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ACKNOWLEDGEMENTS

A formal statement of acknowledgement will hardly meet the ends of justice


while writing these words, we feel obliged to all of them who extended their
inconceivable co-operation towards the hard work whatever we have done.
First of all, we feel very obliged to Director (Haryana Test House
&Consultancy Services Panipat), who made our wish fulfilled to work out
our Summer Training in Haryana Test House.
We got an excellent opportunity to carry out our summer dissertation work
under the honorable and encouraging guidance of Mr.T.L. MEHTA
(Technical Manager Environment Dept). Their didactic, constant
guidance, encouragement, inspiration and kind co-operation that they have
shown towards us in completion of this endeavor are quite hard to match.
Words can never be able to express our heartiest thanks to Prof. C.P.
Kaushik, Chairperson and Dean of the Dept. and Mr. Jitender Pal Training
and Placement Incharge, Faculty of Non Conventional Sources of Energy
and Environmental Science, Department of Environmental Science and
Engineering, Guru Jambheshwar University of Science and Technology,
Hisar for their kind approval for our summer training work.

CONTENTS
1. Introduction
i.

Sources of Water.3

ii.

Water Pollution....4

iii.

Sampling..6

2. Parameter studies in drinking water


i.

Color8

ii.

Turbidity..10

iii.

Odour..11

iv.

pH...12

v.

Alkalinity14

vi.

Total dissolved Solids.16

vii.

Total suspended solids.17

3. Parameters Studies in waste water


i.

C.O.D...22

ii.

B.O.D.......

iii.

Oil and Grease25

INTRODUCTION
2

Chemical Properties:Chemically Active


Reacting with certain metals and metals oxides to form bases. And oxides of
non-metals to form acids. It reacts with organic compounds to from various
products e.g. Alcohols from alkenes.
Completely pure water is poor conductor of electricity, it is much better
conductor than most other pure liquids because of its self ionization i.e.
ability of two water molecules to react to form an OH and H3O+ions.

Sources of Water:Precipitation:The basic source of water is precipitation. This is the water falling from the
atmosphere to the surface of the earth as rain, snow etc.
Run off:Part of the rain and melted snow seeps into the soil. The rest becomes what
is called surface run off which flows down slopes and gathers in ravines that
discharge into rivers. Generally the term surface water indicates the water
that collects on or flows over the surface from rivers lakes, ponds, reservoirs,
canals brooks and creeks.

Ground Water:3

It is the accumulation of water below the surface ground. A portion of the


water falling or precipitation to the earth infiltration to the ground water
reservoirs. The ground water may be regarded as a temporary natural
reservoir. It emerges as springs or can be tapped by means of wells and in
filter galleries.
Importance of Water:1. Water is used for drinking, washing and irrigation purposes.
2. It is used in all metabolic reactions.
3. It is main constituent of blood plasma and 70% of our body weight is
water.
4. It is used I industries as a coolest and also as a solvent. It is also used
in constructions.

Pollution of Water:Any change in physical, chemical and biological properties of water by


human activity that imparts its use for different purpose is called water
pollution.
Sings of Water Pollution:1.
2.
3.
4.
5.
6.

Bad taste of drinking water.


Offensive odour from lakes.
Colour and turbidity and suspended solids.
Unchecked growth of aquatic weeds in water bodies.
Decrease in number of fist in fresh water, river water.
0Oil and grease floating on water surfaces.

Types of Water Pollution:-

A.

Point sources of pollution :- When a source of pollution can be


readily identified because it has a definite source and place where it
enters the water it is said to come from a point source e.g. municipal

B.

and industrial discharge dices.


Non point source of Pollution:- When a source of pollution cannot
be readily identified such as agricultural run-off acid rain etc. are
called non-point source of pollution.

Pollutants:

Organic Pollutants
Inorganic Pollutants
Sediments
Radio-active materials
Thermal Pollutants

Why Analysis of Water & Waste Water is necessary: To assess its quality to provides pure and wholesome water to the
public for drinking and other domestic purposes.
To find out whether water is suitable for the specific Industrial
purpose and if not to choose the most effective treatment.
To determine whether any pollution has occurred in a water course
and to trace the origin and extent of pollution and to suggest a
possible remedy.
To determine the efficiency towards natural purification when
industrial and sewage wastes and discharged in to water course.
To ascertain the effect of heavy rainfall or of long continued drought.
To measure the effect of pumping particularly when the wells are
constructed near sea or an estuary where the tidal influence is
possible.
5

To check the efficiency, uniformity and consistency of treatment and


purification processes.
To find out the possibility and extent of mixing water from two or
more sources.
To find out whether infection by microbial organisms has occurred
and if so, to find out the particular organism and to suggest preventive
measures and effective disinfection procedures.

SAMPLING:Samples are collected for various examinations under different conditions.


Whatever may be method of sampling, the samples must represent the
conditions existing at the pint taken. The sample must be of sufficient
volume to carry out the determinations.
Quality of Sample:Generally 2 liters of sample is sufficient for most of physical and chemical
examinations. For certain special determinations however larger volumes of
sample are necessary.

Sample Container:For most of the purposes, the ordinary stoppered Winchester Quart bottle of
2.5 liters capacity is enough generally glass container are preferable to those
made of polythene or other plastic materials. Polythene containers are
however used in some circumstances e.g. when the sample being examined
extracts substances from the glass or some of the constituents of the sample
adhere to the glass.
6

Samplers:A variety of special sampling devices are available to meet the specific
requirements among them displacement sampler for determination of
dissolved oxygen. When composite samples are to be collected, it is better to
use wide mouthed bottles of capacity 200-300 for the sub-samples. They are
particularly useful in transferring the contents without leaving any settle able
matter.
New glass bottles should be treated either with dil.Hcl or then
repeatedly washed with water and finally with distilled water. Subsequently
they may be cleaned using detergents.
If trace amounts of phosphates are to be determined do not use detergents for
cleaning. If chromium or sulphates are to be determined do not use acid for
cleaning.
Grab Sample of Composite Sample:Grab sample is a manually collected single portion of sample of water
or waste water.
When grab samples of particular water or waste water is collected at
regular intervals for a specific period and mixed, then the integrated sample
is known as Composite Sample.
Preservation of Samples:Preservative should be chosen with regard to the determinations that are to
be made. It should be noted that the preservative added for one constituent
should not affect the determination of other constituent keeping the sample
in the dark at low temperature is the best preservation.
7

PARAMETERS STUDIED IN
DRINKING WATER
1. Colour:IS: 3025 (P-4)
Units: Hazen
Colour is a common constituted of many natural waters and it is caused by
metabolic substances such as iron and manganese compounds, human
materials, peat tannins, algae, weeds and protozoa. The term colour means
the true colour solution ad due to the substances preset as fine colloids. For
true colour determination the sample has to be centrifuged to remove
turbidity. Apparent colour is colour due to both suspended ad dissolved
matters.
Interferences:Turbidity in excess of 5, seriously affects the true colour determination.
Hence it should be removed prior to determination by centrifugation Do not
filter the sample to remove turbidity or suspended matter, since iteration has
a decolorizing effect.
Reagents:8

Standard Colour Solution.


Procedure:Place 50 ml of the sample (centrifuged) in a 50 ml Nester tube compare the
colour of the sample with that of the working colour standards by looking
vertically downwards against a pure white surface placed at such an angle
that light is reflected up wards through the columns of liquid. If the colour
exceeds 70 units dilute the centrifuged sample with distilled water such that
the colour is within the range.
Limit:Desirable 5 max.
Permissible 25 max.

2. Turbidity:Is
Units

3025 (P-10)
NTU

Method:- (Instrumental Method)


Turbidity is an important parameter for characterizing water quality. It is an
expression of optical property of a sample containing insoluble substances
which cause light to be scattered rather than transmitted in straight lines. The
amount and angular distribution of this scattered light is governed not only
by the quantity of the insoluble substances but also by their size shape and
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refractive index. In most of the waters turbidity is due to colloidal and


extremely fine dispersions suspended matter such as clay, slit finely divided
organic and inorganic matter plankton and other microscopic organisms also
contribute to turbidity.
Regents:Stock Turbidity Suspension.
Standard Turbidity Suspension.
Working Turbidity Suspension.
Procedure:Follow the manufacturers operating instructions. If the instrument is
calibrated in terms of formalize turbidity units, use a series of working
turbidity suspensions to standardize the instrument, If calibrated in other
terms prepare a series of working turbidity suspensions covering the range
up to 40 units and measure the reading prepare a calibration curve relating
instrument reading to turbidity. Find out the turbidity of the sample either
directly from the instrument reading as from the calibration graph. The
calibration curve should be checked from time to time.
Following points should be born in mind while determining the
turbidity of the sample.
Shake the sample well to disperse the solids thoroughly. Pour the
sample into the turbid meter tube after all the bubbles have
disappeared.
If the sample is very cold allow it to reach the room-temperature
before testing.
10

If the turbidity exceeds 40 units, dilute the sample appropriately with


turbidity free distilled water.
Express the result in terms of NTU after rounding off them to the
nearest value as given in the schedule.
Limit
Desirable 5 max.
Permissible 10 max.

3. Odour:IS: 3025 (P-5)


No water can be quite satisfactory for domestic and industrial purpose if it
possess any odour. Disagreeable odour and tastes in water are due to the
presence of a variety of objectionable substances particularly living
microscopic organisms or decaying vegetation including algae actinomy
cetes bacteria, fungi and weeds. Sewage and industrial waste also contribute
tastes and odour to receiving waters.
Qualitative Determination of Odour:Collect samples in glass bottles and determine the odour as-soon-as possible
after sample collection. Do not use plastic containers for collection of
samples for odour taste.
Place 250 ml of sample in 500 ml wide mouth earthen Meyer flask at
room temperature and sniff the odour. This is the cold odour quality. Some
odours may be missed at room temperature and it is better to determine. The
hot odour quality also.

11

Place 250 ml sample in 500 ml stoppered uncial flask and heat to


about 58-60oC. Remove the stopper and sniff the odour. Report the nature
and type of odour present.
Limit Unobjectionable

4. pH Value:IS: 3025 (P-11) 1983


Method:-

Electrometric Method

pH is a term used universally to express the intensity of the acid or alkaline


condition of a solution. It is a measure of hydrogen ion concentration as
mare precisely the hydrogen ion activity.
PH is defined as the Logarithm (base 10) of the reciprocal of the
hydrogen ion concentration. Thus if [H+] = 10-6 mole per liter, then pH=6.
pH is an important factor in water chemistry, since it enters into the
calculation of activity and alkalinity and processes such as coagulation,
disinfection, softening and corrosion control.
Principle of Electrometric Method:A pH meter is a high-impedance electrometer calibrated in terms of PH.
Electrometric determination of PH involves the measurement of the
electromotive force of a cell comprising an indicator electrode responsive to
hydrogen ions and a reference electrode both immersed in the test solution.
The indicator electrode commonly used is glass electrode and the reference
electrode is calomel electrode. Measurement of PH values above 10 and at

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high temperature is made with special glass electrodes designed for such
purposes.
Reagents:pH-4 Buffer Solution:Dissolve 1.012 g anhydrous potassium hydrogen phthalate, KHC8H4O4 in
distilled water and make up to 100 ml in a volumetric flask.
pH-9 Buffer Solution:Dissolve 3.81 g sodium borate deca hydrate (borax) Na 2B4O7. 10H2O in
distilled water and make up to 100 ml.
Procedure:Standardize the PH meter using standard buffer solution of PH 4.0 and 9.2
and then determine the PH of the sample of water or waste water.
Limit No Relaxation
0

5. Alkalinity:IS

0 3025 (P-23) 1986

Method used:- Titrimetric


Alkalinity is the quantitative capacity aqueous media to react with
hydrogen ions. The alkalinity of natural and treated waters is normally due
to the presence of bicarbonates, carbonates and hydroxide compounds of
calcium, magnesium sodium and potassium.

13

Phenolphthalein and methyl orange are the indicators commonly used


for alkalinity titrations phenolphthalein gives pink colour in the presence of
hydroxide or normal carbonates. The change from pink to colour less occurs
at a PH 8.3. Methyl orange gives yellow colour in the presence of all the
three types of alkalinity and is orange in the presence of acid. The colour
change occurs at a PH value of about 4.5.
Principle:Alkalinity is directly determined by titration with 0.02NH 2SO4 using
phenolphthalein and methyl orange indicators.
Ca (OH)2 + H2SO4

CaSO4 + 2H2O

2 CaCO3 + H2SO4

Ca (HCO3)2 + CaSO4

Ca (HCO3)2 + H2SO4

CaSO4 + 2CO2 + 2H2O

Reagents:Sulphuric Acid 0.02 N


Phenolphthalein Indicator
Mixed Indicator
Phenolphthalein Alkalinity:Place 25 ml or 50 ml volume of sample in a conical flask. Adjust the volume
to 50 ml with distilled water. Add phenolphthalein indicator solution. If no
pink colour ation occurs, there is no phenolphthalein alkalinity. If a pink
colour appears then titrate with 0.02NH 2SO4 (to PH 8.3) until the solution
becomes colour less.
Total Alkalinity:14

Add 3 drops of mixed indicator solution to the solution in which


phenolphthalein alkalinity has been determined and titrate against
0.02NH2SO4 (to PH 4.6) to light pink.
General Calculations:If the sulphuric acid used for the titration is exactly 0.02N, Phenolphthalein
alkalinity as CaCO3 mg.
= Vol. of H2SO4 till end point (ml) x N x 1 x 1000
Ml of sample taken
Total Alkalinity as CaCO3 mg
= ml of H2SO4 used x N x 1 x 1000
Ml of sample taken
Limit
Desirable 200 max.
Permissible 600 max.

6. Total Dissolved Solids (TDS) :IS

3025 (P-16)

Method Used:- Gravimetric Method


Solids:Solids is a term applied to all matter except the water contained in liquid
materials and thus the definition of solids refers to the matter that remains as
residue upon evaporation and drying at a definite temperature.
15

TDS:Filter a suitable volume of sample through filter paper or a glass fiber filter
paper. Evaporate the filtered sample in a tare dish. Use platinum dish for
water sample and porcelain dish for sewage and industrial effluents dry the
residue at 103 1080C or at 179-1810C. The increase in weight of dish
equals the total dissolved solids (TDS) It may also be obtained by the
difference between the total solids and total suspended solids.
General Calculation:Initial wt. of dish = W1g
Final wt. of dish = W2g
wt. of TDS

= W2-W1 = W3g

TDS = W3g
Limit
Desirable 200 mg 1 lt.
Permissible 2200 mg 1 lt.

7. Total Hardness:IS

3025 (P-21) 1984

Method Used:- EDTA Titrimetric Method


Hardness is deemed to be the capacity of water for reducing and destroying
the lather of soap. Hardness in water is due to the natural accumulation of
salts from contact with soil and geological formations or it may enter from

16

direct pollution by industrial effuluents. Calcium and magnesium are the


principle cautions causing hardness.
Principle:Calcium and magnesium ions react with EDTA to form soluble complexes
and the completion of reaction is indicated by the colour change of a suitable
indicator such as Erichrome black T(EBT)
Ca2+h2V2

Ca

Reagents: Standard EDTA titrant


Ammonia Ammonium Chloride (Buffer)
Erichrome Black T Indicator (EBT)
Procedure:Place suitable volume of sample in a conical flask and dilute to 50 ml.
Add 1 ml of buffer solution per 50 ml volume of sample. The PH of
the titre should be 10.0.
Add one drop of indicator solution or an appropriate amount of dry
powder.
Titrate with standard EDTA solution slowly, until a reddish tinge
appears and add the last few drops within 3-5 seconds. At the end
point the solution will be blue.
The whole titration procedures should be completed within 5 minutes after
the addition of buffer.
Calculation:Hardness as CaCO3 mg =
Ml EDTA titrant x E x 1000
Ml sample taken
17

Where E = CaCO3 equivalent to 1.0 ml EDTA.


Limit
Desirable 300 max.
Permissible 600 max.
CLASSIFICATION OF HARDNESS:Hardness has been classified into Temporary Hardness and Permanent
Hardness.
The portion of hardness that disappears o prolonged boiling is referred
as temporary hardness and is mainly due to the bicarbonates of calcium and
magnesium which are precipitated as normal carbonates by loss of CO 2 on
heating. The hardness that remains after boiling is known as permanent
hardness and is due to the sulphates, chlorides and nitrates of calcium and
magnesium. Temporary hardness also called carbonates Hardness and
Permanent hardness called Non-carbonates Hardness.
Calculation of carbonate and Non-carbonate Hardness:Carbonates Hardness = Alkalinity (as CaCO3)
Non-Carbonates Hardness = Total Hardness Alkalinity (as CaCO3)

Calcium Hardness:IS

3025 (P-40) 1991

Method:- EDTA Titrimetric Method.


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Principle:The PH of the sample is made sufficiently high (12-13) to precipitate


magnesium as hydroxide and calcium only is allowed to react with EDTA in
the presence of a selective indicator.
Mg2 + 2 NaOH

Mg (OH)2 + 2 Na+

Ca2 + 2 EDTA

Ca (EDTA)2 + 2 Na+

Regents: NaOH (IN)


Murexide Indicator
Standard EDTA titrant 0.02N
Procedure:

Place 50 ml of sample in a conical flask.


Add 2.0 ml of NaOH per 50 ml of sample to produce PH of 12-13.
Add 1 or 2 drops of indicator.
Titrate with EDTA to proper end point.

Calculation:If the EDTA is exactly 0.02 N mgIl calcium as CaCO3 =


Ml EDTA titrant x 1 x 1000
Ml sample taken
MgIl calcium as Ca =
Ml EDTA titrant x E x 1000
Ml sample taken
Limit
Desirable 75 max.
19

x 0.40

Permissible 200 max.


Magnesium Hardness:IS

3025 (P-46) 1994

Calculation:Magnesium as (MgCO3) mg1l =


Mg1l Total Hardness Calcium Hardness as CaCO3
Magnesium (as Mg) mg1l =
Magnesium (as MgCO3) mg1l x 0.244
Limit
Desirable 75 max.
Permissible 200 max.

8. Chloride:IS

3025 (P-32) 1988

Method:- Silver Nitrate Method..


Chloride is the common anion found in water and sewage. The concentration
of chloride in natural water varies from foul milligrams to several thousand
milligrams per liter.
Principle:Silver nitrate reacts with chloride ions to form silver chloride. The
completion of reaction is indicated by the red colour produced by the
reaction of silver nitrate with potassium chromate solution which is added as
an indicator.
20

AgNO3 + Cl

Ag Cl + NO3

2AgNO3 + K2CrO4

Ag2 CrO4 + 2KNO3

Reagents:

Standard Silver Nitrate Titrant (0.0282N)


Potassium Chromate Indicator solution.
Sulphuric Acid
Sodium Hydroxide

Procedure:Place 100 ml sample in a porcelain basin of capacity 300 ml capacity. If the


PH of the sample is in range of 7 to 9.5 it can directly be titrated. If the pH is
not within this range. Adjust the PH to be within this range using sulphuric
acid or sodium hydroxide solution. Add 1 ml potassium chromate indicator
solution. Titrate against standard silver nitrate solution with constant stirring
until a slightest perceptible reddish colour action persists. Conduct blank
containing chlorine free distilled water wasted of sample.
Calculation:Mg 1l Chloride as CL =
S = ml AgNO3 used for sample.
B = ml AgNO3 used for blank.
Limit
Desirable 250 max.
Permissible 1000 max.
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PARAMETERS STUDIES IN WASTE


WATER
1.C.O.D.
Is - APHA 21st Edition
Method:- Digestion Method.
C.O.D. Chemical Oxygen Demand:This test is highly useful to find out the pollution strength of industrial
effluents and sewage. Chemical oxygen Demand as the name implies is the
oxygen requirement of a sample for oxidation of organic and inorganic
matter. As the oxidisable inorganic matter is usually negligible in
comparison with the quantity of organic matter, COD is generally considered
as the oxygen equivalent of the amount of organic matter oxidisable by
potassium dichromate.
Principle:The organic matter of the sample is oxidized to water, CO 2 and ammonia by
refluxion with known excess of potassium dichromate in a 50% sulfuric acid
solution. The excess dichromate is titrated with a standard solution of
ferrous ammonium sulfate solution.
60Fe2+ + Cr2O72+ + 14H+

6F3+ + 2 Cr3+ + 7 H2O

Reagents:22

Mercuric Sulfate Crystals


Potassium dichromate.
Ferrion Indicator
Ferrous Ammonium Sulphate.
Sulfuric Acid.

Procedure:Shake the sample well, so that the contents are mixed thoroughly
Place 50 ml sample in the reflux flask. Add mercuric sulfate according
to chloride concentration of the aliquot.
Measure suitable amount of sulfuric acid in a measuring cylinder.
From this amount initially transfer carefully and slowly 5 ml only to
the reflux flask ad mix thoroughly to dissolve the mercuric sulfate.
Cool while mixing to avoid possible loss of volatile matter in the
sample.
Pipette a pre-determined quantity of potassium dichromate solution in
to the flask and mix well.
Carefully add the remaining sulfuric acid in the measuring cylinder to
the reflux flask, cooling the flask simultaneously under tap.
Add a few antidumping granules and place the flask in position.
Attach the condenser and start the cooling water reflux for 2 hrs.
Remove the flame, allow the flask to cool and wash the condenser
with distilled water into the flask.
Transfer the contents of the flask to a 500 ml conical flask and cool it
well.
Add 2 to 3 drops of ferroin indicator and titrate with ferrous
Ammonium sulfate solution.
The end point is the sharp colour change from blue green to reddish
brown.
Conduct a blank using distilled water in place of sample.
23

Calculation:Mg1l COD =
B = Ml of FAS used in titration of Blank sample.
S = Ml of FAS used in titration of sample.
Limit 250 mg 1lt. max.

2. Oil & Grease:IS


Limit

3025 (P-39)
10 max.

Method:Silver Extraction Method


The determination of oil and grease includes all the substances that are
extractable by the specified solvent. Generally the substances that are
extractable are oils, fats and waxes. It is to be noted that the results obtained
indicates only the non-volatile fraction of these materials. Determination of
the volatile fraction is beyond the scope of this book.
Principle:Oil and grease, and other extractable matters are dissolved in suitable
solvent and separated from the aqueous phase. The solvent layer is then
evaporated and the residue is weighed as oil and grease.
24

Reagents: Sulfate Acid.


Petroleum ether
Procedure: Place 1000 ml or appropriate volume of the sample in a suitable
separating funnel.
Add 5 ml sulfuric acid per liter of sample.
Rinse the sample bottle with 15 ml petroleum ether and add the
rinsing to the separating funnel. Add further 25 ml ether to the funnel
and shake vigorously for 2 minutes.
Draw the aqueous phase in to a clear container and transfer the ether
layer through a filter paper containing enough sodium sulphate wetted
with petroleum ether to a clean, tarred distilling flask.
Continue the extraction twice and add the ether extracts to the
distilling flask after passing through a cone of anhydrous sodium
sulfate Na2SO4 to remove traces of water.
Distill off the ether in the distilling flask until about 10 ml remains in
the flask. Dry on water bath.

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