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ECHELON INSTITUTE OF TECHNOLOGY

Faridabad

DEPARTMENT OF CIVIL ENGINEERING

Subject- Environmental Engineering Lab

S.no. Experiments Name


1 Flow Measurement in Closed Conduits- Venture-meter, Orifices.
2. Determination of Color and Turbidity
3 Determination of Solids: Total, Dissolved and Suspended; Dissolved Solids through
Conductivity.
4 Determination of Alkalinity and its Species.
5(a,b) Determination of pH and Acidity and Its Species
6 Determination of hardness
7 Determination of chloride
8 Determination of Fluorides
9 Jar test for Optimum Coagulant Does Estimation
10 Determination of residual chlorine and Chlorine does
Experiment No.1

Aim: To Measure the Flow in Closed Conduits- Venture-meter, Orifice-Meter.

Apparatus Required: Venture-meter, Orifice-Meter, Safety Utensils, Required Chemicals

Theory: Venture-meter and orifice meter are the commonly used flow meters for measuring
mass/volumetric flow rate or velocity of the flowing fluid. These flow meters are also known as
variable head meters. They are categorized as full-bore meter as measurement of the fluid takes place
when it flows through a conduit or channel.

Venture-meter: The venture-meter has a converging conical inlet, a cylindrical throat and a
diverging recovery cone. It has no projections into the fluid, no sharp corners and no sudden
changes in contour. The following figure shows the venture-meter with uniform cylindrical
section before converging entrance, a throat and divergent outlet.

The converging inlet section decreases the area of the fluid stream, causing the velocity to
increase and the pressure to decrease. The low pressure is measured in the center of the
cylindrical throat as the pressure will be at its lowest value, where neither the pressure nor
the velocity will be changing. As the fluid enters the diverging section the pressure is largely
recovered lowering the velocity of the fluid. The major disadvantages of this type of flow
detection are the high initial costs for installation and difficulty in installation and inspection.
The Venture effect is the reduction in fluid pressure that results when a fluid flows through a
constricted section of pipe. The fluid velocity must increase through the constriction to
satisfy the equation of continuity, while its pressure must decrease due to conservation of
energy: the gain in kinetic energy is balanced by a drop in pressure or a pressure gradient
force. An equation for the drop in pressure due to Venture effect may be derived from a
combination of Bernoulli’s principle and the equation of continuity.
The equation for venturi meter is obtained by applying Bernoulli equation and equation of
continuity assuming an incompressible flow of fluids through manometer tubes. If V1 and V2
are the average upstream and downstream velocities and ρ is the density of the fluid, then
using Bernoulli’s equation we get,

……………………… (1) where α1 and α2 are kinetic energy


correction factors at two pressure tap positions. Assuming density of fluid to be constant, the
equation of continuity can be written as:

……………………….. (2) where D1 and D2 are diameter of pipe


and throat in meters respectively.
Eliminating V1 from equation (1) and equation (2) we get,

…………………...... (3) where β is the ratio of the diameter of


throat to that of diameter of pipe.
If we assume a small friction lose between two pressure taps, the above equation (3) can be
corrected by introducing empirical factor Cv and written as,

…………………........ (4)

The small effect of the kinetic energy factors α1 and α2 are also taken into account in the
definition of Cv.
Volumetric flow rate Qa can be calculated as:

Qa = V2S2 = ……………………… (5) where, S2 is the cross sectional area


2
of throat in m .
Substituting (P1 – P2) = ρgH in above equation (5) we get,

Qa = V2S2 = …………………………. (6)

where ΔH is the manometric height difference * (specific gravity of manometric fluid –


specific gravity of manometric fluid of water).
Orifice meter:

Orifice-Meter: An orifice meter is essentially a cylindrical tube that contains a plate with a thin hole
in the middle of it. The thin hole essentially forces the fluid to flow faster through the hole in order to
maintain flow rate. The point of maximum convergence usually occurs slightly downstream from the
actual physical orifice this is the reason orifice meters are less accurate than venturi meters, as we
cannot use the exact location and diameter of the point of maximum convergence in calculations.
Beyond the vena contracta point, the fluid expands again and velocity decreases as pressure increases.
D
Variable distance

Figure 2. Orifice meter

The above figure 2 shows the orifice meter with the variable position of vena contracta with respect
to plate. Orifice meter uses the same principle of continuity equation and Bernoulli principle to
calculate the volumetric flow rate, as shown above for venturi meter.
So,

Qa = V2S2 = …………………………. (7) Here Co is the orifice discharge


coefficient.
Procedure:

Check all the clamps for tightness.


Check whether the water level in the tank is sufficient such that the suction pipe of pump is
completely immersed.
For measurement through venturi, open the outlet valve of the venturi meter and close the valve of
orifice meter.
For a good amount of variation in discharge also close the by-pass valve of pump.
Now switch on the pump.
Open the gate valve and start the flow.
If any air bubbles exist in U-tube manometer remove them through air cock valve. Operate the air
cock valve slowly and cautiously to avoid mercury run away through water.
Wait for a while for stabilization of flow.

Close the gate valve of measuring tank and measure the time for discharge of five liters of water and
the manometer difference. Before taking any measurements, make sure the flow is stable.
Repeat the procedure by changing the discharge by slowly opening the by-pass valve and take the six
readings.

Note: Repeat the same for orifice meter.


Given data:

For ventur- meter:

Cross sectional area of throat in venture-meter (S2) = 1.76*10-4 m2


Ratio of diameter of throat to pipe (β) = 0.4848

For orifice meter:

Cross sectional area of throat in venture-meter (S2) = 1.54*10-4 m2


Ratio of diameter of throat to pipe (β) = 0.4904

Observations and calculations:

Venture-meter

Reading no. h1 (cm) h2 (cm) time (seconds) Qm (m3/sec)

Orifice-meter

Reading no. h1 (cm) h2 (cm) time (seconds) Qm (m3/sec)

Result Obtained:
Experiment No. 2

Aim: Determination of Color and Turbidity

Apparatus Required: Nephelo-meters turbidity-meter, Sample tubes.

Reagents Preparation:
1. Dissolve 1.0gm Hydrazine sulphate and dilute to 100ml
2. Dissolve 10gm Hexa-methylene Tetra min& and dilute in l00ml
3. 5ml of each of the above solution (1 and 2) in a l00ml volumetric flask and allow
to stand for 24 hrs at 25±3°C and dilute to l000ml. This solution has a turbidity of
40NTU.

Procedure:
1. The Nephelometer turbidimeter in switched on and waited for few minutes till it
warms up.
2. The instrument is set up with a 4ONTU standard suspension
3. The sample is thoroughly shaked and kept it for sometimes so the air bubbles are
Eliminated.
4. The sample is taken in Nephelometer sample tube and the sample is put in Sample
chamber and the reading is noted directly.
5. The sample is diluted with turbidity free water and again the turbidity is read.

Environmental Significance
Turbidity is objectionable because of
a. Aesthetic considerations and
b. Engineering considerations
When turbid water in a small, transport container. such as drinking glass is help up
to the light, an aesthetically displeasing opaqueness or Ǯmilky coloration is apparent
The colloidal material which exerts turbidity provides adsorption sites for chemicals
that may be harmful or cause undesirable tastes and odours & for biological
organism that may be harmful. Disinfections of turbid water is difficult because of
the adsorptive characteristics of some colloids and because the solids may partially
shield organisms from disinfectant.
In natural water bodies, turbidity may impart a brown or other colour to water and
may interfere with light penetration and photosynthetic reaction in streams and
lakes.
Turbidity increases the load on slow sand filters. The filter may go out of operation,
if excess turbidity exists.

Application of Turbidity Data in Environmental Engineering Practice:


Turbidity measurements of particular importance in the field of water supply. They
have limited use in the field of domestic and Industrial waste treatment.
1. Knowledge of the turbidity variation in raw water supplies along with other
Information is useful to determine whether a supply repairs Special treatment by
Chemical coagulation and filtration before it may be used for a public water supply.
2. Turbidity measurements are used to determine the effectiveness of the treatment
Produced with different chemicals and the dosages needed.

3. Turbidity measurements help to gauge the amount of chemicals needed from day-today
in the operation of water treatment works.
4. Measurement of turbidity is settled water prior to filtration is useful in controlling
Chemical dosages so as to parent excessive loading or rapid sand filters.
5. Turbidity measurements of the filtered water are needed to check o faculty filter
Operation.
6. Turbidity measurements are useful to determine the optimum dosage of
Coagulants to treat the domestic and Industrial waste.
7. Turbidity determination is used to evaluate the performance of waste treatment Plant

Observation Table:

% of chlorine
Reading (ml)
in powder
Vol Na2S2O3
S.No. sample =
Initial Final consumed X (ml)
X*0.71
M

Calculation:
Chlorine in mg/L in chlorine solution = ml of Na2S2O3 consumed i.e
X*35.5*1000*.0.025
Ml of chlorine solution

% age chlorine in sample = mg/1 of chlorine


Mg/1 of powderX10
= X 35.5×100
= X*0.71
gm of sample used

Result:
The turbidity of Tap water =
Synthetic sample =
Experiment No. 3

Aim: Determination of Solids: Total, Dissolved and Suspended; Dissolved Solids through Conductivity.

Apparatus Required: Porcelain evaporating dishes of 150–200 mL capacity, Steam bath, Drying
oven, Desiccators, Analytical balance or monopan balance, Filter paper (preferably of glass
fibre), Electric muffle furnace, Imhoff cone

Principle: ‘Total solids’ is the term applied to the material left in the vessel after evaporation of a sample
of water/waste water and its subsequent drying in an oven at a definite temperature. Total solids include
“total suspended solids” the portion of total solids retained by a filter and “total dissolved solids” the
portion that passes through the filter. Fixed solids is the residue remaining after ignition for 1 hour at
550°C. The solid portion that is volatilised during ignition is called volatile solids. It will be mostly organic
matter. Waters that are low in organic matter and total mineral content and are intended for human
consumption may be examined under 103–105°C or 179–181°C. But water containing considerable organic
matter or those with pH over 9.0 should be dried at 179–181°C. In any case, the report should indicate the
drying temperature. The sample is filtered and the filtrate evaporate in a weighed dish on a steam bath, the
residue left after evaporation is dried to constant weight in an oven at either 103–105°C or 179–181°C. The
increase in weight over that of the empty dish represents total dissolved solids and includes all materials,
liquid or solid, in solution or otherwise, which passes through the filter and not volatilised during the
drying process.

Procedure:

(a)Total Solids:
1. Ignite the clean evaporating dishes in the muffle furnace for 30 minutes at 550°C and cool in a
desiccator.
2. Note down the empty weight of the dish (W1 ).
3. Pour a measured portion (50 to 100 mL) of the well-mixed sample into the dish and evaporate the
contents by placing the dish on a steam bath.
4. Transfer the dish to an oven maintained at either 103–105°C or 179–181°C and dry it for 1 hour. 5.
Allow the dish to cool briefly in air before placing it, while still warm in a desiccator to complete cooling
in a dry atmosphere.
6. Weigh the dish as soon as it has completely cooled (W2 ). 7. Weight of residue = (W2 – W1 ) mg. W2
and W1 should be expressed in mg.
(b) Total dissolved solids:
1. Filter a measured portion of the mixed sample (50 or 100 mL) through a filter paper and collect
the filtrate in a previously prepared and weighed evaporating dish.
2. Repeat the steps 3 to 6 outlined in total solids procedure.
3. Weight of dissolved solids = (W5 – W4 ) mg. W4 = Weight of empty evaporating dish in mg.
W5 = Weight of empty evaporating dish in mg + Residue left after evaporating the filtrate in mg.

(c)Total suspended solids:


= Total solids – Total dissolved solids.

Observation:

Sl. Item Sample I Sample Sample


no II III
.
1. Volume of sample taken
2. Wt. of empty evaporating dish = W1 mg
(For total dissolved solids)

3. Wt. of dish + total solids = W2 mg


4. Total solids = (W2 – W1) mg
5. Wt. of dish + fixed solids = W3 in mg
6. Fixed solids in mg = (W3 – W1)

7. Wt. of empty evaporating dish = W4 mg


(For total dissolved solids)

8. Wt. of dish + total dissolved solids = W5 mg


9. Total dissolved solids = (W5 – W4) mg
10. Wt. of dish + fixed dissolved solids = W6 mg
11. Fixed dissolved solids = (W6 – W4) mg
12. Total solids in mg/L
13. Total fixed solids in mg/L
14. Total dissolved solids in mg/L
15. Total suspended solids in mg/L
16. Total volatile solids in mg/L
17. Fixed dissolved solids in mg/L
18. Volatile dissolved solids in mg/L
19. Fixed suspended solids in mg/L
20. Volatile suspended solids in mg/L

21. Settleable solids in mg/L

Calculation:
1. mg/L total solids = mg total solids × 1000
mL of sample

2. mg/L total fixed solids = mg total fixed solids × 1000


mL of sample

3. mg/L total dissolved solids = mg of total dissolved solids ×1000


mL of sample

4. mg/L total suspended solids = mg/L of total solids – mg/L of total dissolved solids

5. mg/L total volatile solids = mg/L of total solids – mg/L of total fixed solids

6. mg/L fixed dissolved solids = mg fixed dissolved solids ×1000


mL of sample
7. mg/L volatile dissolved solids = mg/L total dissolved solids – mg/L of fixed dissolved solids

8. mg/L fixed suspended solids = mg/L total fixed solids – mg/L fixed dissolved solids

9. mg/L volatile suspended solids= mg/L total volatile solids – mg/L volatile dissolved solids

Result:

Sl. Items Sample Sample Sample


no. I II III

1. mg/L of total solids


2. mg/L of total fixed solids
3. mg/L of total dissolved solids
4. mg/L of total suspended solids
5. mg/L of total volatile solids
6. mg/L of fixed dissolved solids
7. mg/L of volatile dissolved solids
8. mg/L of fixed suspended solids
9. mg/L of volatile suspended solids
10. mg/L of settleable solids

Experiment-4

Aim: Determination of Alkalinity and its Species .

Apparatus Required: 1. Burette 2. Erlenmeyer flask 3. Pipettes

Principle:
The alkalinity of water is a measure of its capacity to neutralize acids. It is primarily due to salts
of weak acids, although weak or strong bases may also contribute. Alkalinity is usually imparted
by bicarbonate, carbonate and hydroxide. It is measured volumetrically by titration with 0.02 N
sulphuric acid and is reported in terms of CaCO3 equivalent. For samples whose initial pH is
above 8.3, the titration is conducted in two steps. In the first step, the titration is conducted until
the pH is lowered to 8.2, the point at which phenolphthalein indicator turns from pink to
colourless. This value corresponds to the points for conversion of carbonate to bicarbonate ion.
The second phase of titration is conducted until the pH is lowered to 4.5, corresponds to methyl
orange end point, which corresponds to the equivalence points for the conversion of
bicarbonate ion to carbonic acid.

Reagents:
1. Carbon dioxide free distilled water.
2. Phenolphthalein indicator.
3. Methyl orange indicator.
4. 0.1 N sodium thiosulphate solution
5. 0.02 N sulphuric-acid
Procedure
1. Pipette 50 mL of sample into a clean Erlenmeyer flask (V).
2. Add one drop of sodium thiosulphate solution, if residual chlorine is present.
3. Add two drops of phenolphthalein indicator; if the pH is above 8.3, colour of solution
becomes pink.
4. Titrate against standard sulphuric acid in the burette, till the colour just disappears. Note
down the volume (V1).
5. Then add two drops of methyl orange indicator, the colour turns yellow.
6. Again titrate against acid, until the colour turns to orange yellow. Note down the total
volume (V2).
OH + CO3

Phenolphthalein end point

HCO3
Methyl orange end point

Graphical Representation of Titration of Samples


Containing Various Forms of Alkalinity

pH
11

Hydroxide alkalinity

10

Carbonate alkalinity

8.3 Phenolphthalein end point

Bicarbonate alkalinity

4.5 Methyl orange end point


Observation
0.02 N H2SO4 × sample (Methyl orange/phenolphthalein indicator)
Description Trial Burette reading Volume Burette reading Volume
of sample no. (phenolphthalein of acid (methyl orange of acid
indicator) used V1 indicator) used V2
Initial Final Initial Final

Calculation
V1 × 1000
mL of sample
1. Phenolphthalein alkalinity (P) as mg/L
CaCO3 =

V2 ×
2. Total alkalinity (T) as mg/L CaCO 3 = 100
0
mL
of
sam
ple
The types of alkalinities present in the samples are calculated using the equations given in
the following table and the results are tabulated.

Result of Hydroxide Carbonate Bicarbonat


titration alkalinity alkalinity e alkalinity
as CaCO3 as CaCO3 as CaCO3
P=O O O T
P < ½T O 2P T – 2P
P = ½T O 2P O
P > ½T 2P – T 2 (T – P) O
P=T T O O
Results:

Description Hydroxide Carbonate Bicarbonate Hydroxide Carbonate


of alkalinity as alkalinity as alkalinity as carbonate bicarbonate
sample CaCO3 in mg/L CaCO3 in mg/L CaCO3 in mg/L alkalinity as alkalinity as
CaCO3 in mg/l CaCO3 in mg/L
Experiment-5(a)

Aim: Determination of pH and Acidity and Its Species

Principle:
pH value of water indicates the hydrogen ion concentration in water and concept of pH was put forward
by Sorenson (1909). pH is expressed as the logarithm of the reciprocal of the hydrogen ion concentration
in moles/ litre at a given temperature. The pH scale extends from 0 (very acidic) to 14 (very alkaline)
with 7 corresponding to exact neutrality at 25°C. pH is used in the calculation of carbonate, bicarbonate
and CO2, corrosion and stability index etc. While the alkalinity or acidity measures the total resistance to
the pH change or buffering capacity, the pH gives the hydrogen ion activity. pH can be measured
colorimetrically or electrometrically. Colorimetric method is used only for rough estimation. It can be
done either by using universal indicator or by using pH paper. The hydrogen electrode is the absolute
standard for the measurement of pH. They range from portable battery operated units to highly precise
instruments. But glass electrode is less subjected to interferences and is used in combination with a
calomel reference electrode. This system is based on the fact that a change of 1 pH unit produces an
electric charge of 59.1 mV at 25°C.

Apparatus
1. pH meter with electrode 2. Beaker 3. Thermometer
4. Colour comparator with discs 5. Cuvettes

Reagents
1. Buffer solutions 2. pH paper 3. Universal indicator

Procedure
(a) Using Universal Indicator
1. 10 mL of sample is taken in a cuvette.
2. Another 10 mL sample is taken in another cuvette and 0.2 mL of universal indicator is added
and placed in the hole provided for.
3. A colour disc corresponding to this indicator is inserted into the comparator and the disc rotated
such that the 2 circles indicate identical colours.
4. The reading is noted.
5. The procedure can be repeated using an indicator whose range is near the value obtained.
6. The exact pH is obtained.
7. (If comparators are not available, compare the colour with colours given in the chart.)
(b) Using pH Papers
1. Dip the pH paper in the sample.
2. Compare the colour with that of the colour given on the wrapper of the pH paper book.
3. Note down the pH of the sample along with its temperature.
(c) Using pH Meter
1. Follow the manufacturer’s operating instructions.
2. Dip the electrode in the buffer solution of known pH.
3. Switch on the power supply and take the reading. Standardize the instrument using the calibrating
knob.
4. After cleaning, again dip the electrodes in the buffer solution of pH 7. Note the reading. If it is 7, the
instrument is calibrated. If not, correct the value and is manipulated so that the reading in the dial comes
to 7.0.
5. A solution whose pH is to be found is taken in a beaker and the temperature knob is adjusted such that
the temperature of solution is same as that in dial.
6. The electrode is washed with distilled water and reused with the solution and then it is dipped in the
solution.
7. The reading on the dial indicates the pH of the solution.

Results:
pH
Sample no.
pH paper pH meter Universal indicator

3
Experiment-5(b)

Aim: To determine the acidity of the given sample of water.

Principle: Acidity of water is its quantitative capacity to neutralise a strong base to a


designated pH. Strong minerals acids, weak acids such as carbonic and acetic and hydrolysing
salts such as ferric and aluminium sulphates may contribute to the measured acidity. According
to the method of determination, acidity is important because acid contributes to corrosiveness
and influences certain chemical and biological processes. It is the measure of the amount of
base required to neutralise a given sample to the specific pH.
Hydrogen ions present in a sample as a result of dissociation or hydrolysis of solutes are
neutralised by titration with standard alkali. The acidity thus depends upon the end point pH or
indicator used. Dissolved CO2 is usually the major acidity component of unpolluted surface
water. In the sample, containing only carbon dioxide-bicarbonate- carbonate, titration to pH 8.3
at 25°C corresponds to stoichiometric neutralisation of carbonic acid to carbonate. Since the
colour change of phenolphthalein indicator is close to pH 8.3, this value is accepted as a
standard end point for the titration of total acidity. For more complex mixture or buffered
solution fixed end point of pH 3.7 and pH 8.3 are used. Thus, for standard determination of
acidity of wastewater and natural water, methyl orange acidity (pH 3.7) and phenolphthalein
acidity (pH 8.3) are used.
Thus, in determining the acidity of the sample the volumes of standard alkali required to
bring about colour change at pH 8.3 and at pH 3.7 are determined.

Apparatus
1. Burette 2. Pipette
3. Erlenmeyer flasks 4. Indicator solutions

Reagents
1. CO2 free water
2. Standard NaOH solution 0.02 N
3. Methyl orange indicator solution
4. Phenolphthalein indicator solution
5. Sodium thiosulphate 0.1 N.
Procedure:
1. 25 mL of sample is pipette into Erlenmeyer flask.
2. If free residual chlorine is present, 0.05 mL (1 drop) of 0.1 N thiosulphate solution is
added.
3. 2 drops of methyl orange indicator is added.
4. These contents are titrated against 0.02 N hydroxide solution. The end point is noted
when colour change from orange red to yellow.
5. Then two drops of phenolphthalein indicator is added and titration continued till a pink
colour just develops. The volumes of the titrant used are noted down.

Observation:
0.02 N NaOH× Sample (Methyl orange/phenolphthalein indicator)

Description Trial Burette reading Volume of


of sample no. NaOH used A
lnitial Final

Calculation:
=
Acidity in mg/L as CaCO 3
A
×
B
×
5
0
,
0
0
0
V
where,
Results:

Sample no. Acidity in mg/L as CaCO3


Experiment-6

Aim: To determine the total hardness present in the given sample

Apparatus Required:
Burette, Pipette, Conical flask, measuring jar

Chemicals Required:
Eriochrome Black-T (EBT) indicator, Ammonium chloride, Ammonium solution,
EDTA

Reagents Preparation:
EBT indicator
Dissolve 0.2 g of pure solid in 15 ml of distilled water
Standard EDTA Titrant
Take 0.5 g of EDTA. Heat it to 80oC for half an hour and cool it. Take 0.37 g of the
dissolve and add to get distilled water to make 100ml.
1 ml of exactly 0.02 N EDTA1mg of CaCO3
Ammonia Buffer solution
Dissolve 0.7 g of ammonium chloride (NH4C1) in 5.7ml concentrate ammonia
solution and dilute to 100 ml.

Procedure:
1. Take 20 ml of the sample in a conical flask.
2. Add 2ml of ammonia buffer to the flask.
3. Add 5 — 6 drops of EBT indicator to the flask wine red colour will be developed.
4. Titrate it with standard EDTA solution which is filled in the burette till the colour
changes from wine red to blue.
5. Repeat steps I to 4 for different samples with varying hardness and also for
distilled water (blank)
6. For determination of non-carbonate hardness the sample is to be boiled for 30
minutes. The procedure is the same as above.

Sanitary Significance:
Hard water has adverse action with soap since it allows less formation of leather. If
hard water is used in boilers, scaling problem occurs leading to the bursting of
boilers, It makes food tasteless. It affects the working of dyeing process. It is also
precipitate protein of meat and make tasteless.
Observation:

Silver nitrate Vs Sodium Chloride


Volume of Burette AgNO3
S.No. water sample Reading (ml) consumed
(ml) Initial Final (ml)

Concordant Value = ml

Silver Nitrate Vs Sample

Burette Reading (ml) AgNO3


Volume of water Chlorides
S.No. consumed
sample (ml) Initial Final (mg/L)
(ml)

Calculation:

Normality of Silver nitrate: Volume normality of NaCl


Vol of AgNo3
Chloride mg/L = Volume of Agno3x1000x35.45xN
Vol of Sample Taken

Results: Total Hardness in mg of CaCO3 mg/L

Experiment-7

Aim: Determination of Chlorides in Given Sample.

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

Apparatus:
1. Burette
2. Pipettes
3. Erlenmeyer flasks
4. Measuring cylinder

Reagents:
1. Chloride free distilled water.
2. Standard silver nitrate solution (0.0141N)
3. Potassium chromate indicator.
4. Acid or alkali for adjusting pH.
Procedure:
1. Take 50mL of sample (V) and dilute to 100mL.
2. If the sample is coloured add 3mL of aluminium hydroxide, shake well; allow to settle,
filter, wash and collect filtrate.
3. Sample is brought to pH 7–8 by adding acid or alkali as required.
4. Add 1mL of indicator (Potassium chromate).
5. Titrate the solution against standard silver nitrate solution until a reddish brown
precipitate is obtained. Note down the volume (V1).
6. Repeat the procedure for blank and note down the volume (V2).
Observation:

Water sample vs Silver nitrate (0.0141 N)


(Potassium chromate indicator)

Sample Trial Volume Burette reading Volume of Chloride


no. no. of Initial Final silver nitrate mg/L
sample (mL)
(mL)
1

1 2

2 2

3 2

1
Distilled
2
Water
3

(Specimen calculation:) for one sample (Sample No )


V =
V1 =
V2 =
N=

(V1 – V2 ) × N × 35.46 × 1000


Chloride in mg/L = V
(V1 – V2 ) × 500 mg / L
= V
Results:

Description of sample Chloride concentration in mg/L


Experiment-8

Aim: To determine the fluorides present in the give sample.

Apparatus Required:
Burette with stand, Pipette, Conical flask, measuring flask.

Chemical required:
Oxalate, concentrated hydrochloric acid, phenolphthalein indicator, sodium
hydroxide.

Reagents Preparation:
Oxalate Solution:
Dissolve 630mg of oxalate in distilled water and make up to l00ml.

Phenolphthalein indicator:
Add ig of phenolphthalein in 200 ml distilled water and dissolve it. Add 0.02N
Sodium hydroxide solution drop wise until a faint pink colour appears.

Sodium hydroxide solution:


Dissolve 4g of sodium hydroxide in distilled water and make up to 100ml.

Procedure:
Titration — I NaoH Vs Oxalic acid
1. Pipette 20m1 of oralic acid solution into the conical flast.
2. Add one or two drops of phenolphthalein indicator.
3. Titrate against sodium hydroxide solution until the appearance of pink
colour.
4. Repeat the titration for concordant values.
Titration —II NaoH Vs Sample:
1. Take 19m1 of sample in the conical flask and add 1 ml of concentrated
hydrochloric acid.
2. Add one or two drops of phenolphthalein indicator.
3. Titrate against sodium hydroxide solution until the appearance of pink colour.
4. Repeat the titration for concordant values.
Observation:

Titration – I NaoH Vs Oxalic acid


Volume Burette reading (ml) Volume of
Sampl
sample Initial Final NaoH used End Point
e
taken (ml) reading reading (ml)
details

Appearanc
Oxalic acid e of pale
pink colour

Titration – II NaoH Vs Sample


Volume Burette reading (ml) Volume of
Sampl
sample Initial Final NaoH used End Point
e
taken (ml) reading reading (ml)
details

Appearanc
Tap Water e of pale
pink colour

Titration – III NaoH Vs HCL


Volume Burette reading (ml) Volume of
Sampl
sample Initial Final NaoH used End Point
e
taken (ml) reading reading (ml)
details

Appearanc
Conc .HCL e of pale
pink colour
Calculation:

Titration I
Volume of oxalic acid×Normality of
oxalic acid
Normality of NaOHX =
Volume of NaoH

Titration II
Volume of NaOH×Normality of NaOH
Normality of SampleY = Volume of Sample

Titration II-III×X×Y
Amount of Flourides =
Volume of Sample

Titration — Ill NaoH Vs Hcl:

1. Take 19m1 of distilled water in the conical flask and add imi of concentrated
hydrochloric acid.
2. Add one or two drops of phenolphthalein indicator.
3. Titrate against sodium hydroxide solution until the appearance of pink colour.
4. Repeat the titration for concordant values.
OBSERVATION :
Source of sample :
Date of collection :
Time :
Temperature
: Tabulation
Titration – I NaoH Vs Oxalic acid
Volume Burette reading (ml) Volume of
Sampl
sample Initial Final NaoH used End Point
e
taken (ml) reading reading (ml)
details

Appearanc
Oxalic acid e of pale
pink colour

Concordant Value = ml

Titration – II NaoH Vs Sample


Volume Burette reading (ml) Volume of
Sampl
sample Initial Final NaoH End Point
e
taken (ml) reading reading used (ml)
details

Appearanc
Ammonia
e of pale
solution
pink colour

Concordant Value = ml

Titration – III NaoH Vs HCL


Volume Burette reading (ml) Volume of
Sampl
sample Initial Final NaoH used End Point
e
taken (ml) reading reading (ml)
details

Appearanc
Sewage e of pale
pink colour

Concordant Value = ml
Result:

Amount of fluorides present in the given sample (Tap water)


_______________mg/L.
Experiment-9

Aim: To determine the optimum dosage of coagulant required for a given sample of waste water.

Apparatus Required:
1. 1 .Laboratory flocculator with stirring paddles
2. Glass Jars
3. Analytical balance

Reagents Required: Alum

Theory:
The amount of coagulant required for coagulation depends on the turbidity
of the waste water. The use of optimum amount of coagulant is indicated by the
formation of the large feathery flakes. This can be approximately determined in
the laboratory by Jar test. The test involves rapid mixing to disperse the
chemicals (coagulants) in the sample and slow mixing for the floc formation.

PROCEDURE:
1. Fill 1 litre waste water sample in each of the six jars
2. Attach the sample jars to the stirring device by lifting he paddles in the
right upward direction.
3. Add coagulant (Alum) in progressive dosages into the series of the six sample jars.
4. The coagulant dosage can be selected randomly depending on the
characteristics of waste water.
5. Mix the sample rapidly for about 10 mm with mechanically operated
paddles at 180rpm followed by gentle stirring about 10 mm. at 30—40 rpm
6. Remove the jars from the stirring device after stirring is completed
7. Let the sample in the jars stand for 30 mm. for settling of floc.
8. The dose of coagulant versus floc formation is plotted as graph.
9. The dose of coagulant which gives the best floc is the optimum dose of coagulants.
OBSERVATION :

Test on water sample Test on water sample


quantity
ml (Burette Reading) ml (Burette Reading)
of water Chlorine
S.No. sample Na2S2O3 Na2S2O3 residuals
used in Initial Final Used (x Initial Final Used (y Mg/L
ml ml) ml)

Calculation:

Residual Chlorine in original water sample

= (x – y)× 1000 ×0.8895

ml of water sample
= Mg/L

Result: The optimum coagulant dosage mg/L


Experiment-10

Aim: To determine the residual chlorine for the given water sample

Apparatus Required
1. Burette with stand, tiles
2. Pipette
3. Conical flask
4. Beaker
5. Glass funnel
6. Measuring jar
Principle:
Chlorine combines with water to form Hypochlorous and Hydrochloric acids
C12+H2O->HOC1+H++C1-
In water chlorine, hypochiorous acid and hypo chlorite ions are referred as free
chlorine residuals and the chloramines are called combined chlorine residuals.
The chlorine demand of water is the amount of chlorine that must be supplied to
leave a desired free combined or total residual after a specified contact period.
The starch iodide test is an age old method for testing the total chlorine residual in a
given water sample and is still being used, depending upon the oxidizing power of
free and combined chlorine to convert iodide ion to free iodide. This free iodine
liberates iodine ions when titrated with sodium thiosulphate as shown below;
C12+2I¯ ----------I2+2C1-
I2+Starch ----------Blue colour
I2+Na2S2O3 -----------Na2S4O6+2NaI
(Or) I2+2S2O3 ---------S4O6+2I

Reagents Required:
Chlorine water I gmL /
Acetic Acid
Standard N/40 Sodium thiosulphate solution
Starch indicator

Reagents Preparation:

Starch Indicator:
Weigh I g of starch and make it into a paste with 10 ml of hot water and dilute it to
100 ml.
Standard N/40 Sodium Thiosulphate solution:
Dissolve 1.575 gm of NaS2O3 in distilled water and make up to 1 litre. Procedure
1. Take 25 ml of given water sample in a conical flask.
2. Add a small crystal of KI and distilled water to the above flask containing water
sample, to make 1 00m
3. Add about 0.5 ml conc.HC1 or about 100ml acetic acid to act as buffer to reduce
the pH to a low value between 3.5 to 4.2 to avoid conversion of Cl2 into HOCI and
OCL-
4. Titrate the above yellow coloured iodine solution against standard Sodium thio
sulphate till yellow becomes light or faintly yellow.

5. Add 1 ml of soluble starch solution (end point indicator) to change the colour
from light yellow to blue in the conical flask.
6. Continue the titration with standard sodium thiosulphate till the blue colour just
disappears.
7. Note. down the total amount of titrant used in the entire titration. Let it be x ml.
8. Repeat the titration with distilled water as sample and determine the amount of
sodium thiosuiphate .let it be y ml.

Calculation:

Volume of
EDTA
water Hardness
S.No. Burette Reading (ml) Consumed
sample (mg/L)
(ml)
(ml)
Initial Final

Calculation:

Hardness in mg/1 of CaCO3 = ml of EDTA usedx 1000


ml of water sample

Result
Residual Chlorine residuals for given water sample by Starch Iodide Test is =
____________________mg/L.

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