ANALYSIS OF WATER (Laboratory Test)

Physical Characteristics of Water

1. Turbidity of Water
The turbidity is measured by a turbidity rod or by a turbidity meter with optical observations
and is expressed as the amount of suspended matter in mg/l or parts per million (ppm).

For water, ppm and mg/l are approximately equal.

The standard unit is that which is produced by one milligram of finely divided silica (fuller’s
earth) in one litre of distilled water.

Turbidity Meters
Turbidity Rod:
The turbidity can be easily measured in the field with the help of a turbidity rod. It consists of
an aluminium rod which is graduated as to give turbidity directly in silica units (mg/l)
Turbidimeter:
The turbidity can be easily measured in the laboratory with the help of a instruments called
turbidity meter. In general, a turbidity meter works on the principle of measuring the
interference caused by the water sample to the passage of light rays.
Jackson’s candle Turbidimeter:
The height of water column will therefore be more for less turbid water and vice versa.
Longer the light path lower the turbidity. Such a turbidimeter can not measure turbidites
lower than 25 JTU.

It can be used for natural sources only and can not be used to measure the turbidity of treated
water supplies, for which Baylis turbidity meter or modern nephelometers are used.
Baylis Turbidimeters
One of the two glass tubes is filled with water sample (whose turbidity I to be measured) and
the other is filled with standard water solution of known turbidity. The electric bulb is lighted
and the blue colour in both the tubes is observed from the top of the instrument.
Modern Nephelometer: for low turbidity less than 1 unit.
NTU – Nephelometric Turbidity Units
FTU – Formazin Turbidity Units

Ratio turbidimeter: River water has maximum amount of turbidity.

2. Colour
The presence of colour in water is not objectionable from health point of view, but may spoil
the colour of the clothes being washed. The standard unit of colour is that which is produced
by one milligram of platinum cobalt dissolved in one litre of distilled water.

For public supplies, the colour number on cobalt scale should not exceed 20 and should be
preferably less than 10.

Colour determined by an instrument is known as tintometer.

3. Taste and Odour
The extent of taste or odour present in a particular sample of water is measured by a term
called odour intensity, which is related with the threshold odour or threshold odour
number.
Water to be tested is therefore gradually diluted with odour free water, and the mixture at
which the detection of odour by human observation is just lost, is determined. The number of
times the sample is diluted represents the threshold odour number.

For public supplies, the water should generally free from odour, i.e. the threshold number
should be 1 and should never exceed 3.

4. Temperature of Water
For potable water, temperature of about about C is desirable. It should not be more
than C.

5. Specific Conductivity
The total amount of dissolved salts present in water can be easily estimated by measuring the
specific conductivity of water.

Chemical Characteristics of Water

1. Total Solids and Suspended Solids
Total solids (suspended solids + dissolved solids) can be obtained by evaporating a sample of
water and weighing the dry residue left and weighing the residue left on the filter paper.

The suspended solid can be found by filtering the water sample. Total permissible amount of
solids in water is generally limited to 500 ppm.

2. pH value of Water

If concentration increases, pH decreases and then it will be acidic.

If concentration decreases, pH increases and then it will be alkaline.

pH + pOH = 14

if the pH of water is more than 7, it will be alkaline and if it is less than 7, it will be acidic.

The alkalinity is caused by the presence of bicarbonate of calcium and magnesium or by the
carbonates of hydroxides of sodium, potassium, calcium and magnesium.

Some, but not all of the compounds that cause alkalinity also cause hardness.

pH Measurement:
the pH value of water can be measured quickly and automatically with the help of
a Potentiometer.
The pH can also be measured by indicators as given below:
Permissible pH value for public supplies may range between 6.6 to 8.4.

The lower value of pH may cause incrustation, sediment deposits, difficulty in chlorination.

3. Hardness of Water
Hard waters are undesirable because they may lead to greater soap consumption, scaling of
boilers, causing corrosion and incrustation of pipes, making food tasteless etc.

Temporary Hardness: If bicarbonates and carbonates of calcium and magnesium are present
in water, the water is render hard temporarily as this hardness can be removed to some extent
by simple boiling or to full extent by adding lime to water. Such a hardness is known as
temporary hardness or carbonate hardness.
Permanent Hardness: If sulphates, chlorides and nitrates of calcium or magnesium are
present in water, they can not be removed at al by simple boiling and therefore, such water
require special treatment for softening. Such a hardness is known as permanent hardness or
non-carbonate hardness.
It is caused by sulphates, chlorides, nitrates of Ca and Mg.

Carbonate hardness = Total hardness or Alkalinity (which ever is less)

Non-carbonate hardness = Total hardness – Alkalinity

 Carbonate hardness is equal to the total hardness or alkalinity which ever is less
  Non-carbonate hardness is the total hardness in excess of the alkalinity. If the
alkalinity is equal to or greater than the total hardness, there is no non-carbonate
hardness.
 One French degree of hardness is equal to 10mg/l of CaCO3.
 One British degree of hardness is equal to a hardness of 14.25mg/l.
 Water with hardness upto 75 ppm are considered soft and above 200 ppm are
considered hard and in between is considered as moderately hard.
 Underground waters are generally harder than surface waters.
 The prescribed hardness limit for public supplies range between 75 to 115 ppm.
4. Chloride Content
The chloride content of treated water to be supplied to the public should not exceed a value of
about 250 ppm.

The chloride content of water can be measured by titrating the water with standard silver
nitrate solution using potassium chromate as indicator.

(5) Nitrogen Content

The presence of nitrogen in water may occur in one or more of the following reasons:

1. Free ammonia: It indicates very first stage of decomposition of organic matter. It

should not exceed 0.15mg/l
2. Albuminous or Organic Matter: It indicates the quantity of nitrogen present in
water before the decomposition of organic molten has started. It should not exceed
0.3mg/l
3. Nitrites: Not fully oxidized organic matter in water.
4. Nitrates: It indicates fully oxidized organic matter in water (representing old
pollution).

 Nitrites is highly dangerous and therefore the permissible amount of nitrites in water
should be nil.
 Ammonia nitrogen + organic nitrogen = kjeldahl nitrogen
 Nitrates in water is not harmful. However the presence of too much of nitrates in
water may adversely affect the health of infants causing a disease
called methemoglobinemia commonly called blue baby disease.
 The nitrate concentration in domestic water supplies is limited to 45 mg/l.
6. Metal and other chemical substances in water:
Iron – 0.3ppm, excess of these cause discolouration of clothes.

Manganese – 0.05ppm

Copper – 1.3ppm
Sulphate – 250 ppm

Fluoride – 1.5 ppm, excess of this effects human lungs and other respiratory organs.

Fluoride concentration of less than 0.8 – 1.0 ppm cause dental cavity (tooth decay). If
fluoride concentration is greater than 1.5ppm, causing spotting and discolouration of teeth (a
disease called fluorosis).

7. Dissolved gases
Oxygen gas is generally absorbed by water from the atmosphere but it being consumed by
unstable organic matter for their oxidation. Hence, if the oxygen present in water is found o
be less than its saturation level, it indicates presence of organic matter and consequently
making the waters suspicious.

Biological Oxygen Demand (BOD):

The extent of organic matter present in water sample can be estimated by supplying oxygen
to this sample and finding the oxygen consumed by the organic matter present in water. This
oxygen demand is known as Biological oxygen demand (BOD).

It is not practically possible to determine ultimate oxygen demand. Hence, BOD of water
during the first five days at C is generally taken as the standard demand.

= Loss of oxygen in mg/l x dilution factor.

The BOD of safe drinking water must be nil.

Bacterial and Microscopic Characteristics of Water

Five types of parasitic organisms (i.e. bacteria, protozoa, viruses, worms and fungi) are
generally known to be infective to main and are found in water.

1. Bacteria
These are the minute single cell organisms possessing no defined nucleus and having no
green material to help them manufacture their own food. They are reproduced by binary
fusion and may of various shapes and sizes are 1 to 4 microns, examined by microscope.

a) Non-disease causing bacteria – Non pathogenic bacteria.

b) Disease causing bacteria – Pathogenic bacteria.

2. Protozoa
These are single cell animals and are the lowest and the simplest form of animal life. They
are bacteria eaters and thus destroy Pathogens. They are counted by microscope.

3. Viruses
4. Worms
These are the larva of flies.

5. Fungi
These are those plants which grow without sunlight and live on other plants or animals, dead
or alive.

Classification of bacteria based on oxygen requirement:

1. Aerobic bacteria: Those which require oxygen for their survival.

2. Anaerobic bacteria: Those which flourish in the absence of free oxygen.
3. Facultative bacteria: Those which can survive with or without free oxygen.
Pathogenic bacteria
These can be tested and counted in the laboratories but with great difficulty. These tests are
therefore, generally not performed in routine to check up of the water quality. The usual
routine tests are generally conducted to detect and count the presence of coliforms which in
themselves harmless organisms, but their presence or absence indicates the presence or
absence of pathogenic bacteria.

Methods to measure the presence of coliform bacteria:

1. Membrane filter technique (modern technique)

 2. Mixing different dilution of a sample of water with lactose froth and incubating them
in test-tubes for 48 hours at C. the presence of acid or carbon dioxide gas in
tubes will indicate the presence of coliform bacteria.
Most probable number (MPN) represent the bacterial density.

Coliform index
It may be defined as the reciprocal of the smallest quantity of a sample which would give a
positive portion. Coliform sometimes called bacteria coli (B-coli) or Escherichia (E-coli) are
harmless aerobic micro-organisms.

If not more than 1 coliform is present per 100ml of water, then water is said to be safe for
drinking.

Objective:

 To determine chemical parameters such as hardness, alkalinity, and chemical oxygen demand
COD) of water samples.

Theory:

It is needless to emphasize the importance of water in our life. Without water, there is no life
on our planet. We need water for different purposes. We need water for drinking, for
industries, for irrigation, for swimming and fishing, etc.
Water for different purposes has its own requirements for composition and purity. Each body
of water needs to be analysed on a regular basis to confirm to suitability. The types of
analysis could vary from simple field testing for a single analyte to laboratory based multi-
component instrumental analysis. The measurement of water quality is a very exacting and
time consuming process, and a large number of quantitative analytical methods are used for
this purpose.

Total hardness:
Theory:

Hardness in water is that characteristic, which “prevents the lathering of soap”. This is due to
presence in water of certain salts of calcium, magnesium and other heavy metals dissolved in
it. A sample of hard water, when treated with soap does not produce lather, but on other hand
forms a white scum or precipitate. This precipitate is formed, due to the formation of
insoluble soaps of calcium and magnesium.

Thus, water which does not produce lather with soap solution readily, but forms a white curd,
is called hard water. On the other hand, water which lathers easily on shaking with soap
solution, is called soft water. Such water consequently does not contain dissolved calcium
and magnesium salts in it.

Temporary or carbonate hardness: It is caused by the presence of dissolved bicarbonates

of calcium, magnesium and other heavy metals and the carbonate of iron. Temporary
hardness is mostly destroyed by mere boiling of water, when bicarbonates are decomposed,
will produce insoluble carbonates or hydroxides, which are deposited as a crust at the bottom
of vessel.

Permanent or non-carbonate hardness: It is due to the presence of chlorides and sulphates

of calcium, magnesium, iron, and other heavy metals. Unlike temporary hardness, permanent
hardness is not destroyed on boiling.

The degree of hardness of drinking water has been classified in terms of the equivalent
CaCO3 concentration as follows:
In a hard water sample, the total hardness can be determined by titrating the Ca2+ and
Mg2+ present in an aliquot of the sample with Na2EDTA solution, using NH4Cl-NH4OH
buffer solution of pH 10 and Eriochrome Black-T as the metal indicator.
Na2H2Y (Disodium EDTA solution) → 2Na+ + H2Y-
Mg2+ + HD2- (blue) → MgD (wine red) + H+
D (metal-indicator complex, wine red colour) + H2Y- →Y- (metal EDTA complex colourless)
+ HD- (blue colour) + H+
Ethylenediamine tetra-acetic acid (EDTA) and its sodium salts form a chelated soluble
complex when added to a solution of certain metal cations. If a small amount of a dye such as
Eriochrome black T is added to an aqueous solution containing calcium and magnesium ions
at a pH of 10 ± 0.1, the solution will become wine red. If EDTA is then added as a titrant, the
calcium and magnesium will be complexed. After sufficient EDTA has been added to
complex all the magnesium and calcium, the solution will turn from wine red to blue. This is
the end point of the titration.

Units of Hardness:

1. Parts per million (ppm): Is the parts of calcium carbonate equivalent hardness per
106 parts of water, i.e, 1 ppm = 1 part of CaCO3 eq hardness in 106 parts of water.

2. Milligram per litre (mg/L): Is the number of milligrams of CaCO3 equivalent hardness
present per litre of water. Thus:
1 mg/L = 1 mg of CaCO3 eq hardness per L of water.

3. Clarke’s degree (oCl): Is number of grains (1/7000 lb) of CaCO3 equivalent hardness per
gallon (10 lb) of water. Or it is parts of CaCO3equivalent hardness per 70,000 parts of water.
Thus,
1oClarke = 1 grain of CaCO3 eq hardness per gallon of water.

4. Degree French (oFr): Is the parts of CaCO3 equivalent hardness per 105 parts of water.
Thus,
1o Fr = 1 part of CaCO3 hardness eq per 105 parts of water.

Relationship Between Various Units of Hardness:

1ppm =1 mg/L=0.1oFr =0.07oCl
1mg/L=1 ppm=0.1oFr =0.07oCl
1oCl=1.43oFr=14.3 ppm=0.7omg/L
1oFr=10 ppm=10 mg/L=0.7oCl

Alkalinity:
Theory:

 Alkalinity is an aggregate property of the water sample which measures the acid-
neutralizing capacity of a water sample.
 It can be interpreted in terms specific substances only when a complete chemical
composition of the sample is also performed.
 The alkalinity of surface water is due to the carbonate, bicarbonate and hydroxide
content and is often interpreted in terms of the concentrations of these constituents.
 Higher the alkalinity, greater is the capacity of water to neutralize acids. Conversely,
the lower the alkalinity, the lesser will be the neutralizing capacity.

Alkalinity of sample can be estimated by titration with standard H2SO4 or HCI solution.
Titration to pH 8.3 or decolourisation of phenolphthalein indicator will indicate complete
neutralization of OH- and 1/2 of CO32-, while to pH 4.5 or sharp change from yellow to
orange of methyl orange indicator will indicate total alkalinity.
To detect the different types of alkalinity, the water is tested for phenolphthalein and total
alkalinity, using Equations:

Where,

A = titrant (mL) used to titrate to pH 8.3

B = titrant (mL) used to titrate to pH 4.5
N = normality of the acid (0.02N H2SO4 for this alkalinity test)
50,000 = a conversion factor to change the normality into units of CaCO3

Once PA and TA are determined, then three types of alkalinities, i.e, hydroxides, carbonates
and bicarbonates can be easily calculated from the table:
 Chemical Oxygen Demand (COD):
Theory:
COD is used as a measure of oxygen equivalent to organic matter content of a sample that is
susceptible to oxidation by a strong chemical oxidant.
For samples from a specific source, COD can be related empirically to BOD. COD
determination has advantage over BOD determination in that the result can be obtained in
about 5 hours as compared to 5 days required for BOD test.

The organic matter gets oxidized completely by K2Cr2O7 in the presence of H2SO4 to produce
CO2 and H2O. The excess of K2Cr2O7 remained after the reaction is titrated with ferrous
ammonium sulphate. The dichromate consumed gives the O2 required for oxidation of
organic matter.

Procedure:

 Under the chemical content, select the tests- Hardness, Alkalinity or COD.

a. Determination of Hardness of Water Sample

1. Select the titrant.

2. Adjust the speed of the drops from the burette.
3. Adjust the molarity of titrant.
4. Select a definite volume of water sample.
5. Choose the indicator & start the titration.
6. When colour changes from wine red to blue click the "stop" button & note the volume of
EDTA used.
7. Then calculate the hardness of water sample in ppm using the equation as follows.

Observations And Calculations:

 Volume of EDTA used=..................mL.
Molarity of EDTA =..................M.
Volume of the water sample =..................mL.
Therefore the total hardness of the sample is

= =.................ppm.

Result:

Total Hardness of the water sample = ..................ppm.

b. Determination of Alkalinity of Water Sample.

1. Select the titrant.
2. Select the normality.
3. Adjust the speed of the drops from the burette.
4. Select the titrate & choose a definite volume of the water sample.
5. Select the indicator, phenolphthalein to get a pink colour.
6. Stop titration when the solution becomes colourless & calculate phenolphthalein alkalinity
(PA) as CaCO3 (mg/L) using the equation. Let A is the volume of titrant (mL) used in the
titration (V1).
7. Add methyl orange to the same flask & continue titration till the colour changes from yellow
to orange. The total volume of titrant corresponds to total alkalinity (TA) as CaCO3 (mg/L).
Let B is the total volume of titrant (mL) consumed with both the indicators (V2).

Observations and Calculations:

Volume of HCl corresponding to phenolphthalein end point (A)=..................mL.

Normality of acid =..................N
Volume of the water sample =..................mL.
 Normality of water corresponding to phenolphthalein end point =

=..................ppm.
Volume of HCl corresponding to methyl orange end point (B)=..................mL.
Normality of acid =..................N
Volume of the water sample =..................mL.
Normality of water corresponding to methyl orange end point =

=..................ppm.

Results:

Alkalinity is due to............ =..............ppm.

c. Determination of COD of water sample

1. Select the water sample.

2. To reflux the contents in the RB flask click the "switch on mantle" button.
3. Click "start titration" to titrate the contents.
4. Select the normality of ferrous ammonium sulphate (FAS).
5. Start titration & note the volume of titrant consumed when colour changes from bluish green
to wine red. (Let the volume of titrant be V2 mL).
6. Repeat the same with the blank (Let the volume of the titrant be V1mL).
7. COD calculated using the equation.

Observations And Calculations:

Volume of FAS used= (V1-V2) =..................mL.
Normality of FAS =..................N.
Volume of the water sample =..................mL.
Therefore COD of the water sample

= =..............ppm.

Result:

COD of water sample =....................ppm.