Name:ArnabKrPahari

RollNo.:133180006
EXPERIMENT NO. 1
pH VALUE
Date:28.07.13
Aim:
To measure the pH of two unknown solutions.

Principle:
The basic principle ofelectrometricpHisdeterminationoftheactivityofthehydrogen
ionsbypotentiometricmeasurementusingaglasselectrodeandareferenceelectrode.A
pH meter measures theelectrochemical potential between aknownliquid inside the
glasselectrodeandtheunknownsamplesolution.pHofhydrogenionactivitydetermines
theintensityoftheacidityoralkalinityofasolution.
Numerically pH is expressed as the logarithm of the reciprocal of the hydrogen ion
concentrationinmolesperliteratagiventemperature.
pH=log[H+]

Apparatus:
(a) pH meter: The electrometric pH meter determines the activity of hydrogen ions by
potentiometic measurements using a glass electrode and a reference electrode.
(a) Glass wares such as round bottom volumetric flask, beaker, weighing balance

Reagents:
(a) Distilled water
(b) pH standard solutions:
(i) Potassium hydrogen phthalate (KHC8H8O4) (pH=4.008)
(ii) Potassium dihydrogen phosphate (KH2PO4) and Disodium hydrogen
phosphate (Na2HPO4) (pH=7.413)

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Procedure:

(1) The glasswares such as volumetric flasks and beakers were properly washed and
rinsed in distilled water.
(2) 0.912 g of potassium hydrogen phthalate was weighed and dissolved in 100 ml of
distilled water.
(3) 0.1263 g of potassium dihydrogen phosphate and 0.3943 g of disodium hydrogen
phosphate was dissolved in 100 ml of distilled water.
(4) The pH of the two standard solutions prepared was recorded by dipping the electrodes
of the electrometric pH meter.

Result:

The pH of solution I containing potassium hydrogen phthalate is 3.98 and solution II containing
potassium dihydrogen phosphate and disodium hydrogen phosphate is 7.25

Environmental significance:

Determination of pH is one of the most frequently used tests in the analysis of water
and waste water.
Water or other solvents having a very high or low pH are not feasible for drinking and
other domestic purposes. The concentration range suitable for most biological life is
quite narrow i.e. typically 6-9.

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EXPERIMENT NO. 2
CONDUCTIVITY
Date:28.07.09
Aim:
To measure conductivity of an unknown sample solution.

Principle:
The ability of an aqueous solution to carry electric current is numerically expressed as
conductivity. It depends on the presence of ions, their total concentrations, mobility, valence,
relative concentrations and the temperature of measurement. Solutions of mostly inorganic
compounds are good conductors.
The physical measurement made in determination of conductivity in a laboratory is
usually made by measuring the resistance of the sample in ohms. The magnitude of the resistance
measured depends on the characteristics of the conductivity cell used. For measurement of
conductivity therefore two measurements are needed, i.e. measurement of the cell constant(C)
and measurement of the resistance of the sample (R) which is given as follows:
C=ks/Gs
Also, conductance of a solution can be calculated as follows:
Conductance G = 1/R
G = k (A/L),
Where k is the conductivity, A is the surface area; L is the distance between electrodes.
The unit of conductivity k is given by milli siemens per meter (mS/m).

Apparatus:
(1) Conductivity meter
(2) Glass wares such as round bottom volumetric flasks, beaker, pipette with bulbs.

Reagents:
(a) Distilled Water

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(b) Standard Potassium Chloride solution of 0.01 N

Procedure:
(1) The conductivity cell was calibrated by rinsing with 0.01 N standard KCl solution.
(2) The unknown sample solution provided was diluted with distilled water and volume
made up to 50 ml in a volumetric flask.
(3) A portion of the solution was taken for rinsing of the conductivity cell. Then another
portion of the same sample solution was taken in a beaker for measuring the
conductivity by dipping both the conductivity electrode and the electrode for sensing
the temperature of the solution.
(4) Finally the temperature and the conductivity values were recorded.

Sample reading:

Conductivityvalueofthedilutedsamplewas0.185mS/mat32C.

Result / Calculation:

The conductivity of the unknown sample at 25 C was calculated as follows:

1.94
C 32 = C 25 1 32 25
100

1.94
=> 0.185 = C 25 1 32 25
100

=> 0.185 = C 25 [1 + 0.1358]

=> C 25 = 0.185/ 1.1358 = 0.163 mS/m

The conductivity of the unknown sample is 0.163 mS/m at 25 C

Environmental significance:

Conductivity is another physical parameter which determines water quality and

qualifies it if fit for drinking, other domestic purpose, irrigation based on the presence
of ions.

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The conductivity of a water sample is directly related to the presence of cations and
anions in water which indicates the presence of dissolved solids in water. Thus
measurement of conductivity is an indirect way of subjective assessment of total
dissolved solids in raw water and wastewater, in treatment plants.

Water having high dissolved solids can cause corrosion of metal surfaces and scaling
of industrial equipments and domestic sanitary items. Increase amount of dissolved
solids may give mineral taste to water.

Conductivity is used to determine ionic strength of a solution.

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EXPERIMENT NO. 3
TURBIDITY
Date: 27.07.09
Aim:
To measure turbidity of an unknown sample solution.

Principle:
The measurement of turbidity by nephelometric method is based on the comparison of
the intensity of light scattered by the sample solution under defined conditions with the intensity
of light scattered by a standard reference suspension under the same conditions. Formazin
polymer is used as the standard reference suspension. The turbidity of a specified concentration
of formazin suspension is 4000 NTU.
Turbidity can be determined for any water sample which is free from debris and rapidly settling
sediments. Often use of dirty glass wares and presence of air bubbles interfere while measuring
the turbidity values.

Apparatus:
(a) Turbidimeter
(b) Sample tubes
(c) Glasswares such as round bottom volumetric flasks (50 ml), Beakers (100 ml), Pipette
with bulb.

Procedure:
(1) The unknown sample was taken in the clean volumetric flask (50 ml).
(2) The volume was made upto the mark i.e. 50 ml with distilled water using a beaker
and finally with a pipette. It was mixed thoroughly for removal of bubbles if any.
(3) The turbidimeter was calibrated and required amount of the diluted sample was
taken for analysis in the sample tubes.

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(4) The values that appeared in the display screen were recorded.

Sample reading:
Readingoftheturbidimeterwas44.8NTU.

Result:

The turbidity value of the given unknown sample solution was 44.8 NTU.

Environmental Significance:

Turbidity is an important parameter that determines drinking water quality. Hence this
experiment is an important technique for water quality control.
Turbidity is an expression of the clarity of water and the clarity of a natural water
body is a major determinant of the efficiency of the water treatment plants. Clarity of
water is also important for producing products destined for human consumption and
in many manufacturing operations.

Turbidity in water is caused by suspended and colloidal matter such as clay, silt,
finely divided organic and inorganic matter; it is an expression of optical property and
is often correlated with size, shape and refractive index of the particles which affect
the light scattering properties of the suspension.

Excessive turbidity in water bodies reduces the penetration of sunlight thus affecting
photosynthesis of microscopic plants and algae thereby disturbing the overall
environmental balance.

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EXPERIMENT NO. 4
IRON
Date:11.08.09
Aim:
To measure the total iron (ferrous & ferric) content of an unknown sample solution.

Principle:
Iron is brought into solution, reduced to ferrous sulphate by boiling with acid and
hydroxylamine and treated with 1, 10 phenanthroline at a pH of 3.2 to 3.3. Three molecules of
phenanthroline chelate each atom of ferrous iron to form an orange red complex. The coloured
solution obeys Beers law, which states that whenabeamofmonochromaticradiationisdirected
atasamplesolution the dissolvedcompoundsabsorbultraviolet(UV)orvisiblelight,absorptive
capacityisdirectlyproportionaltotheconcentrationofthedissolvedcompounds.Theamountof
radiationabsorbedbystocksolutionsofironfordifferentknownconcentrationsandunknown
sample solution are measured by spectrophotometer and the absorbance values of the stock
solutionsisplottedagainsttherespectiveconcentrationtoobtainastandardcalibrationcurve.
Theironcontentoftheunknownsamplesolutionisderivedfromthecalibrationcurve.

Apparatus:
(a) Volumetric flasks, 50 ml, 100 ml & 250 ml
(b) Conical flasks, 250 ml
(c) Pipettes, 5 ml and 10 ml
(d) Hot plate

Reagents:
(a) Conc. hydrochloric acid (HCl)

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(b) Hydroxylamine solution: 10 g of NH4OH.HCl was dissolved in distilled water
and volume was made up to 100 ml.
(c) Ammonium acetate buffer solution: 25 g of ammonium acetate (NH4C2H3O2) was
dissolved in 15 ml of distilled water and 70 ml of conc. (glacial) acetic acid was added to
make the buffer solution.

(d) Phenanthroline solution: 100 mg of 1, 10 phenanthroline monohydrate

(C12H8N2.H2O) was dissolved in 100 ml of distilled water by stirring and heating at about 80

C.

(e) Stock iron solution: 0.1404 gm of ferrous ammonium sulphate was dissolved in 5
ml of distilled water and 2 ml of conc. H 2SO4 was added to it. 0.1 N KMnO 4 solution was
added to it drop wise till the solution turned faint pink colour. Then it was diluted and volume
was made up to 100 ml. Here, 1 ml of the solution corresponds to 200 g of Fe.

(f) Standard Fe solutions:

(i) From the above solution, i.e. 1 ml = 200 g of Fe or 200ppm, 5 standard Fe solutions
were prepared by taking 1 ml, 2ml, 3 ml, 4 ml and 5 ml corresponding to 2ppm,
4ppm, 6ppm, 8ppm and 10ppm respectively.

Procedure:
1. To each of the 5 standard Fe solutions, 1ml of hydroxylamine (NH 2OH.HCl) solution,
1ml of sodium acetate, 10 ml of phenanthroline solution was added and then volume of all
was made up to 100 with distilled water.
2. Total Iron Content:
The unknown sample solution provided was diluted to 50 ml and the total diluted sample
was taken in a 250 ml conical flask. Then 2ml of conc. HCl and 1ml NH2OH.HCl solution
was added and heated till boiling. Finally 10 ml of ammonium acetate buffer (NH 4C2O3H2)
solution and 2 ml phenanthroline solution was added, volume was made upto the mark. It
was kept as such till the development of colour.
3. Ferrous Iron Content:
The unknown sample solution was acidified with 2ml conc. HCl, volume was made upto
50ml, then 20ml phenanthroline solution and 10ml NH4C2O3H2 solution was added and
thouruoghly mixed, finally diluted to 100ml.

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4. The absorbance of the unknown sample solutions, the blank and the standard iron
solutions at 510nm were measured in a spectrophotometer. Then the calibration curve was
drawn by taking concentration of standard solutions in X-axis and absorbance readings in Y-
axis.

Absorbance readings:

Sl. No. Concentration of the standard Fe Absorbance recorded.

solution in mg/l (ppm)

1 Blank 0.0

2 2 0.384

3 4 0.776

4 6 1.058

5 8 1.451

6 10 1.331

8 Unknown sample (Total Iron) 0.549

9 Unknown sample (Ferrous Iron) 0.243

Calibration Curve:

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Calculation:

The above calibration curve for absorbance versus concentration satisfies to the equation

y = 0.159x, where

y = Absorbance

x = Concentration in mg/L

Absorbance for total iron was measured as 0.549 and for ferrous ion as 0.243, therefore,

0.549 = 0.159 x
0.549
x= = 3.452 mg/L (Total Iron)
0.159

Similarly,

0.243= 0.159 x
0.243
x= = 1.528 mg/L(Ferrous ion)
0.159

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Result: Thus, total iron content of the unknown sample solution was found to be 3.452mg/L and
ferrous iron content was found to be 1.528 mg/L

Environmental significance:

Water with higher content of iron becomes turbid due to oxidation when exposed to
air and is not acceptable from aesthetic point of view. Oxidation of Fe (II) to Fe (III)
forms reddish colloidal precipitates due to formation of insoluble ferric oxide.
Iron in water also imparts a different taste and colour to foods which is detectable
even at very low concentrations and such taste is generally not acceptable for
human consumption.

Presence of elevated iron levels in water also causes staining in industrial activities
like in large laundries, plumbing and cooking utensils.

EXPERIMENT NO. 5
SODIUM
Date: 11.08.09

Aim:
To measure the sodium content of an unknown sample solution by flame emission
photometric method.

Principle:
The principle of operation of the flame photometer is simple. The unknown sample
solution is sprayed as affine mist into a non-luminous flame, which becomes colored according
to the characteristics emission of sodium (Na: 589 nm). A photodetector which views the flame

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through a selected narrow band of optical filter that only passes the wavelengths centered on the
characteristics emission of the sodium (Na) monitors the flame. The output of the photodetector
is fed to an electronic module, which provides digital output of the concentration of sodium (Na).
Before analyzing the unknown sample solution, the system is standardized with solution of
known concentrations of sodium.
Apparatus:
(a) Flame photometer
(b) Volumetric flasks (100 ml)
(c) Conical flasks (250 ml)
(d) Pipette (5 ml)

Reagents:
1) Stock sodium solution: 0.2542 g dried sodium chloride (NaCl) was dissolved in
deionised water and then volume of the solution is made up to 100 ml. This was
the stock sodium solution having strength of 1 ml = 1 mg Na or 1000 ppm.
2) Standard sodium solution: For the standard stock solutions, 2 ml, 4ml, 6ml, 8ml
and 10 ml of the stock sodium solution was taken and was diluted to 100 ml to get
a strength of 20 ppm, 40 ppm, 60 ppm, 80 ppm and 100 ppm sodium respectively.
3) Deionized water

Procedure:

1. The unknown sample solution provided was diluted to 100 ml with deionized
water.
2. The emission intensity readings of the diluted sample, the blank and the standard
sodium solutions were measured in the flame photometer.

Flame photometer readings:

Sl. No. Concentration of the standard Na Intensity reading

solution in mg/L recorded.

1 20 21.32

2 40 39.64
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3 60 65.91

4 80 82.11

5 100 100.46

6 Unknown sample 63.03

Result: The sodium content of the unknown sample solution was found to be 63.03 mg/L.

Environmental significance:

Sodium is the sixth most abundant element on earth and is found in all natural water
bodies. The ratio of sodium to total cations is important in agriculture uses and human
physiology.
Soil permeability is affected when sodium is present in higher concentrations in water
and such water becomes unusable for agriculture purpose.

Persons having cardiac problems are recommended for consumption of water or food
with low sodium concentration.

About 2-3 mg/L of sodium is recommended for feed waters in high pressure boilers.

EXPERIMENT NO. 6
ALKALINITY
Date: 10.08.09
Aim:
To measure the alkalinity of an unknown sample solution.

Principle:

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Alkalinity is defined as the property of water containing dissolved salts, characterized by
the ability to neutralize acids. It is the quantitative capacity of water to react with a strong
acid to a designated pH and the measured values vary to a significant extent with the end
point pH used. The hydroxyl ions present in a water sample as a result of dissociation or
hydrolysis of solute reacts with the acid added. Alkalinity thus depends on the end point
pH used.

Apparatus:
(i) Volumetric flasks (1000 ml) & conical flasks (250 ml)
(ii) Burette (50 ml) & Pipette (5 ml)
(iii) pH meter

Reagents Preparation:
(a) Sodium carbonate solution (0.05 N):
2.5 g of the provided sodium carbonate (Na2CO3) salt was dissolved in distilled
water and then volume was made up to 1000 ml in a volumetric flask.
(b) Standard Sulphuric acid (0.1 N):
3 ml of conc. sulphuric acid (H 2SO4) was diluted with distilled water and volume
was made up to 1 L.
(c) Phenolphthalein indicator
(d) Methyl orange indicator
Procedure:
1. The standard sulphuric acid prepared was standardized against 0.05 N sodium carbonate
solution. The colour of Na2CO3 solution changed from colourless to pink. The volume of
acid used for standardization was noted down. Normality of the standard acid was
calculated.
2. The standard acid prepared was diluted by taking 200 ml of acid and making up the
volume to 1000 ml by adding distilled water. The normality of the acid after dilution was
calculated.
3. The unknown sample solution was taken and diluted up to 100 ml. 10 ml of the diluted
solution was taken for titration. 2 drops of phenolphthalein indicator was added and while

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titrating against sulphuric acid in the burette, colour changed from pink to colourless. The
volume of acid consumed was noted down and also the pH of the solution was checked.
4. Finally 2 drops of methyl orange indicator was added and titration was continued till
colour changed to orange. The volume of acid consumed was noted down and pH of the
solution was checked in the pH meter.

Titration Reading:

Sl. Titration for Initial burette Final burette Volume of H2SO4

No. reading reading consumed in ml

1 Phenolphthalein alkalinity 0 0.5 0.5

2 Total alkalinity 0 1.8 1.8

Calculation/ Result:

(1) Then normality of the acid was calculated as follows:

( A B)
Normality (N) = ;
(53 C)

Where,
A = Weight of Na2CO3 taken = 2.5 gm
B = Volume of Na2CO3 solution consumed during standardization = 10 ml
C = Volume of acid used in ml = 5ml
( 2.5 10)
Thus, normality of standard sulphuric acid = = 0.094 N 0.01N
(53 5)

(0.094 200)
(2) The normality of the diluted acid = = 0.019 N 0.02N
1000

Alkalinity, mg CaCO3/L = ;

Where,
A= ml standard acid used
N= normaliy of standard acid used

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(0.5 0.019 50000)
(3) Phenolphthalein alkalinity = = 47.5 mg CaCO3
10
Thus, Phenolphthalein alkalinity to pH - 7.73 = 47.5mg CaCO3/ml

(1.8 0.019 50000)

(4) Total alkalinity = = 171 mg CaCO3
10
Thus, Total alkalinity to pH - 2.99 = 171mg CaCO3/ml

Environmental significance:

Alkalinity plays an important role in treatment of raw water and wastewater, for
interpretation and control of water and wastewater systems.
It is a function of the presence of bicarbonates, carbonates and hydroxides in surface
water and is taken as an indicator of concentration of these components. The value of
alkalinity also may include borates, phosphates, silicates and other bases, if they are
present in water.

Suitability of any water for agricultural use or irrigation purposes can be determined if
alkalinity is in excess of the alkaline earth metals.

Alkalinity is important for fish and aquatic life because it provides buffering action and
protects them from sudden pH changes.

Alkalinity is a measure of how much acid can be added to a liquid without causing a large
change in pH. Higher alkalinity levels in surface waters can buffer acid rain and other
acid wastes and prevent pH changes that are harmful to aquatic life.

EXPERIMENT NO. 7
CHLORIDE
Date: 24.08.09

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Aim:
To measure the chloride content of an unknown water sample by argentometric method.

Principle:
In a solution of pH in the range of 7 to 10, i.e. in neutral or slightly alkaline range,
potassium chromate can indicate the end point of the titration of silver nitrate by sodium
chloride. Silver nitrate is precipitated quantitatively before reddish brown silver chromate is
formed.

Apparatus:
1. Volumetric flasks, 250 ml and 50 ml
2. Burette, 50 ml
3. Pipette, 5 ml and 10 ml
4. Erlenmeyer flasks, 250 ml

Reagents:
(a) Potassium Chromate indicator solution
(b) Standard silver nitrate (AgNO3 titrant (0.0141 N): 2.395 g of silver nitrate
(AgNO3) was weighed and dissolved in distilled water and volume is made up to
1000 ml. The solution was then standardized against 0.0141 N sodium chloride
(NaCl). Here, 1 ml = 500g Cl
(c) Standard sodium chloride (NaCl) solution (0.0141N): NaCl (dried at 140 C) was
taken and 824 mg is weighed and dissolved in distilled water. Then volume was
made up to 1000 ml in a volumetric flask.
(d) Sodium hydroxide (NaOH) solution (1N): 4gm of Sodium hydroxide (NaOH)
was taken and dissolved in distilled water and volume was made up to 50 ml in a
volumetric flask.
(e) Sulphuric acid (H2SO4) solution (1N): 2.7 ml of Sulphuric acid was taken and the
volume was made upto 100 ml in a volumetric flask with distilled water.
Procedure:

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1. The AgNO3 solution prepared was standardized by NaCl solution. 10 ml of NaCl solution
was taken in conical flask and was titrated. Potassium chromate indicator was used
during the titration and volume of AgNO 3 solution consumed was noted down.
Normality of AgNO3 solution was calculated.

2. The unknown sample was taken and diluted to 100 ml with distilled water. pH of the
diluted sample was measured to be 5.67. Thus, a pH correction was made using 1N
NaOH and final pH was 9.62.

3. AgNO3 solution was again taken in a 50 ml burette.

4. 10 ml of distilled water was taken in a conical flask as blank solution. 1-2 drops of
potassium chromate indicator was added and colour changed to light yellow. It was
titrated against the silver nitrate solution till colour changed to reddish brown. The
volume of AgNO3 solution consumed was noted.

5. 10 ml of the unknown diluted sample was taken in a conical flask and 1-2 drops of
potassium chromate indicator was added. The colour changed to light yellow. The
sample was titrated against silver nitrate solution till colour changed to reddish brown.
The volume of AgNO3 solution consumed was noted.

Sample reading:

Standardization of AgNO3 solution:

Sl Initial Final Volume of AgNO3

No. burette burette consumed in ml
reading reading

1 0 11 11

2 13 24 11

Titration of Blank and unknown sample:

Sl Titration for Initial burette Final burette Volume of AgNO3

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No reading reading consumed in ml

1 Blank 0 0.2 0.2

2 2.2 0.2

2 Unknown sample 0 1.9 1.9

1.9 3.8 1.9

Calculation/ Result:

(0.0141 10)
Normality of AgNO3 solution, N = = 0.0128 N
11

((A B) N 35450)
Chloride in unknown sample = ml of sample

((1.9 0.2) 0.0128 35450)

=
10

= 77.13 mg/L

mg NaCl/L = mg Cl/L x 1.65

= 77.13 x 1.65 = 127.2 mg/L

Environmental significance:

Chloride in natural water is resulted from leaching of chloride bearing rocks and soils
with which water comes in contact.
In coastal areas, there is intrusion of saltwater resulting in higher chloride content of
water. In addition to these, agricultural, domestic and industrial sources also contribute to
increase in chloride content of water bodies.

It gives a salty taste to the water and also increases the conductivity.

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EXPERIMENT NO. 8
HARDNESS
Date: 29.09.09
Aim:
To measure the hardness of an unknown sample solution by EDTA titrimetric method.

Principle:

When ethylene-diamine-tetraacetic acid and its sodium salts (EDTA) is added to solution
containing metallic cations it forms a chelated soluble complex. Upon addition of a dye such as
erichrome black-T to a solution containing calcium and magnesium ions, it becomes wine red
and when the solution is titrated with EDTA the calcium and magnesium ions are complexed and
at the end point of the titration the colour becomes blue indicating that all the calcium and
magnesium ions have been complexed.

Apparatus:
(b) Volumetric flasks, 50 ml, 100 ml & 250 ml
(c) Conical flasks, 250 ml
(d) Burette, 50ml
(e) Pipettes, 1 ml, 5 ml and 10 ml
(f) Hot plate

Reagents:
(a) Ammonium buffer solution:
A solution of 1.179 g of disodium salt of ETDA and 780 mg of hydrated magnesium
sulphate (MgSO4.7H2O) was prepared by mixing with 5 ml of distilled water. Another
solution of 16.9 g of ammonium chloride (NH 4Cl) mixed with 143 ml of ammonium
hydroxide (NH4OH) was also prepared. Both the solutions were mixed and volume was
made up to 250 ml to prepare the ammonium buffer solution.
(b) Standard EDTA titrant of 0.01 M:

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This was prepared by mixing 3.723 g of di-sodium salt of EDTA with distilled
water. Volume of the solution was made up to 1000 ml.
(c) Standard calcium solution:
1 g of anhydrous calcium carbonate (CaCO 3) powder was taken in a conical flask
and conc. hydrochloric acid (HCl) solution (1 volume to one volume of distilled
water) was added drop by drop till all the calcium carbonate was dissolved. 200 ml of
distilled water was added and the solution was then boiled to allow CO 2 to escape out.
Then it was cooled in air and 2 drops of methyl red indicator was added. The volume
of the solution was then made up to 100 ml. That was the standard calcium solution
having a strength of 1 ml = 1.00 mg Ca CO3.

Procedure:

1) The standard calcium solution was standardized by taking 10 ml of the solution in a

conical flask and titrating the same against standard EDTA titrant. The indicator
used was erichrome black-T. Volume of EDTA consumed was noted down.
2) An unknown sample solution was taken, out of which 25 ml was taken in a conical
flask. 1 ml of ammonium buffer solution and 2 drops of erichrome black-T indicator
was added to it. Then it was titrated against the standard EDTA titrant till the colour
changed from light red to blue and volume of EDTA consumed was noted down.

Sample reading and calculations:

Volume of EDTA titrant consumed during standardization of standard calcium solution = 9.8 ml

10
Equivalent CaCO3 = = 1.02 = B
9 .8

Volume of EDTA titrant consumed during titration = 3 ml = A

A B 1000 3 1.02 1000

Hardness = ml of sample =
25

= 122.4 mg/l

Result: The hardness of the unknown water sample was measured to be 122.4 mg/l

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Environmental significance:

Hardness in water or hard water requires higher amount of soap to produce foam
and is of common mans interest from economic point of view.
Hardness in water leads to scaling in water pipes, boilers, heaters and other
industrial applications and thus is of importance from the point of view of both
economics and productivity. Such hard water is required to be softened before use
and account for a lot of money in industries.

Generally, ground water has more hardness than surface water.

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EXPERIMENT NO. 9
RESIDUAL CHLORINE
Date: 29.09.09
Aim:
To measure the residual chlorine content of an unknown sample solution by DPD ferrous
titrimetic method.

Principle:
During the titration of the chloride bearing sample with ferrous ammonium suphate
(FAS), N, N-diethyl-p-phenylene-diamine (DPD) is used as an indicator. In absence of iodine
ions, free chlorine reacts with the DPD indicator to produce a red colour. When it is titrated
against FAS, there is a sharp colourless end point. In presence of iodine ions, nitrogen trichloride
(NCl3) is included with the free chlorine and the total is reported as the total residual chlorine.

Apparatus:
(a) Burette
(b) Volumetric flasks, 100 ml, 500 ml & 1000 ml
(c) Beakers, 100ml
(d) Pipettes, 5 ml and 10 ml
(e) Glass rod

Reagents and chemicals:

(a) Phosphate buffer solution:
A solution of 6 gm Na2HPO4 and 11.5 gm KH2PO4 was made with distilled water.
Another solution of 200 mg of EDTA salt and distilled water was prepared. Both the
solution was mixed together and volume was made up to 250 ml.
(b) N, N-diethyl-p-phenylene-diamine (DPD) solution:
(c) Standard ferrous ammonium suphate (FAS) solution:
1 ml of the above mentioned acid solution (1 volume of conc. H 2SO4 and 3
volumes of distilled water) was taken and mixed with distilled water. 1.106 gm of ferrous
ammonium suphate salt was dissolved in it and then volume was made up to 1000 ml.
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(d) Potassium iodide (KI) salt:
(e) Sodium Hypochlorite Solution

Procedure:

1) Some amount of the unknown sample solution was taken in different 25 ml

volumetric flasks. Increasing amounts of sodium hypochlorite was added to
successive portions in the series. The volumetric flasks were made up to the mark
with the unknown sample.

2) Sample from each volumetric flask was titrated against the prepared FAS solution.
Before titration, 2.5 ml of DPD solution, 2.5 ml of Phosphate Buffer Solution and
0.25 g of KI salt was added in the sample solution. The end point of the titration was
from red to colorless.

3) After the titration, different volumes of FAS required for the titration of different
concentration of chlorine dosage was recorded and the graph was plotted of the
chlorine dosage against residual chlorine.

Readings:

Sl Volume of Chlorine Volume Sl Volume of Chlorine Volume of

No the sample doses in of FAS No the sample doses in FAS
in ml mg/l consume in ml mg/l consumed
d
100
1 100 0.3 0.1 11 1.3 0.7
100 100
2 0.4 0.3 12 1.4 0.8
100 100
3 0.5 0.4 13 2 1.2
100 100
4 0.6 0.5 14 2.1 1.5
100 100
5 0.7 1 15 2.2 1.7
100 100
6 0.8 1.2 16 2.7 1.7

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100 100
7 0.9 1.4 17 2.8 1.8
100 100
8 1 2.2 18 2.9 1.9
100
9 1.1 0.5
100
10 1.2 0.6

Graph of Chlorine doses vs. Residual chlorine:

Break point

A B

Result:

As observed from the graph, the break point of chlorination is at chlorine dose of 1.1
mg/l. The left side of the break point (marked as A) refers to predominance of combined
chlorine residuals and the right side (marked as B) refers to predominance of free residual
chlorine.

Environmental significance:

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Disinfection is a process of killing harmful pathogenic bacteria and other organisms
during the process of water treatment. Such disinfection is usually done by chlorine
or sodium hypochlorite and in the process some quantity of the disinfectant remains
in dissolved condition and that is referred as residual chlorine.
Chlorine, hypochlorite and hypochlorous acids consist of the free chlorine residual
chlorine. Chlorine reacted with ammonia form chloramines and combining
chloramines with residual chlorine is referred as total available chlorine. During
disinfection of water both residual and total chlorine are measured and presence of
some amount of residual chlorine indicates effective disinfection. The byproducts
formed during chlorination such as trihalomethanes are carcinogenic by nature.
EXPERIMENT NO. 10
AMMONIA-NITROGEN
Date:31.08.09
Aim:
To measure the ammonia-nitrogen content of an unknown sample solution by
Nesselerisation method.

Principle:
When Nesslers reagent react with ammonia present in water, the colour of the solution
changes from yellow to brown and it strongly absorb light over a wide wavelength range. The
intensity of the colour is measured by spectrophotometer at 420 nm wave length. The intensity of
light absorbed is plotted against the known concentrations of the solution to obtain a calibration
curve. The concentration of ammonia-nitrogen of the unknown sample solution is estimated by
comparing its corresponding intensity with the calibration curve. Nesselerisation method is
applied only for purified drinking waters, natural water and highly purified waste water effluents.

Apparatus:
(a) Spectrophotometer
(b) Volumetric flasks, 100 ml & 250 ml
(c) Beakers, 100 ml
(d) Pipettes, 5 ml and 10 ml

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Reagents:
(a) Stock ammonium solution: 0.3819 g of anhydrous ammonium chloride (NH 4Cl) was
dissolved in distilled water and volume was made up to 100 ml. This was the stock
ammonia solution having strength of 1 ml = 1 mg Nitrogen = 1.22 mg NH3.
(b) Standard ammonium solution: 10 ml of the stock ammonium solution was taken and was
diluted to 1000 ml to get strength of 1 ml = 10 g Nitrogen =12.2 g NH3. From this
solution, 5 ml, 10 ml, 15 ml, 20 ml, 25 ml, 30 ml, 35 ml, 40 ml, 45 ml and 50 ml was
taken and each was diluted to 100 ml to obtain standard ammonium solutions of 0.5, 1,
1.5, 2, 2.5, 3, 3.5, 4, 4.5 and 5 mg/l Nitrogen concentration respectively.
(c) Nesslers reagent: 10 g of HgI2 and 7.0 g of KI were mixed in 50 ml distilled water with
stirring to prepare a mixture. Then 16 g of NaOH was added slowly with stirring and the
final volume was made upto 100 ml with distilled water. A clear yellow colour solution
was obtained.
Procedure:

(a) The unknown sample solution provided was diluted to 50 ml and was transferred into a
beaker. 2 ml of the prepared Nesslers reagent was added to it. A brown colour was
developed.
(b) The procedure was followed for all the standard solutions and the blank and colour was
found to be developed in all except the blank.
(c) The absorbance readings of all the coloured solutions were taken at 420 nm in the
spectrophotometer. Then a calibration curve was drawn by taking the concentration in X-
axis and absorbance readings in Y- axis.

Spectrophotometer readings:

Sl. No. Concentration of the standard Intensity reading

ammonium solution in mg/l recorded.

1 Blank 0

2 0.5 0.075

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3 1.0 0.186

4 1.5 0.238

5 2.0 0.322

6 2.5 0.416

7 3.0 0.460

8 3.5 0.553

9 4.0 0.640

10 4.5 0.733

11 5.0 0.796

12 Unknown sample 0.337

Calibration Curve:

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Calculation:

The above calibration curve for absorbance versus concentration satisfies to the equation

y = 0.160 x, where

y = Absorbance reading of spectrophotometer

x = Concentration in mg/l

0.337 = 0.160 x
0.337
x= = 2.106 mg/l N2, i.e. 2.106 x 17/14 = 2.557 mg/l NH3
0.160

Result: The nitrate-nitrogen content of the unknown sample solution was found out to be 2.106
mg/liter Nitrogen or 2.557 mg/liter ammonia.

Environmental significance:

When nitrogenous organic matter is destroyed by microbiological activity, ammonia is

produced and is therefore found in many surface and ground waters.
Higher concentrations occur in water polluted by sewage, fertilizers, agricultural wastes or
industrial wastes containing organic nitrogen, free ammonia or ammonium salts.
Certain aerobic bacteria convert ammonia into nitrites and then into nitrates. Nitrogen
compounds, as nutrients for aquatic micro-organisms, may be partially responsible for the
eutrophication of lakes and rivers. Ammonia can result from natural reduction processes
under anaerobic conditions.
Nitrogen is responsible for various adverse effects such as photochemical smog, global
warming, ozone depletion.
The amount of nitrogen in water determines the extent upto which chloride is needed to
obtain free residual chlorine.
Excess nitrogen in the treated effluents leads to eutrophication.
Information about nitrogen is required for biological processes.

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EXPERIMENT NO. 11
NITRATE-NITROGEN

Date:29.09.09

Aim:
To measure the nitrate-nitrogen content of an unknown sample solution by colorimetric
method.

Principle:
When brucine reacts with nitrate, the solution yields a sulphur yellow colour. The
intensity colour is measured by spectrophotometer at 410 nm wave length as light absorbance
and intensity of light absorbed is plotted against the known concentrations to arrive at a
calibration curve. The concentration of nitrate-nitrogen of unknown sample is estimated by
comparing its corresponding intensity with the calibration curve.

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Apparatus:
(a) Spectrophotometer
(b) Volumetric flasks, 100 ml & 500 ml
(c) Beakers, 100ml
(d) Pipettes, 5 ml and 10 ml

Reagents:
(a) Stock nitrate solution: 0.0722 gm of potassium nitrate (KNO 3) was dissolved in distilled
water and volume was made up to 100 ml. This was the stock nitrate solution having
strength of 1 ml = 100 g N.
(b) Standard nitrate solution: 50 ml of the stock nitrate solution was taken and was diluted to
500 ml to get strength of 1 ml = 10 g N. From this solution, 5ml, 10 ml, 20 ml, 40 ml,
60 ml, 80 ml and 100 ml was taken and each was diluted to 100 ml to obtain standard
nitrate solutions of 2, 4, 6, 8 and 10 mg/L nitrate concentration respectively.
(c) Brucine-sulfanic acid solution: 0.5 gm of brucine sulphate and 0.05 gm of sulfanic acid
were mixed with 35 ml of hot distilled water and the solution was diluted to 50 ml.
(d) Sulphuric acid solution: 100 ml of conc. Sulphuric acid (H2SO4) was mixed with 15 ml of
distilled water.

Procedure:

(a) The unknown sample solution supplied was diluted to 100 ml.
(b) 2 ml from solution from the unknown sample, blank and standard solutions were taken in
beakers.
(c) And 1 ml of sulfanilic acid solution was added to each of the beakers.
(d) 10 ml of H2SO4 solution was taken in another beaker and it was mixed slowly with the
sulfanilic acid solution of unknown sample by transferring from one to another. This
process of adding sulphuric acid was repeated for all the standard solutions and the blank.
A deep brown colour was developed in all the solutions.
(e) All the coloured solutions were taken to the spectrophotometer for measuring the
absorbance readings at 410 nm, which were noted down. Then a calibration curve was
drawn by taking the concentration in X- axis and absorbance readings in Y- axis.
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Spectrophotometer readings:

Sl. No. Concentration of the standard Intensity reading

nitrate solution in mg/l recorded.

1 Blank 0.0

2 2 0.308

3 4 0.602

4 6 1.143

5 8 1.414

6 10 1.281

7 sample 0.197

Calibration Curve:

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Concentration(mg/L)

Calculation:

The above calibration curve for absorbance versus concentration satisfies to the equation

y = 0.173 x, where

y = Absorbance reading of spectrophotometer

x = Concentration in mg/L

0.197 = 0.173 x
0.197
x= = 1.138 mg/L
0.173

Result: The nitrate-nitrogen content of the unknown sample was measured to be 1.138 mg/L.

Environmental significance:

Nitrate, the most highly oxidized form of nitrogen compounds, is commonly present
in surface and ground waters, because it is the end product of the aerobic
decomposition of organic nitrogenous matter.
Significant sources of nitrate are chemical fertilizers from cultivated land and
drainage from livestock feedlots, as well as domestic and some industrial waters.

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The determination of nitrate helps in the assessment of the character and degree of
oxidation in surface waters, in groundwater penetrating through soil layers, in
biological processes and in the advanced treatment of wastewater.
Unpolluted natural waters usually contain only minute amounts of nitrate. In surface
water, nitrate is a nutrient taken up by plants and assimilated into cell proteins.

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EXPERIMENT NO. 12
FLUORIDE

Date:01.09.09
Aim:
Measurement of the fluoride content of an unknown sample solution by SPADNS method.

Principle:
The colorimetric method of determination of fluoride in water is based on the reaction
between fluoride and zirconium ions. Fluoride reacts with the dye and dissociates it into a
colourless complex and the dye. As the concentration of fluoride increases in water, the colour of
the dye becomes lighter. The rate of reaction between fluoride and zirconium ions is influenced
by the acidity of the solution. A solution of zirconylacidreagentandSPADNSsolutionasdye
areusedforthepurpose.SPADNSreducestheinterferenceduetootherions.Thedeveloped
colour is measured by measuring the absorbance at 570 nm in a spectrophotometer and a
calibrationcurveispreparedforestimatingtheunknownfluorideconcentration.

Apparatus:
(a) Spectrophotometer
(b) Volumetric flasks (500 ml, 100 ml and 50 ml)
(c) Conical flasks
(d) Pipettes
(e) Beakers
(f) Glass rod

Reagents:

(a) Stock fluoride solution: 221 mg of anhydrous sodium fluoride (NaF) was dissolved in
distilled water and volume of the solution was made up to 1000 ml. The strength of this
stock solution was of 1 ml = 100 g F-.
(b) Standard sodium solution: 10 ml of the prepared stock solution was taken and diluted up
to 1000 ml to get a strength of 1 ml = 10 g F-.
(c) SPADNS Solution: 958 mg of SPADNS, (sodium 2- (parasulfophenylazo) - 1, 8 dihydroxy-3, 6-
naphthalene disulfonate) was dissolved in distilled water and volume was made up to 500 ml.

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(d) Zirconyl acid reagent: 133 mg of zirconyl chloride octahydrate (ZrOCl2.8H2O) was
dissolved in 25 ml distilled water. 350 ml of conc. HCl was added to the above solution
and then volume of the resultant solution was made up to 500 ml.
(e) Acid Zirconyl SPADNS reagent: Equal volumes each of 60 ml SPADNS solution and 60
ml Zirconyl-acid reagent was mixed to obtain the reagent.
(f) Reference solution: 10 ml of prepared SPADNS solution was mixed with 100 ml distilled
water. A second solution was prepared by mixing 7 ml of HCl to 10 ml of distilled water.
Both the solutions were mixed to prepare the reference solution.

Procedure:

(a) Fromthestandardfluoridesolutionprepared,5ml,10ml,15ml,20mland25mlwere
takeninto50mlflasksandvolumesweremadeuptothemark.This wastoobtain
standardsolutionshavingfluorideconcentrationas1,2,3,4and5mg/lrespectively.
(b) 10mlofAcidZirconylSPADNSreagentsolutionwasaddedtoeachofthestandard
solutionsamples.
(c) The reference solution was taken for reading the absorbance reading in
spectrophotometerat570nmandthenthespectrophotometerwassetatzero.
(d) Absorbancereadingsforallthestandardsolutionsweretakenbyspectrophotometerat
570nm.
(e) Absorbance reading of the blank (distilled water) and unknown sample solution was
takenbyadditionof10mlofAcidZirconylSPADNSreagentsameasabove.
(f) ThecalibrationcurvewaspreparedbytakingtheknownconcentrationsinXaxisand
absorbancevaluesinYaxis.
(g) Concentrationoffluorideoftheunknownwatersamplewascalculatedfromthestandard
calibrationcurve.
Spectrophotometer readings:

Sl. No. Strength of the standard F solution Absorbance recorded.

in mg/l

1 Reference 0

2 1 0.243
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3 2 0.183

4 3 0.083

5 4 0.075

6 5 0.033

7 Unknown sample -0.051

8 Distilled water 0.146

Calibration Curve:

Results and Calculation:

The above calibration curve for absorbance versus concentration satisfies to the equation
y = -0.052x + 0.281
y = Spectrophotometer reading = -0.051(unknown sample solution)
x = Concentration in mg/l
or, -0.051 = -0.052x + 0.281

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or, x = 6.38 mg/l
For distilled water, absorbance reading was 0.146 and concentration of fluoride as
determined from the above equation was found out to be 2.59 mg/l.

Result:
Flouride content of the unknown sample solution was found to be 6.38 mg/l.

Environmental significance:
Inmanycountries,fluorideispurposefullyaddedtothewatersupply,toothpasteand
sometimesotherproductstopromotedentalhealth.
Fluoride is also found in the atmosphere (mostly from production of phosphatic
fertilizersandaluminiumsmelters),sotheamountoffluoridepeopleactuallyingest
maybehigherthanassumedasrequirement.
InmanypartsoftheworldandinIndia,ahighconcentrationoffluorideoccurring
naturally in groundwater has caused a widespread bone disease called fluorosis
amonglocalpopulations.
The extent of the damage varies from place to place depending on the level of
fluorideindrinkingwater,durationofintakesandtheabsorbingrateofhumanbody
visvisfoodhabits.Severe,chronicandcumulativeoverexposurehaspotentialto
causetheincurablecripplingofskeletalfluorosis.
Thepermissibleupperlimitforfluorideindrinkingwaterwasconsideredtobe1.5
mg/lbyWHO.However,Indiahaslowereditspermissibleupperlimitfrom1.5to1.0
mg/lin1998.

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EXPERIMENT NO. 13
BOD
Date:08.09.09
Aim:
To measure the biochemical oxygen demand (BOD) of a supplied water sample.

Principle:
Measurement of BOD of wastewaters, effluents and polluted waters is the measurement
of oxygen required for biochemical degradation of organic matter as well as the oxygen required
for oxidation of inorganic materials such as sulfides and ferrous iron present in such water. The
method involves measurement of dissolved oxygen levels of the water sample before and after
incubation under specified conditions and BOD is calculated from the difference between initial
and final DO.

Apparatus:
(a) Burette
(b) Volumetric flasks, 100 ml, 500 ml & 1000 ml
(c) Beakers, 100 ml
(d) Pipettes, 1 ml, 5 ml and 10 ml
(e) Glass rod
(f) BOD bottles (Incubation bottles)

(g) BOD incubator

Reagents and chemicals:

(a) Sodium thiosulphate solution (0.025 M): 1.551 g of Na2S2O3.5H2O was dissolved in
distilled water and then 0.1 gm of NaOH solid salt was added to it and dissolved. The
volume of the solution was made up to 250 ml.

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(b) Manganous sulphate solution: 36.4 g of MnSO 4.H2O was dissolved with distilled water
and volume was made up to 100 ml. The insolubles were allowed to settle down and the
supernatant solution was used.
(c) Alkali iodide azide reagent: A solution of 50 gm of NaOH and 15 gm of KI were
dissolved in dissolved in distilled water and volume was made up to 100 ml. A second
solution was prepared by dissolving 1 gm of NaN 3 in 4 ml of water and then both the
solutions were mixed together.
(d) Starch solution: 1 gm of laboratory grade soluble starch powder was dissolved in hot
distilled water and then volume was made up to 50 ml.
(e) Dilution water:

Procedure:

Dilution of the sample:

(a) Two incubation bottles were taken and their volume was measured.
(b) 10 ml of an unknown water sample was provided in each of the two incubation bottles
and then diluted and filled completely with the prepared dilution water.
(c) The glass stopper was closed ensuring that no air bubble was left inside. One bottle was
taken for dissolved oxygen (DO) measurement.
Incubation: The second bottle was kept inside the BOD incubator for five days at 20 C.

DO measurement:
(a) The stopper of the first incubation bottle was opened and 1 ml each of manganous
suphate solution and alkali iodide azide reagent was added. Then stopper was closed
ensuring that no air bubble was left inside and then mixing was done by inverting the
bottle for a few number of times.
(b) The precipitates formed were allowed to settle down and after about 50 % settling, the
stopper was again opened and 1 ml conc. H2SO4 was added to it. The stopper was closed
and the solution was mixed till all the precipitates were dissolved and colour became
yellowish brown.
(c) Volume of the solution to be titrated was calculated as 201 ml (corresponding to 200 ml
of original sample) and was taken in a conical flask. 0.025 M sodium thiosulphate
solution was taken in the burette and titration was carried out till the yellowish brown

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colour changed to pale yellow. Then two drops of starch solution was added as indicator
and colour of the solution changed to blue. Titration was continued till the blue colour
changed to colourless. The initial and final readings of burette corresponding to the
sodium thiosulphate consumption were noted down.
(d) The initial DO was calculated as 1 ml sodium thiosulphate (0.025 M) = 1 mg/l of DO.

(e) After incubation for five days at 20 C the second sample was taken out. The procedure
of DO measurement was repeated and final DO was calculated.

Readings and calculations:

Initial DO:

Volume of the incubation bottle used for initial DO measurement = 300 ml.
300
Volume of solution taken for titration corresponding to 200 ml of sample =
298
200 201
ml, where

342 = Volume of the incubation bottle in ml

340 = Volume of the diluted sample = 342 ml- (1 ml MnSO4 + 1 ml alkali iodide azide)

Final DO:

Volume of the incubation bottle used for incubation and final DO measurement = 300 ml
300
Volume of solution taken for titration corresponding to 200 ml of sample =
298
200 201
ml, where,

300 = Volume of the incubation bottle in ml

298 = Volume of the diluted sample = 300 ml- (1 ml MnSO4 + 1 ml alkali iodide azide)

Sl Sample Initial Final Volume of Measured

No burette burette sodium DO in mg/l
reading reading thiosulphate
consumed in ml

1 Initial DO of seed 0 6.7 6.7 6.7

2 Final DO of seed 0 5.5 5.5 5.5

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Sl Sample Initial Final Volume of Measured

No burette burette sodium DO in mg/l
reading reading thiosulphate
consumed in ml

1 Initial DO of sample 6.7 13.5 6.8 6.8

2 Final DO of sample 14.9 18.5 3.6 3.6

Then BOD is calculated as

(D1 D 2 )
BOD = ,
P

Where, D1 = Initial DO of sample

D2 = Final DO of sample

P = Volumetric fraction of sample used in titration

6 .8 3 .6
Then, BOD = = 96 mg/l,
10 / 300

When dilution water is seeded,

BOD, mg/L = (D1- D2) (B1- B2) f / P

Where,

D1 = DO of diluted sample immediately after preparation

D2 = DO of diluted sample after 5 days incubation at 20C mg/L

P = decimal volumetric fraction of sample used= 10/300 = 0.03

B1 = DO of seed control before incubation mg/L

B2 = DO of seed control after incubation mg/L

f = ratio of seed in sample to seed in control = (300 - 10) /300 = 0.96

Hence, BOD = ((6.8 3.6) (6.7 5.5) 0.96) / 0.03 = 68.3 mg/L

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Thus, BOD of the supplied water sample was found out to be 68.3 mg/L.

Environmental significance:

Dissolved oxygen content of water bodies is an important parameter for aquatic

ecosystem. When the organic matter concentration in such water bodies increase due to
anthropogenic activities, dissolved oxygen level comes down as the microorganisms
present in water decomposes the organic matter utilizing DO.
BOD is the demand of oxygen required for such decomposition and is an indicator of the
level of organic matter present in water bodies.

It is the single most important parameter based on which effluent treatment plants and
sewage treatment plants have been designed.

The basic objective of these treatment plants is to reduce the BOD level in the discharges
to water bodies so that the load of organic matter into the recipient water bodies reduces
and the DO level of water is maintained.

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EXPERIMENT NO. 14
SULPHATE
Date:08.09.09
Aim:
To measure the sulphate content of an unknown sample solution by Turbidimetric
method.

Principle:
Sulphate ions present in water reacts with BaCl 2 to form BaSO4 in a medium of
hydrochloric acid. Formation of BaCl2 crystals makes the water turbid. The light absorbance of
the suspension is measured by nephelometer which is plotted against the known concentrations
of the solution to obtain the calibration curve. The concentration of the suphate of unknown
sample solution is estimated by comparing its corresponding turbidity with the calibration curve.

Apparatus:
(a) Nephelometer
(b) Volumetric flasks, 100 ml & 250 ml
(c) Beakers, 100 ml
(d) Pipettes, 5 ml and 10 ml
(e) Glass rod

Reagents and chemicals:

(a) Standard sulphate solution: 147.9 mg of anhydrous Na2SO4 was dissolved in distilled
water and volume was made up to 500 ml. This was the stock sulphate solution having
strength of 1 ml = 100 g sulphate.

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From the standard solution, 10 ml, 20 ml, 30 ml and 40 ml was taken and each
was diluted to 100 ml to obtain known solutions having 10, 20, 30 and 40 mg/l sulphate
respectively.
(b) Conditioning reagent: 6 ml of conc. hydrochloric acid (HCl) was mixed with a solution
containing 60 ml of distilled water. Then 20 ml of ethyl alcohol and 15 gm of NaCl was
added to the solution and dissolved thoroughly. Finally 10 ml of glycerol was then mixed
with the prepared solution.
(c) Barium Chloride (BaCl2) crystals: one spoonful.
Procedure:

(a) The unknown sample solution supplied was diluted to 100 ml in a volumetric flask. Then
5 ml of the conditioning agent was added and the solution was mixed properly. One
spoonful of BaCl2 crystals were then added and stirred for exactly one minute. Then
turbidity of the solution was measured by nephelometer.
(b) The procedure was followed for all the standard solutions of known concentrations and
the blank solution.
(c) A calibration curve was drawn by taking the concentration in X- axis and turbidity
readings in Y- axis.

Nephelometer readings:

Sl. No. Concentration of the standard Intensity reading

suphate solution in mg/l suphate recorded.

1 Blank 0

2 10 44

3 20 79

4 30 124

5 40 138

7 Unknown sample 103

Calibration Curve:
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Calculation:

The above calibration curve for turbidity versus concentration satisfies to the equation

y = 3.753 x, where

y = Turbidity in NTU

x = Concentration in mg/L

103 = 3.753 x
103
x= = 27.4 mg/L sulphate,
3.753

Result: The sulphate content of the unknown water sample was measured to be 27.4 mg/L
sulphate.

Environmental significance:

Sulphate is an abundant ion in the earths crust and its concentration in water can range
from a few milligrams to several thousand milligrams per litre.
Industrial wastes and mine drainages may contain high concentrations of sulphate.
Sulphate also results from the breakdown of sulphur-containing organic compounds.

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It is one of the least toxic anions and WHO does not recommend any guideline value for
it in drinking water. However, catharsis, dehydration and gastrointestinal irritation have
been observed at high concentrations in drinking water and WHO therefore suggests that
health authorities should be notified when concentrations of sulphate in drinking water
exceed 500 mg/l.

Experiment No. 15
COD
Date: 08.09.09
Aim: To measure the Chemical Oxygen Demand (COD) of a water sample.

Principle:
Most of the organic matter present in water gets oxidized when boiled with a mixture of
chromic and sulfuric acids. A water sample is digested in strong acidic solution having
excess of potassium dichromate (K2Cr2O7) and after digestion, the residual unreduced
potassium dichromate (K2Cr2O7) is titrated against ferrous ammonium solution (FAS) to
determine the amount of K2Cr2O7 consumed by the organic matter during digestion. The
oxidizable organic matter is calculated and expressed in terms of oxygen equivalent.

Apparatus:
(a) Digestion tubes
(b) Heating Block
(c) Burette
(d) Volumetric flasks, 100 ml
(e) Beakers

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(f) Pipettes
(g) Glass rod

Reagents :
(a) Standard potassium dichromate solution: 0.4903g of K2Cr2O7 (previously dried at 103C)
was mixed with 16.7 ml conc. H 2SO4 and 3.33g HgSO4, finally diluted to 100ml. It was
allowed to dissolve and cool down to room temperature.
(b) Sulfuric acid reagent
(c) Conc. sulfuric acid
(d) Ferroin indicator: 1.485 gm of 1, 10 phenanthroline monohydrate and 695 mg of FeSO 4.7
H2O was weighed and added in distilled water and volume was made up to 100 ml.
(e) Standardferrousammoniumsulfate(FAS),0.1M:3.92gmofferrousammoniumsulfate
(Fe(NH4)2(SO4)2.6H2O)wasdissolvedindistilledwaterand2mlofconc.H 2SO4 was
addedtoit.Theresultantsolutionwascooledandvolumewasmadeupto100ml.
Procedure:

Standardization of FAS:

(a) FAS was taken in a burette and initial reading was taken.
(b) 10 ml of potassium dichromate solution was taken in a conical flask, 2 drops of ferroin
indicator was then added. It was titrated against FAS and the volume of FAS consumed
was noted down. Colour of solution changed slowly from deep yellow to wine red.

Sample preparation and digestion:

(a) The digestion tubes and their caps were rinsed with conc. sulphuric acid.
(b) 2.5 ml of unknown sample, 1.5 ml of potassium dichromate solution and 3.5 ml of
sulfuric acid reagent were taken in the digestion tube. The total sample volume became
7.5 ml. The same procedure was also followed for the blank sample. Caps of the
digestion tubes were tightened.
(c) The digestion tubes were transferred into the heating block and digestion was conducted
at 150 2C for 2 hrs.
(d) After digestion, the sample was cooled down and transferred into a conical flask (100 ml)
and titrated against FAS. During titration the sample was stirred continuously and it was

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continued till colour of changed from blue green to reddish brown. The volume of FAS
consumed was noted down.
(e) The titration procedure was also repeated for the blank sample.

Sample readings:

Standardization of FAS:

Sl Initial burette Final burette Volume of FAS

No reading reading consumed in ml

1 0 10 10

Titration of sample with FAS:

Sl Sample Initial burette Final burette Volume of FAS

No reading reading consumed in ml

1 Blank 0.9 2.3 1.4

2 Unknown sample 0 0.9 0.9

Calculations:

Volumeof digestion solution used

Molarity of FAS= 0.1
Volume of FAS consumed

10ml
= 0.1 = 0.1 M
10ml

Then COD is calculated as

(A B) M 8000
COD = ml of sample

Where, A = ml of FAS used for blank

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 Name:ArnabKrPahari
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B = ml of FAS used for sample

M = Molarity of FAS

(1.4 0.9) 0.1 8000

Then COD = = 160 mg/l
2.5

Result: The COD of the unknown sample solution was found to be 160 mg/l.

Environmental significance:
Chemical oxygen demand of any water or wastewater system refers to the demand of oxygen
for oxidation of all the organic matter present in water.
It is based on the fact that all organic compounds with only a few exceptions can be oxidized by
the action of strong oxidizing agents under acidic conditions.
Values of COD are always larger than that of BOD in any water or wastewater systems as the
total organic matter regardless of its biological assimilability are oxidized.
The major advantage of the test is the short time required for evaluation. The determination of
COD can be made in about 3 hours rather than 5 days as required for measurement of BOD.
Variations in BOD to COD ratio of waste-water coming from an industry indicate about
variation in use of raw materials or intermediate processes. BOD to COD ratio less than 0.3
indicates presence of toxic materials in the wastewater.

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