred for collecting and storing samples for fluoride analysis.
Glass bottles are satisfactory, provided that they have not previously contained high-
fluoride solutions. Always rinse the bottle with a portion of the sample.

Principle

Sodium 2-(parasulphophenylazo)-1,8-dihydoxy-3,6-naphthalene disulphonate: SPADNS

This method is used for estimation of fluoride in natural water in the concentration range
0-1.4 mg/l. The test is based on the fact that fluoride ion combines with zirconium on 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.

Procedure

1. The sample should be free from chlorine, if chlorine present, it shall be dechlorinated
with a slight excess of sodium thio sulphate solution before use.
2. If the sample contains excess interfering ions, the sample should be appropriately
diluted and distillated before test.
3. Take 0, 1, 2, 6, 8, 14 ml of Standard sodium fluoride solution in six Nessler tubes.
[The range should be such that it is between 0 and 1.4 mg/l]
4. Add 5m1 of acid zirconium reagent in each Nessler tube.
5. Similarly add 5m1 of acid zirconium reagent into the Nessler tubes containing 100m1
of sample.
6. Mix thoroughly and compare the colors after standing for one hour.

Comments

Environmental Significance

Fluoride ions have dual significant in water supplies. High concentration of F- causes
dental fluorosis (disfigurement of the teeth) and skeletal fluorosis. At the same time, a
concentration less than 0.8mg/l results in ‘dental caries’. Hence, it is essential to maintain
the F- concentration between 0.8 to 1.0mg/l in drinking water.

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Experiment No.: 11 Date : ..../..../…...

MPN TEST{B/E-COLI) COLIFORMS INDEX}

Aim

To determine the most probable number (MPN) index of coliforms and E-coli organisms
in the given water sample by multiple tube fermentation tube technique.

Apparatus

Incubator, fermentation tubes, test tubes, EMB agar plate, Petri-dishes, microscopes,
Autoclave, Pipettes, Measuring jars, Inoculating equipments [platinum loop], Media
preparation utensils.

Reagents

1. Lauryl tryptose broth


2. Brilliant green lactose bile broth
3. Endo methylene blue agar.
4. Eosin methylene blue agar.
5. Lactose broth

Theory

Coliform group comprises of all the aerobic, facultative and anaerobic gram-negative
non-spore forming rod shaped bacteria that ferment lactose with gas formation within 48
hours at 35°C. The standard test for this group may be carried out either by multiple tube
fermentation technique or by membrane filter technique. Escherichia coli (E.coli) is used
as an indicator organism for the purpose of sanitary examination of water. The E.coli test
by multiple tube fermentation technique consists of 3 phases – presumptive, confirmed
and completed. The results are expressed in terms of MPN (Most Probable Number),
which is based on certain probability formulae. The estimate may give a value greater
than the actual number of coliform present. The accuracy of any single test depends on
the number of tubes fermented. This method helps in describing the sanitary quality of
water. The safety of the water is generally judged from the knowledge of sanitary
condition and mentioned by the number of samples yielding positive or negative results.
If more than 95% should yield negative results, the safety is usually assured.

Procedure

1. Collect the sample in sterilized bottles


2. Prepare the sterilized media necessary for the bacteriological test and keep them re0y
in test tubes containing Durham tubes / fermentation tubes.
3. Inoculate the sample in an exponential order le 10, 1 and 0.1 ml in 5 tubes each of
lauryl tryptose broth under asceptic conditions.
4. Incubate all the tubes at 35°C.
5. After 24 hours examine the tubes for gas formation.
6. The tubes containing the gas are marked positive and are taken out of the incubator for
further analysis. Remaining tubes are further incubated at 35°C for another 24 hours.
This is the presumptive test for coliform organisms.
7. One or two loop full of the liquid from the positive lauryl tryptose tubes are transferred
into the sterilized EC medium tubes and incubated for 24 hours at 44°C.
8. The gas production after 24 hours confirms the presence of E-Coli or feacal Coliforms.

DEPARTMENT OF CIVIL ENGINEERING ACHARYA INSTITUTE OF TECHNOLOGY


ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

DEPARTMENT OF CIVIL ENGINEERING ACHARYA INSTITUTE OF TECHNOLOGY


ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Observations

Computation of MPN

The number of positive finding of coliform group organisms resulting from the multiple
portion decimal dilution planting should be computed as the combination of positives and
recorded in terms of the Most Probable Number (MPN). The MPN may be estimated by
Thomas’ simple formula:

Result : MPN/100 ml =

Conclusion

DEPARTMENT OF CIVIL ENGINEERING ACHARYA INSTITUTE OF TECHNOLOGY


ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Experiment No.: 12 Date: ..../..../…...

NITRATES

Aim

To determine the concentration of Nitrate Nitrogen present in the given sample of given
water sample.

Apparatus

Spectrophotometer or Colorimeter, Nessler tubes (capacity-100ml), Beakers (capacity-


100ml and Water bath.

Reagents

1. Stock nitrate solution


2. Standard nitrate solution
3. Standard silver sulphate
4. Potassium Hydroxide [12N]
5. Phenol di sulphonic acid (PDA)
6. Concentrated Ammonium hydroxide [NH4OH].

Principle

Nitrate reacts with Phenol di sulphonic acid and produces a nitro-derivative which in
alkaline medium develops a yellow color. The color produced follows the Beer's law and
is directly proportional to the concentration of nitrate present in the sample.

Procedure

1. Take 50ml of filtered sample in an Erlenmeyer flask.


2. Add an equivalent amount of silver sulphate to remove chlorides
(1 mg/l Cl = l ml Ag2SO4 solution)
3. Heat slightly and filter the precipitate of AgCl.
4. Evaporate the filtrate in a porcelain disc to dryness.
5. Cool and dissolve the residue in 2m1 phenol di sulphonic acid and dilute to 50 ml.
6. Add 10 m1 of liquid ammonia to develop the yellow color.
7. Read the color developed at 410 nm with a light path of 1cm.
8. Calculate the concentration of nitrate nitrogen from the standard curve.
9. Prepare the standard curve using suitable aliquots of standard nitrate solution in the
range of 5-500 mg NO3-N following the above procedure.

Interferences

Chlorides and nitrite are the two main sources of interferences. Pretreatment of sample is
necessary when the interfering radicals are present.

Result:

Conclusion:

Environmental Significance

In surface waters, nitrate may cause objectionable eutrophication. Nitrates are poisonous
to infants, animals including humans. In humans it can cause 'methemoglobinemia'.

DEPARTMENT OF CIVIL ENGINEERING ACHARYA INSTITUTE OF TECHNOLOGY


ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

WORKING SPACE PREVIOUS EXPERIMENT

WORKING SPACE NEXT EXPERIMENT

DEPARTMENT OF CIVIL ENGINEERING ACHARYA INSTITUTE OF TECHNOLOGY


ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Experiment No.: 13 Date : ..../..../…...

SODIUM
Aim
To determine the concentration of Sodium in given water sample by Flame Photometer.

Apparatus
Flame photometer

Reagents
Stock sodium solution, Intermediate sodium solution, Standard sodium solution

Storage
Store samples containing low sodium concentrations or alkaline samples in polyethylene
bottles to eliminate the possibility of sample contamination due to leaching of the glass
container.

Principle of Quantification
Trace amounts of sodium can be determined by flame emission photometry at the
wavelength of 589 nm. The sample is sprayed into a gas flame and excitation is carried
out under carefully controlled and reproducible conditions. The calibration curve may be
linear but has a tendency to levels off at higher concentrations.

Procedure

1. Follow instructions of flame photometer manufacturer for selecting proper photocell,


wavelength, slit width adjustments, fuel gas and air pressure, steps for warm up,
correcting for interference and flame background, rinsing of burner, sample ignition
and emission intensity measurements.
2. Prepare a blank and sodium calibration standards, in any of the applicable ranges, 0-
100, 0-10, or 0-1 mg Na/l. Set instrument zero with standard containing no sodium.
3. Measure emission at 589 nm and prepare calibration curve.
4. Determine sodium concentration of the sample, or diluted sample, from the curve..

Calculation

Dilution mg Na/l = mg Na/l [from the calibration curve] x Dilution

Where,

Observations

Sample Size Absorbance


0
5
10
15
25
Unknown Sample

Result

DEPARTMENT OF CIVIL ENGINEERING ACHARYA INSTITUTE OF TECHNOLOGY


ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

Experiment No.: 13 Date: ..../..../…...

POTASSIUM

Aim

To determine the concentration of Potassium in given water sample by Flame


Photometer.
Apparatus
Flame photometer

Reagents
Stock Potassium solution, Intermediate potassium solution, Standard potassium solution

Storage
Do not store samples in soft-glass bottles because of the possibility of contamination
from leaching of the glass. Use acid washed polyethylene or borosilicate glass bottles.
Adjust sample to pH <2 with nitric acid. This will dissolve potassium salts and reduce
adsorption on vessel walls.

Principle of Quantification
Trace amounts of potassium can be determined in either a direct-reading of internal
standard type of flame photometer at a wavelength of 766.5 nm. The sample is sprayed
into a gas flame and excitation is carried out under carefully controlled and reproducible
conditions. The calibration curve may be linear but has a tendency to levels off at higher
concentrations.

Procedure
1. Follow instructions of flame photometer manufacturer for selecting proper photocell
wavelength, slit width adjustments, fuel gas and air pressure, steps for warm up,
correcting for interference and flame background, rinsing of burner, sample ignition
and emission intensity measurements.
2. Prepare a blank and potassium calibration standards, in any of the applicable ranges, 0-
100, 0-10, or 0-1 mg/l. Calibrate instrument, set instrument to zero absorbance with
blank solution containing no potassium.
3. Measure emission at 766.5 nm and prepare calibration curve.
4. Determine potassium concentration of the sample, or diluted sample, from the curve.

Calculation
mg K/l = mg K/l [from the calibration curve] x Dilution

Where,

Observations
Sample Size (ml) Absorbance
0 [BLANK]

Unknown Sample

Result

DEPARTMENT OF CIVIL ENGINEERING ACHARYA INSTITUTE OF TECHNOLOGY


ENVIRONMENTAL ENGINEERING LAB MANUAL 06CVL77

WORKING SPACE PREVIOUS EXPERIMENT

DEPARTMENT OF CIVIL ENGINEERING ACHARYA INSTITUTE OF TECHNOLOGY