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LABORATORY MANUAL
Mr. SATHISHKUMAR A.S Mr. VETRISUBAM
Prepared By
WATER AND WASTE WATER ANALYSIS LABORATORY
LAB MANUAL
Academic Year : 2022 - 2023
Subject Code : CE8512
Regulations : R21
Class : V Semester (CE)
DEPARTMENT OF CIVIL ENGINEERING
SBM COLLEGE OF ENGINEERING AND TECHNOLOGY
SBM Nagar, Thamaraipadi, Dindigul - 624 005
Registration Number : ____________________________________
Name of the Student : ____________________________________
Assistant Professor Assistant Professor
2
CE8512 - WATER AND WASTE WATER ANALYSIS LABORATORY
LIST OF EXPERIMENTS
1.Determination of pH , Turbidity , Conductivity
2.Determination of Hardness
3.Determination of Alkalinity and Acidity
4. Determination of Chlorides
5.Determination of Phosphates and Sulphates
6.Determination of Iron and Fluoride
7.Determination of Optimum Coagulant dosage
8.Determination of residual chlorine and available chlorine in bleaching powder
9.Determination of oil and Grease
10.Determination of suspended , settleable , volatile and fixed solids
11.Determination of Dissolved oxygen and BOD for given sample
12.Determination of COD for given sample
13.Determination of SVI of biological sludge and microscopic examination
14.Determination of MPN index of given sample
.
3
CONTENTS
S.No Experiments Name Pg No
1
Determination of pH , Turbidity , Conductivity
a) Ph 6
b) Turbidity 9
c) Conductivity 12
2 Determination of Hardness 16
3
Determination of Alkalinity and Acidity
a) Alkalinity 20
b) Acidity 23
4 Determination of Chlorides 27
5
Determination of Phosphates and Sulphates
a) Phosphates 31
b) Sulphates 36
6
Determination of Iron and Fluoride
a) Iron 40
b) Fluoride 44
4
7 Determination of Optimum Coagulant dosage 49
8 Determination of residual chlorine and available chlorine in
bleaching powder
53
9 Determination of oil and Grease 57
10 Determination of suspended , settleable , volatile and fixed
solids
61
11
Determination of Dissolved oxygen and BOD for given sample
a) DO 66
b) BOD 68
12 Determination of COD for given sample 73
13 Determination of SVI of biological sludge and microscopic
examination
79
14 Determination of MPN index of given sample 83
VIVA VOCE QUESTIONS 87
CONCLUSION 97
5
EXP NO 1
DETERMINATION
of
pH, TURBIDITY
AND CONDUCTIVITY
6
1.a) DETERMINATION OF pH :-
AIM :-
To determine the pH of the given waste water sample.
APPARATUS REQUIRED
1. pH meter with pH electrodes.
2. Thermometer.
ACIDS / REAGENTS REQUIRED
1. Buffer solution.
2. pH tablets no = 4, 7, 10
7
SAMPLES TAKEN :
2 Beakers
a) first = pH buffer tablet no 4 ( colorless )
b) second = pH buffer tablet no 7 ( colorless )
PROCEDURE:-
1. Calibrate the electrodes with two standard buffer solution of pH 4 and 9
buffer solution. It is a solution offering resistances.
2. The sample temperature is determined at the same time and is entered into
the meter to allow for a temperature correction.
3. Raise the electrodes thoroughly mix it with ionized distilled water and
carefully wipe it with a tissue paper.
4. Dip the electrode into the sample solution wait upto 1 min for steady reading
the pH meter reading within ±0.1 pH unit will be adequate for such work.
5. The reading is taken and the indicator value remains constant for about 9
minutes
pH= log10 [
𝟏
𝑯+
]
8
TABULATION :-
Description of sample Temperature Ph
Blank
4.0
7.0
END POINT :-
RESULT
The pH value of the given waste water sample is ____________
9
1b. DETERMINATION OF TURBIDITY :-
AIM :-
To determine the turbidity of the given sample of waste water using
nephelometric turbidity meter.(20NTU)
PRINCIPLE :-
Nephelo turbidity meter operator on the principle of light passing through a
substance of light passing. In this a strong light beam is passing upward
APPARATUS REQUIRED
1. Nepheolo turbidity water meter
GLASSWARE REQUIRED :-
 Cuvette
 Measuring Cylinder
 Beaker
 Rinser
10
ACIDS / REAGENTS REQUIRED :-
 H2SO4 ( colorless )
SAMPLES TAKEN :
Beaker :- H2SO4 ( Colorless )
PROCEDURE:
1. Switch ON the instrument and let the instrument warm for 15-20 minutes.
2. Insert the cell with distilled water into the cell holder. Cover the cell with
light shield.
3. Select the sang [ 1-100 NTU] as yield by range on panel meter with the help
of “Set Zero” control knobs.
4. Select the range for use insert the all with standards solution [20 NTU] cell
holder. Adjust standardized control to set to 20 on the panel.
5. Insert cell rider in 100 NTU range and adjust to panel meter.
6. Repeat step 3 and 4 till you get zero and standard control.
7. Now insert all the sample solution and note the reading.
8. The meter scale is marked from 0-100 for NTU range read 100 as 20 NTU.
(A). In 100 NTU range inserts cell riser first, insert the cell will distilled water and
adjust to zero.
(B). Always adjust zero in highest sensitivity to set better adjustment.
H2SO4  H2 + SO4
11
TABULATION :-
Sample Range selected Turbidity NTU
END POINT :-
RESULT :-
Turbidity of given sample ________________ NTU
12
1.c) DETERMINATION OF ELECTRICAL CONDUCTIVITY :-
AIM :-
To determine the electrical conductivity of given water sample
PRINCIPLE :-
Electrical conductivity of water is the ability to conduct an electric current .
Salts and other chemicals that dissolve in water can break down in to positively
and negatively charged ions . It depends upon the concentration of the ions.
Conductivity is the reciprocal of resistance . Its unit is μmho/cm
G= k (A/L)
Where k is the conductivity or specific conductance
APPARATUS REQUIRED :-
1. Conductivity meter with conductivity cell
13
GLASSWARES REQUIRED :-
 Beaker
 Rinser
 Measuring Cylinder
ACIDS / REAGENTS REQUIRED :-
 KCl ( colorless )
SAMPLES TAKEN :
 Beaker – KCl ( colorless solution )
PRINCIPLE :-
1.Calibarte the conductivity meter as per the directions were given by the
manufacturer’s manual using standard solutions
2. Rinse the cell with the sample , measure the sample resistance or conductivity
PROCEDURE :-
 Take 50ml of water sample
 Add 2g of KCl in it and mix properly
 Switch ON the conductivity meter and warm it in for 5minutes
 Keep the Calibration control as it by constant it will shows green light
 Set the temperature at 27°C
 Turn it in to Calibration control again it will shows red light
 Rinse the electrode in prepared KCl solution and note down the proper
reading
KCl  K+
+ Cl-
14
TABULATION :-
Sample details Conductivity
measured corrected
CALCULATION :-
Conductivity of cell = Measured value * cell constant * Correction factor
= ------ μmho/cm
Where ,
Cell constant – 1.02
Correction factor – 1.05
RESULT :-
Electrical conductivity of the water = -------- μmhos/cm
15
Exp No 2
DETERMINATION
OF HARDNESS
16
Exp No 2 DETERMINATION OF HARDNESS
AIM :-
To determine the total hardness of water
PRINCIPLE:-
Hardness in water is that characteristics which prevents the formation of
sufficient foam or lather when such hard waters are mixed with soap . It is usually
caused by presence of Ca and Mg salts present in water , which forms scum by
reaction with soap .
Bicarbonates and carbonates of Ca and Mg ions are called temporary while
sulphates , nitrates , chlorides of Ca and Mg
The total hardness of the given sample of water be easily computed by
titration method by using EDTA solution either in a solution or salt .
The indicator dye which is found to be serve an excellent indicator to show
all hardness ions is called Eriochrome Black T having blue colour is added to
water with pH of 10 ,. It combined with divalent metallic ion having wine red in
colour
S.No Category Hardness
1 Soft 0-75
2 Moderately Hard 75-150
3 Hard 150-300
4 Very hard >300
GLASSWARES REQUIRED :-
1. Conical flasks
2. Burette
3. Pipette
4. Beakers
17
ACIDS / REAGENTS REQUIRED :-
1. Standard N/50 EDTA solution (Colorless)
2. EBT indicator( Black)
3. Ammonia buffer (Colorless)
SAMPLES TAKEN :
Beaker = Water sample with EBT indicator added ( wine red solution )
Burette = EDTA solution ( Colorless )
Final = Solution ( Sky blue colour )
PROCEDURE:-
1. Take 100ml of water sample in conical flask
2. Add 1ml of ammonia buffer to flask
3. Add 6 drops of EBT indicator in to flask . Wine red colour will be developed
4. Titrate it with EDTA solution till the colour changes from wine red to deep
blue
5. Hardness in mg/lt =
𝑚𝑙 𝑜𝑓 𝐸𝐷𝑇𝐴 𝑢𝑠𝑒𝑑∗
𝑁
50
∗50∗1000
𝑚𝑙 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
as CaCO3
TABULATION :-
Sample No ml of water
sample used
in flask
(2)
Initial
burette
reading
(3)
Final
burette
reading
(4)
ml of N/50
EDTA used
in ml
(5)
Hardness
mg/lt
CaCO3 =
(5/2)*1000
18
END POINT :-
RESULT :-
Hardness of the given water sample = ------------ mg/lt
19
EXP NO 3
DETERMINATION
OF
ALKALINITY
AND
ACIDIITY
20
3.a) DETERMINATION OF ALKALINITY :-
AIM :-
To measure alkalinity by using indicators to find phenolphthalein alkalinity and
total alkalinity
PRINCIPLE :-
Alkalinity is due to presence of salts of weak acids . It is a classified as in three
forms . They are Hydroxide alkalinity , carbonate alkalinity, Bicarbonate
alkalinity. Among these Bicarbonate alkalinity is major constituent . It is measure
on CaCO3 scale as mg/lt of CaCO3 .
APPARATUS REQUIRED :-
1. Burette
2. Conical flask
3. Measuring cylinder
4. Beakers
ACIDS / REAGENTS REQUIRED :-
1. Phenolphthalein indicator ( colorless )
2. Methyl orange indicator ( red orange )
3. Standard N/50 sulphuric acid ( colorless )
SAMPLES TAKEN :-
2Beakers
a) 1st
= Phenolphthalien with water sample ( light pink )
b) 2nd
= methyl orange with water sample ( light orange )
Burette = H2SO4 ( Colorless )
Final
a) 1st
= colorless
b) 2nd
= light orange
21
PROCEDURE :-
1) Fill the burette with H2SO4 solution up to mark
2) Take 100ml of sample which is to be tested in measuring cylinder and filled
in to conical flaks and note down the initial reading
3) Now 3-4 drops of Phenolphthalein in to this solution and mixed thoroughly
and it turns to pink colour and titrate it with H2SO4 solution
4) Open the cock of burette with constant rate when the pink colour
disappears and note down the reading as final reading as of
phenolphthalein indicator
5) Then add 1 drop of methyl orange indicator in the same solution and it is
titrated with H2SO4 till it gets appearance of light orange colour and
note down the final reading as of methyl orange indicator
6) Repeat the procedures for 3-4 trails
7) To find the H2SO4 volume , to deduct the final reading from initial reading
8) Then find the total volume by adding both values ( phenolphthalein and
methyl orange of sample
TABULATION :-
a)As a phenolphthalein indicator
S.No Sample
volume (ml)
Initial reading Final reading Volume of
H2SO4 used
(ml)
b)As a Methyl Orange indicator
S.No Sample
volume (ml)
Initial reading Final reading Volume of
H2SO4 used
(ml)
22
END POINT OF PHENOLPTHALEIN :-

END POINT OF METHYL ORANGE :-

CALCULATIONS :-
a)Phenolphthalein alkalinity = (P*1000) /( ml of sample) = ---------mg/lt
b)Total alkalinity = (T*1000)/ (ml of sample ) = ----- mg/lt
RESULT :-
Phenolphthalein alkalinity = ----- mg/lt
Total alkalinity = ------ mg/lt
23
3.b) DETERMINATION OF ACIDITTY :-
AIM :-
To measure acidity by using mineral and phenolphthalein acidity
PRINCIPLE :-
Acidity is the caused by CO2 and mineral acids , sulphates of iron and
aluminium . It is measure on CaCO3 scale as mg/lt of CaCO3 .
GLASSWARES REQUIRED :
1. Burette
2. Conical flask
3. Measuring cylinder
4. Beakers
ACIDS / REAGENTS REQUIRED :-
1. Methyl orange ( red orange solution )
2. Phenolphthalein indicator ( colorless )
3. Standard N/50 NaOH solution (colorless)
SAMPLE TAKEN :
Beaker :-
a) First beaker – light orange ( sample with methyl orange )
b) Second beaker – colorless ( sample with phenolpthalien )
Final = orange to pink / lavender
PROCEDURE :-
1) Fill the burette with NaOH solution up to mark
2) Take 100ml of sample which is to be tested in measuring cylinder and
filled in to conical flaks and note down the initial reading
3) Add 1 drop of methyl orange indicator in the same solution and it is
titrated with NaOH till it gets appearance of light orange colour
24
4) Then add 0.5ml of Phenolphthalein in to this solution and mixed
thoroughly and it is colourless
5) Note the initial reading of both indicator values
6) Now these can be titrated with NaOH solution , it turns to lavender
colour . It is end point . Now it is persist for 30seconds
7) Note the final reading
END POINT :-

TABULATION :-
a)As a phenolphthalein indicator
S.No Sample
volume (ml)
Initial reading Final reading Volume of
NaOH used
(ml)
25
b)As a Methyl Orange indicator
S.No Sample
volume (ml)
Initial reading Final reading Volume of
NaOH used
(ml)
CALCULATIONS :-
a) Mineral acidity mg/lt =
𝑚𝑙 𝑜𝑓 𝑁𝑎𝑂𝐻 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 𝑢𝑠𝑒𝑑 𝑤𝑖𝑡ℎ 𝑚𝑒𝑡ℎ𝑦𝑙 𝑜𝑟𝑎𝑛𝑔𝑒
𝑚𝑙 𝑠𝑎𝑚𝑝𝑙𝑒
b) Total acidity mg/lt =
𝑚𝑙 𝑜𝑓 𝑁𝑎𝑂𝐻 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 𝑢𝑠𝑒𝑑 𝑤𝑖𝑡ℎ 𝑝ℎ𝑒𝑛𝑜𝑙𝑝ℎ𝑡ℎ𝑎𝑙𝑒𝑖𝑛
𝑚𝑙 𝑠𝑎𝑚𝑝𝑙𝑒
RESULT :-
Mineral acidity = -----------mg /lt
Total acidity = ---------- mg/lt
26
Exp NO 4
DETERMINATION
OF
CHLORIDES
27
Exp NO 4 DETERMINATION OF CHLORIDES
AIM :-
To determine the chloride content in given water sample
PRINCIPLE :-
Chloride is the one of the inorganic matter in water sample . The chloride
content in raw water is slight highly . So this can be determined by Mohr’s method
uses silver nitrate solution with normality of 0.014 which is titrated against the
standard sodium chloride solution . But the indicatr KMnO4 is added to realize the
end point of this experiment
AgNO3 + NaCl  NaNO3 + AgCl
This AgCl is substance which is in milky white which denotes end point of
this experiment . It is limited up to 250mg/lt – 600mg/lt
APPARATUS REQUIRED :-
1. Beaker
2. Burette
3. Pipette
ACIDS / REAGENTS REQUIRED :-
1. KMnO4 as indicator ( Dark Yellow )
2. Silver nitrate solution ( Colorless )
3. NaCl (Colorless)
SAMPLE TAKEN :
Burette = Silver nitrate ( Colorless)
Beaker = Pale yellow solution ( KMnO4 + sample )
Final = Brickish red solution
28
PROCEDURE :-
1) Take 20ml of water sample in measuring cylinder and pour in it without
air bubbles and this is transfer in to conical flask
2) Take 5ml of NaCl solution in cylinder and add this also in to flask
3) Now take silver nitrate solution in to burette up to mark
4) Now take indicator KMnO4 as in 4-5 drops in to prepared conical flask
solution
5) Now flask solution is titrated with burette solution until it turns in to pale
yellow colour which denotes the chloride in water sample
6) The Silver nirate reacts with potassium chromate which gives a final
solution as silver chromate which is in a red brown colour
TABULATION :-
S.No Sample
volume (ml)
Initial reading Final reading Volume of
AgNO3 used
(ml)
CALCULATION :-
Chloride ion concentration (mg/lt)
= (A*N*35.45*1000) / Volume of sample (V)
= --------- mg/lt
AgNO3 + K2CrO4  Ag2CrO4 + 2KNO3
Ag2CrO4 denotes the red brown colour
29
END POINT

RESULT :-
Chloride content = ------- mg/lt
30
EXP NO 5
DETERMINATION
OF
PHOSPHATES
AND
SULPHATES
31
5.a) DETERMINATION OF PHOSPHATES :-
AIM :-
To Determine the phosphates content in water sample by spectrophotometer.
PRINCIPLE :-
Phosphates in acidic condition reacts with ammonium molybdate to
form molybdophosphoric acid which is then reduced to molybdenum blue by
adding stannous chloride. The intensity of the blue colored complex is measured
spectrophotometrically,which is directly proportional to the concentration of
phosphate present in the sample.
APPARATUS REQUIRED :-
1. Spectrophotometer
GLASSWARES REQUIRED :-
1) Pipettes
2) Measuring cylinder
3) Glass-rod
4) Beakers
5) Dropper.
32
ACIDS / REAGENTS REQUIRED :-
1. Ammonium molybdate solution
2. Stannous chloride solution
3. Standard Phosphate Solution
SAMPLES TAKEN :-
Beaker = Ammonium Molybdate ( creamy white / creamy green solution )
Stannous Chloride solution ( colorless )
Burette = Standard phosphate solution ( Colorless solution )
Final = Sky blue solution
REAGENTS PREPARATION :-
1.Ammonium molybdate solution
In 175 ml of distilled water, add 25 g of ammonium molybdate. Now add 280
ml of conc.sulphuric acid in 400 ml of distilled water and cool it. Make the volume
upto 1 litres with distilled water which gives faint green solution
2. Stannous chloride solution
Dissolve 2.5 g of stannous chloride in 100 ml glycerol by heating in a water
bath
3. Standard Phosphate Solution
Dissolve 4.388 g of anhydrous potassium hydrogen phosphate in 1000 ml
distilled water. Dilute this solution to 100 times (10ml-1000ml).This solution
contains 10 mg P/l (1ml = 0.01 mg P) which is used as standard phosphate
solution.
33
PROCEDURE :-
1. Switch ON the spectrophotometer and allow 20 minutes for warm up and
set 410 nm by adjusting the wavelength knob.
2. For calibration of the instrument take distilled water in the cuvette holder
and place in the compartment on the light path and close the
compartment.
3. Press the mode button to set transmittance mode and set 100 % T.
4. Again press the mode button to set it for absorbance to read 0.00.
5. Fill the prepared standard solutions in the cuvette holders and place in
the compartment.
6. Read the colour developed on the display and note down the peak value.
7. Take 25 ml of filtered and clear sample.
8. Add 1 ml of ammonium molybdate solution and 2 drops of stannous
chloride which gives faint green solution
9. Measure the blue color developed at 690 nm on a spectrophotometer
using a distilled water blank with the same chemicals.
10.Note down the readings of spectrophotometer after 5 minutes but before
12 minutes of the addition of the last reagent.
11.Find out the concentration of the phosphate with the help of the standard
curve.
TABULATION :-
S No Initial volume Final volume Volume of
ammonium
molybdate
solution
34
END POINT :-
MODEL GRAPH :-
Display
Readings
Phosphate concentration in mg 
35
RESULT :-
The amount of phosphates determined from the given sample is ________mg/l.
36
5.b)DETERMINATION OF SULPHATES
AIM :-
To determine the sulphates of the sample by spectrophotometer method
APPARATUS REQUIRED :-
1)Spectrophotometer
ACIDS / REAGENTS REQUIRED :-
1. Barium Chloride
2. Magnesium sulphate
SAMPLES TAKEN :
Beaker –
a) Barium shloride solution ( colourless )
b) Magnesium sulphate solution ( colourless )
Final = Greenish Solution
37
PROCEDURE :-
1. Set the meter to zero and calibrate it without keeping at air passing place
2. Take Barium chloride powder is added in to magnesium sulphate sample of
10ml and mixed well which gives greenish solution
BaCl2 + MgSO4  BaSO4 + MgCl2
3. Place the cuvette in holder of the meter and rotate it to stand in position
4. Press READ button for 3 seconds and count down will starts from 5
minutes
5. This resultant value is shown in spectrophotometer screen
TABULATION :-
Sample No Initial reading
(mg/lt)
Final reading
(mg/lt)
Volume of
barium chloride
used (mg/lt)
38
END POINT :
RESULT :-
Amount of sulphates = ----- mg/lt
39
EXP No 6
DETERMINATION
OF
IRON
AND
FLUORIDES
40
6.a) DETERMINATION OF IRON :-
AIM :-
To determine the iron content in water sample by spectrophotometer method
PRINCIPLE :-
Iron is only toxic at very high concentrations , it acts as a useful surrogate for
other heavy metals . So it is limit up to 0.3ppm
APPARATUS REQUIRED :-
1. Spectrophotometer
GLASSWARES REQUIRED :-
2. Volumetric flasks
3. Beakers
4. Flasks
5. Volumetric flask
ACIDS / REAGENTS REQUIRED :-
1. Standard iron solution
2. Unknown solution
3. Hydroxyammonium chloride
4. Phenanthroline indicator
41
SAMPLES TAKEN :
Pipette – Iron solution ( Green solution )
6 Volumetric flasks
a) 1st
volumetric flask – blank( colorless )
b) 2nd
volumetric solution – 2.5ml of iron solution ( light orange )
c) 3rd
volumetric solution – 5ml of iron solution ( slight orange )
d) 4th
volumetric solution – 7.5ml of iron solution ( thin orange )
e) 5th
volumetric solution – 10ml of iron solution ( thickish dark orange )
Phenonthraline indicator ( thick red colour )
Beaker – Light orange solution
PROCEDURE :-
1. Take 200ppm of iron solution and pipette it with 25ml
2. Add it to 500ml A grade Volumetric flask and add distilled water about of
its half
3. Shake well and finalize the volume with 500ml up to mark of flask and add
distilled water up to this mark
4. Shake well and intermediate iron solution of 10ppm is ready Take
membrane filter unit to find dissolved iron in water sample by closing filter
base with filter paper and close it tightly
5. Add sample water and connects suction pump and give such pressure by
sucking out
6. Calibration standard from blank , 0.1ppm , 0.5ppm,1.0ppm,1.5ppm,2ppm
iron and take each beaker for each solution
7. Pipette 50ml of sample water after filter unit
8. Add 0.5ml to prepare 0.1ppm Fe , 2.5ml to prepare 0.5ppm Fe , 5ml to
prepare 1ppm Fe , 7.5ml to prepare 1.5ppm Fe , 10ml to prepare 2ppm Fe
9. Add 1+1 Hl is pipette and add 2ml to each beaker to reduce interference by
organic matter
10. 1ml of hydroxyammonium chloride to each beaker and it is used as
reducing agent to reduce ferric ions to ferrous ions
11.Then add 50ml distilled water to each beaker except in sample
42
12.Now Heat all beakers in hot plate inside fume hood to digest heat until
volume reduced to 10-20ml
13.After cooling this residual volume
14.Transfer each in to 50ml A grade volumetric flask is labeled as 0.1-2ppm Fe
and sample and rinse properly
15. Then take ammonium acetate and pipette it with 10ml to each flask which
is used to maintain pH about 3.5 for complete complexation of ferrous ions
with phenanthroline and shake it well
16.Finally add phenonthroline in each beaker of 4ml with ferrous ions to give
pale orange complex
17.Add 50ml of distilled water in each flask as final volume reading and shake
well
Fe + 3 Phen  Fe(Phen)3
END POINT :-
43
MODEL GRAPH
Fe abs
0 0.5 1 1.5 2 2.5 3 3.5
Concentration (ppm) 
RESULT :
Iron Content = ------- mg/lt
44
6.b)DETERMINATION OF FLUORIDE
AIM :-
To determine the fluoride content in given water sample by spands method
ACIDS / REAGENTS REQUIRED :-
1. Spands Tri-sodium salt solution
2. Zinconyl acid reagent
3. Sodium arsenite solution
GLASSWARES REQUIRED :-
1. Burette
2. Pipette
3. Conical flask
45
SAMPLES TAKEN :
6 Volumetric flasks
a) First flask = blank ( colorless )
b) Second flask = 0.5ml of SPADNS solution ( thinnish red )
c) Third flask = 1ml of SPADNS solution ( slight thickish red )
d) Fourth solution = 1.5ml of SPADNS solution ( thickish red )
e) Fifth solution = 2ml of SPADNS solution ( normal red solution )
f) Sixth solution = 2.5ml of SPADNS solution ( blood red solution )
Pipette – zirconyl chloride solution ( colorless )
Flask – Sodium arsenite solution ( colourless )
Final = Blood red solution
PROCEDURE :-
a)Preparation of sample :-
1. Take Spadns tri-sodium salt of 0.3g in 500ml volumetric flask and half of
the distilled water to that flask and shake well
2. It is in beetroot red colour solution and store it in a amber glass bottle
protected from direct sunlight
3. To prepare Zinconyl acid reagent by adding conc .HCl and Zinconyl
chloride octahydrate of 0.133g zinconyl chloride in 500ml volumetric flask
and add 25ml of distilled water in it , also add 350ml conc . HCl slowly and
carefully upto mark
4. It is store in a reagent glass bottle
5. Mix equal volume of both spadns solution and zinconyl acid solution
6. Sodium arsenite NaASO2 is prepared by this salt weighed of 2.5gm in
volumetric flask
7. Add distilled water up to half of the flask and shake well
b)Test procedure :-
1. Pipette 10ml of spadns solution and add in 250ml volumetric flask and then
add 100ml distilled water
2. Take 3ml of distilled water in measuring cylinder and 7ml of Conc HCl is in
it carefully and safely And add this in to standard Spadns solution
46
3. It is thick blood red colour
4. To find the fluoride content in this sample , add sodium fluoride of 0.2gm in
1000ml volumetric flask and add distilled water to half of flask , shake well
of fluoride 10ppm by knowing blank , 0.5ppm , 1.0ppm , 1.5ppm and
sample solution
5. Add 10ml of zinconyl acid + spadns solution in this each flask , shake well
and add distilled water in it to half level
END POINT :-
47
TABULATION :-
Sample no Initial reading Final reading Volume of
spands
solution
Volume of
zinconyl acid
solution
RESULT :-
Fluorides Content = -----mg/lt
48
EXP No 7
DETERMINATION
OF
OPTIMUM COAGULANT
DOSAGE
49
Exp No 7 DETERMINATION OF OPTIMUM COAGULANT DOSAGE
AIM :-
To determine the optimum coagulant dosage by using jar test
PRINCIPLE :-
Raw water contains some suspended impurities . Some of these can be
removed by sedimentation and some of them cannot be easily removed . So we
have do the coagulation process . Optimum dose of coagulant is the miminum dose
of the coagulant that will be remove the maximum turbidity in water by using jar
test
APPARATUS REQUIRED :-
1. Jar test – Having 6 pedals can be independently move up or down , electric
motor operates the jar , speed control , time control , platform transparent
sheet with tube light , Counter measures number of rotation
GLASSWARES REQUIRED :-
1) 6 glass jars of 1lt capacity
2) Measuring cylinder of 1lt
3) Pipette of 10ml
4) Bucket Raw water of 20-25lt
50
ACIDS S/ REAGENTS REQUIRED :-
1) Coagulants – Alum / Ferric Chloride / Hydrated lime
SAMPLES TAKEN :
8 GLASS JAR BEAKERS
a) First : Blank solution ( colorless)
b) Second : 5ml of alum solution ( colorless)
c) Third : 10ml of alum solution ( colorless)
d) Fourth : 15ml of alum solution ( colorless)
e) Fifth : 20ml of alum solution ( colorless)
f) Sixth : 25ml of alum solution( colorless)
g) Seventh : 30ml of alum solution ( colorless)
h) Eight : distilled water sample mixing ( colorless)
PROCEDURE :-
1. Pour raw water up to mark in measuring cylinder and pass in to all beakers
2. Here we use alum is the main coagulant to determine the coagulant dosage
3. To get Alum / Ferric Chloride / Hydrated lime solution by adding 1 gm of
Alum / Ferric Chloride / Hydrated lime in 1 liter of distilled water
4. Adding 5ml of solution is pipetted in to first beakers and add 5ml increment
of each subsequent beakers
5. Place each beaker on platform of jar test
6. Load the pedals and locked them in position which is submerge in to
solution
7. Stir the sample by rotating speed control from 100-120rpm for 1-2minutes
and reduce speed to 20rpm and free for 20minutes
8. Observe the extent of removal of turbidity in all beakers by putting tube light
51
TABULATION :-
Volume of sample = 1 liter
Beaker
No
Coagulant
dosage ml
Floc
formation
designation
Color Turbidity pH Akalinity
Blank -
1 5
2 10
3 15
4 20
5 25
6 30
END POINT :-
RESULT :-
Optimum coagulant dosage = -------- ml
52
Exp No 8
DETERMINATION
OF
RESIDUAL CHLORINE
AND
AVAILABLE CHLORINE
IN BLEACHING POWDER
53
Exp No 8 DETERMINATION OF RESIDUAL CHLORINE NAD
AVAILABLE CHLORINE IN BLEACHING POWDER
AIM :-
To determine the residual chlorine and available chlorine in bleaching powder
sample
PRINCIPLE :-
It is done by determining chlorine content in water sample to find disinfection.
It is called chlorination . It is 0.1-0.2ppm of residual chlorine at consumers end
ACIDS / REAGENTS REQUIRED :-
1. Bleaching powder
2. Sodium thiosulphate solution
3. Potassium iodide
4. Starch Indicator
GLASSWARES REQUIRED :-
1) Burette
2) Pipette
3) Conical flask
4) Beaker
5) Measuring cylinder
54
SAMPLES TAKEN :
Beaker = dark blue solution
a) Bleaching powder solution ( colorless)
b) Pottasium iodide ( yellowish colour )
c) Starch indicator ( black colour )
Burette = sodium thiosulphate solution ( colorless )
Final = colourless solution
PROCEDURE :
1. Weigh a 1gm of bleaching powder in paper in weighing balance
2. Add make this in to powder form by mortaring it until it gets fine powder
3. Take 100ml of distilled water in measuring cylinder and transfer in to beaker
4. Add another 100ml of distilled water in measuring cylinder again add it in to
beaker
5. Now , Prepared bleaching powder mix is transferred in to beaker by mixing
it thoroughly and shake well
6. Take 25ml of this sample is in conical flask and add 2ml of acetic acid in it
7. Add pinch of potassium iodide crystal powder in that solution , add 2 drops
of starch solution in it
8. Take sodium thiosulphate solution in burette
9. This is titrated with flask solution until colour changes to colourless
10.The mark of the place which denotes the residual chlorine content in
bleaching powder
55
TABULATION :-
Volume = 200ml
S.No Initial reading Final reading Ml of sodium
thiosulphate added
CALCULATION :-
Residual chlorine = V1*N*34540/V2 = -------- mg/lt
V1 – volume of sodium thiosulphate used
V2 – volume of sample
N – Normality of sodium thiosulphate – 1/100
RESULT :-
Chlorine content = ------ mg/lt
56
Exp No 9
DETERMINATION
OF
OIL AND GREASE
57
Exp No 9 DETERMINATION OF OIL AND GREASE
AIM :-
To determine the oil and grease content in water sample by partition
gravimetric method
APPARATUS REQUIRED :-
1. Sulfuric acid
2. Ethyl alcohol
3. Petroleum ether
GLASSWARES REQUIRED :-
1. Volumetric flask
2. Conical flask
3. Pipette
ACIDS/ REAGENTS REQUIRED :
a) H2SO4
b) Petroleum ether
c) Ethyl alchohol
SAMPLE TAKEN :
Burette = Petroleum ether
Beaker = Dirty colourless ( water + petroleum ether )
Final = Swelly colourless solution
PROCEDURE :-
1. Add 250ml of the water sample in beaker
2. This is added to petroleum ether in beaker in two layers of about 200ml in
beaker
3. This will form in 2 layers after the settling of about 1hour
58
4. The water is discard in bottom of from funnel and petroleum ether on top is
drained through filter paper
5. It is poured in to filter paper to ensure no oil and grease stuck in paper
6. The conical flask is placed in hot bath and allows petroleum ether to
evaporate and allowed to cool
7. Add 10ml of sulfuric acid , 50ml of petroleum ether , 3ml of ethyl alcohol
are added to sample prepared and well shake
END POINT :-
TABULATION :-
Volume = 250ml
SAMPLE
NO
Volume of Ether
added
Volume of sample
after hot bath
Volume of Ethyl
alcohol
59
CALCULATION :-
Oil content = { 1000 * (Wa-Wb) } / V
Where Wa- weight of conical flask and reside after hot bath
Wb- Weight of sample conical flask after hot bath
V- Volume of sample – 250ml
RESULT :-
Oil and grease content = -------- mg/lt
60
EXP no 10
DETERMINATION
OF
SUSPENDED ,
SETTLEABLE ,
VOLATILE AND FIXED
SOLIDS
61
Exp no 10 DETERMINATION OF SUSPENDED , SETTLEABLE ,
VOLATILE AND FIXED SOLIDS
AIM :-
To determine the suspended , settleable , volatile and fixed solids in given
water sample
PRINCIPLE :-
Generally water contains solids and impurities . The given water sample also
contains suspended , settleable , volatile , fixed solids .
APPARATUS REQUIRED :-
1. Hot Air Oven
2. Weighing Balance
GLASSWARES REQUIRED :-
1) Imhoff cone
2) China dish
62
PROCEDURE :-
A)Total solids :-
1. Ignite the evaporating dish in muffle furnace for 30minutes at 550C and cool
in dessicator
2. Note down the empty weight of dish (W1)
3. Pour a measured portion of 50-100ml in to dish and contents by placing dish
to oven
4. Transfer the dish to oven maintained a 103-105ᵒC and dry it for 1 hour
5. Allow dish to cool briefly in air before placing it , while still warm in
dessiccator to complete in dry atmosphere
6. Weigh the dish , it has completely cooled (W2)
7. Weigh of residue = W2-W1 in mg
B)Total Fixed solids :-
1. Keep the dish used for determining the total residue in muffle furnace for 1
hour at 550C
2. Allow the dish to partially cool in air until the most of heat has been
dissipated
3. Weight dish as soon as it has cooled W3
4. Weigh of total fixed residue = W3-W1 in mg
C)Total Dissolved solids :-
1. Filter a measured portion of mixed sample of 50-100ml through filter paper
2. Repeat he steps from 3-6 in total solids
3. Weight of dissolved solids = W5-W4 mg
Where W4- weight of empty evaporating dish
W5- weight of empty dish + residue left after evaporating the filtrate in mg
D)Total suspended solids :-
1.Total solids – Total dissolved solids
E)Total volatile solids :-
1.Total solids – Total fixed solids
63
F)Fixed dissolved solids
1. Keep the evaporating dish used in determining TDS in muffle furnace for 1
hour at 550C
2. Repeat the 2-3 in total fixed solids
3. Weight of fixed dissolved solids = W6-W4 in mg
Where W6-weight of empty evaporating dish + fixed solids left after ignition
G)Volatile dissolved solids
1. Total fixed solids – TDS
H)Fixed suspended solids
1. Total fixed solids – Volatile dissolved solids
I)Volatile suspended solids
1.Total volatile solids – Volatile dissolved solids
J) Settleable solids
1.Fill imhoff cone to 1lt with thoroughly mixed sample and settle for
45minutes
2. Gently stir the sides of cone with rod
3. Settle for 15minues
64
TABULATION :-
Item Sample 1 Sample 2
Volume of sample
Weight of empty evaporating dish W1
Weight of dish + total solids W2
Total solids W2-W1
Weight of dish + fixed solids W3
Fixed solids W3-W1
Weight of empty evaporating dish W4
Weigh of dish + total dissolved solids
W5
Total dissolved solids W5-W4
Weight of dish + fixed dissolved
solids W6
Fixed dissolved solids W6-W4
Total solids
Fixed solids
Dissolved solids
Suspended solids
Volatile solids
RESULT :-
i) Suspended solids =------- m/l
ii) Settleable solids = -------m/l
iii) Volatile solids = ------ m/l
iv) Fixed solids = ------- m/l
65
EXP No 11
DETERMINATION
OF
DISSOLVED OXYGEN
AND
BOD OF THE GIVEN
SAMPLE
66
11.a) DETEMINATION OF DISSOLVED OXYGEN :-
AIM :-
To determine the DO for the given water sample by winkler’s method
APPARATUS REQUIRED :-
1. DO meter or potentiometer with electrodes which is silver anode and gold
cathode
GLASSWARES REQUIRED :-
1) Burette
2) Pipette
3) Conical flask
ACIDS / REAGENTS REQUIRED :-
1. Distilled water
2. Sodium sulphate
3. Potassium chloride
4. Starch ,
5. Conc sulphuric acid
67
SAMPLES TAKEN :
Beaker = NaSO4 ( Colorless)
KCl ( yellow colour )
Starch indicator ( thick blue )
Conc Sulphuric acid ( colorless )
Final =
PROCEDURE :-
1. Add KCl in electrolyte cell and slowly insert the electrode and wipe it
cleanly
2. Put cell in sodium sulphate solution
3. Switch ON the meter by allowing it to stand in warm up condition
4. Temperature is also controlled at same time by temperature probe
5. Adjust the reading to 0
6. Take out cell and clean with distilled water
7. Dip the probe in solution and stirred it gently until correct reading observes .
Note down the reading
OBSERVATION :-
Sample details = tap water
Instrument used = potentiometer
DO observed i) at initial stage = ------- mg/lt
ii) At 5 days = -------mg/lt
RESULT :-
DO )1= ---------mg/lt
DO)5 = -------- mg/lt
68
11.b)DETERMINATION OF BOD
AIM :-
To determine the BOD for given sample by inhibited BOD test
PRINCIPLE :-
BOD is briefly called as Biochemically Oxygen Demand .. The amount of
dissolved oxygen that bacteria need for consumption of organic matter in a sample.
It can be neither CBOD (Carbonaceous BOD ) or NBOD (Nitrogenous BOD) .
Criteria Need :-
A) It must be free from chlorine
B) pH range from 6.5-7.5
C) Adequate microbial population
APPARATUS REQUIRED :-
1. Incubator
69
GLASSWARES REQUIRED :-
1. BOD Bottle
2. Burette
3. Pipette
4. Flask
ACIDS / REAGENTS REQUIRED :-
1. 2 chloro 6 Trichloromethyl Pyridine
PROCEDURE :-
1. Add 2 chloro 6 Trichloromethyl Pyridine at final concentration of 10mg/lt
for nitrification inhibition . It has been that chemical does not suppress the
organic matter oxidation
2. First we have to collect the water sample
3. First of all about , we have already determining the amount of DO in 11.a) ,
to determine the BOD at each day . i.e BOD at first day is (BOD)1
4. Here we have usually to find BOD of the given sample at more of 5 days
(BOD)5
5. Organic matter + micro organism + nutrients - CO2 + H2O + micro
organisms
6. BOD (mg/lt) = (DO)1 – (DO)5
70
TABULATION :-
Day Volume of
sample
(ml)
Initial
burette
reading
Final
burette
reading
Volume of
titrant used
sodium
thiosulphate
(ml)
DO(mg/lt)
CALCULATION :-
DO)1 = ---------mg/lt
DO)5 = ----------mg/lt
BOD = DO)1 – DO)5 = ---- mg/lt
71
GRAPH :-
Nitrogen BOD
BOD5 carbon BOD
BOD
0 5 10 15
Incubation days
RESULT :-
BOD for given water sample = ------ mg/lt
72
Exp No 12
DETERMINATION
OF
COD FOR
GIVEN WATER SAMPLE
73
Exp No 12 DETERMINATION OF COD FOR GIVEN WATER SAMPLE
AIM :-
To determine the COD for given water sample
PRINCIPLE :-
COD is briefly known as Chemically Oxygen Demand . It is defined as
amount of oxygen need to oxidize the organic carbon completely to CO2 , H2O
and ammonia . It requires rapid test of 2-4hours
GLASSWARES REQUIRED :-
1. Burette
2. 2 Pipettes of 250ml
3. Flask
4. weighing bottle
APPARATUS REQUIRED :-
1. Incubator
74
ACIDS / REAGENTS REQUIRED :-
1. FAS (ferrous ammonium sulphate ) salt
2. Potassium dichromate
3. 1:1 sulphuric acid
4. Dilute sulphuric acid
5. Ferrion indicator
SAMPLES TAKEN
Beaker
a) FAS ( whitish blue solution )
b) Dil H2SO4 ( colorless )
c) K2CR2O7 ( yellow colour )
d) Ferroin indicator ( green colour )
Burette – distilled water ( colorless )
Final = Reddish brown solution
PROCEDURE:-
1. Fill the weighing bottle with FAS salt as W1
2. This is transferred in to flask and take the empty weighing bottle as W2
3. W1-W2 = we get the weight of the salt
4. We have to add half of the test tube is filled with dilute sulphuric acid and
added to flask solution and shake well
5. First , we have to fill burette with distilled water
6. Then add distilled water up to neck of flask and its remaining portion will
be titrated with distilled water solution from burette to flask mark , mix
them in 5-6 minutes , which is colourless
7. The water in burette is washed out and add prepared FAS solution in it
8. Take another flask and 25ml of water sample is pipette in to it and
transferred in to flask’
9. Take 25ml of potassium dichromate solution by pipette it in to flask which
is yellow colour
75
10.Add 1;1 sulphuric acid in this prepared solution and add also 3 drops of
ferrine indicator
11.This solution is mixed will until it gets turns from yellow to green colour
12. Now this solution is totally titrated with burette FAS solution until the
green colour to reddish brown colour
13.Now we prepare the solution only for given sample . It is called as back
titration
14.But , we have also calculate the blank titration without using water sample
by repeating steps 6-12 except that no distilled water can be added
END POINT :-
76
TABULATION :-
S.No Initial burette
reading
Final burette
reading
Volume of FAS
solution
1
2
3
GRAPH :-
800
600
400
200
0.1 0.2 0.3
77
CALCULATION :-
a) NORMALITY , N= ( Weight of FAS *4 ) / Equivalent weight of
b) COD of given sample = ( 10*(V1-V2)*N* 8*1000 ) / Vs
Where 8 – constant
N – Normality
Vs- Volume of sample
RESULT :-
COD = ------ mg/lt
78
EXP No 13
DETERMINATION
OF
SVI OF
BIOLOGICAL SLUDGE
AND
MICROSCOPIC
EXAMINATION
79
Exp No 13 DETERMINATION OF SVI OF BIOLOGICAL SLUDGE AND
MICROSCOPIC EXAMINATION
AIM :-
To determine the SVI of biological sludge by microbiological examination
PRINCIPLE :-
SVI is the sludge volume index . It is the indicator of sludge settleability
between the water content between flocs and SVI . It is the measure of activated
sludge to separate from mixed liquor in order to achieve adequate sludge recycle
and final efficient with low suspended solids concentration . It is defined as
volume occupied by 1 g of sludge after 30minutes settling in a 1liter unstirred
cylinder
GLASSWARES REQUIRED :-
1. Burette
2. Pipette
3. Conical flask
4. Gradual water sample of volume 1 liter
5. Stirrer for SSVI test
6. Sludge sample
PROCEDURE :-
1. Measure the concentration of sludge sample with TSS test
2. Fill 1Liter of gradual cylinder with sludge sample and allow sample to settle
3. But it is not easy to settle
4. So we have to add supernatent liquid to settle it quickly
5. After 30 minutes of settling , read the volume occupied by sludge from
graduated cylinder (SV30 in ml )
6. Calculate the SVI from relation with Xrss being measured sample
concentration in gL-1
80
TABULATION :-
S.No Volume of sludge
(V1)
Volume of sludge
(V2)
Total volume (V)
(Xrss)
1
2
3
CALCULATION :-
SSVI = SVss / Xrss = ---- ml g-1
Where Xrss - concentration of sludge sample – V2-V1
SVss - volume of sludge occupied by cylinder
81
END POINT :-
RESULT :-
SVI = --------- ml g-1
82
Exp No 14
DETERMINATION
OF
MPN INDEX
OF THE
GIVEN SAMPLE
83
Exp No 14 DETERMINATION OF MPN INDEX OF THE GIVEN SAMPLE
AIM :-
To Determine the MPN index of the given sample
PRINCIPLE :-
MPN is briefly known as Most Probable Number . It is the index used to
estimate the concentration of viable microorganisms in a sample by means of
replicable liquid broth growth in tenfold dilutions . It is most commonly applied
for quality testing of water sample . That is the whether the water is safe or not . It
is mainly tested for coli-forms bacteria present in water
GLASSWARES REQUIRED :-
1. Burette
2. Pipette
3. 12 Test tubes
4. 3 Lactose broth test tubes
PROCEDURE :-
1. Take drinking water sample
2. This is accounts in to 3 samples of 12 lactose broth test tubes
3. Take 10ml of water sample and passed in to each broths in 1st
sample
4. Take 1ml of same sample in to each broths in 2nd
sample
5. Take 0.1ml of same in to each broths in 3rd
sample
6. All these samples are kept in incubator at 37ᵒC for 1 day
7. After this , these can be colour changes from colourless to dirty state , but
not bin all broths , in 1 or 2 broths of sample definitely
8. We have see the number of broths which have colour changes to dirty , for
example , In first sample , only 4 broths have colour changed and in 2nd
, 3
are coloured and 3rd
1 is changed
9. From this results , By consult reference table pattern of most probable
number for this sample is 4:3:1 ( for eg ) ., MPN value = 33 /ml
84
TABULATION :-
85
END POINT :-
RESULT :-
MPN = -------- /ml
86
VIVA VOCE QUESTIONS
87
1A)DETERMINATION OF pH
1. Define pH ?
pH is the measure of alkalinity and acidity of the water sample by
concentration of H+ ions in solution
2. Define the full form of pH ?
pH means potential of Hydrogen ions
3. What are methods available for determining pH ?
a) Indicator method , b) Electrode method , c)pH meter , d) pocket pH
meter
4. What are conditions needed for test sample ?
It depends upon type of pH sensor , holder material , room temperature
5. Which solution is immersed inside the solution of pH glass electrode ?
AgCl , where Ag acts as cation and Cl acts as anion
6. What is permissible limit of pH in water ?
6.5-7.5 for potable water
7.What is the unit of pH ?
It has no unit
1B) DETERMINATION OF TURBIDITY
1. Define Turbidity ?
Turbidity is measure of cloudiness and haziness f water caused by large
number of individual particles that are generally invisible to naked eye
2. What are methods available to determining turbidity ?
Nepheleometric Turbidity meter , Jackson Candle Turbidity Meter ,
Bayli Turbidimeter , turbidity rod
3. What is the unit of Turbidity ?
If nepheleometric turbidity meter is used , it is as NTU while jackson
turbidity candle turbidity meter is used , it is used as JTU
4. What are causes for turbdity ?
It is caused by suspended particles dissolved in water that scatter light
making the water appear cloudy or milky
5. The material which is sued for determination of nepheleomteirc
turbidity meter ?
Silica
88
6. What is light source for nepheleomtric turbidity meter ?
Tungsten Vapour lamp
7. What is limit of turbidity in water ?
5-10 NTU
1C)DETERMINATION OF CONDUCTIVITY
1. Define conductivity ?
It is defined as the ability of conducting heat , electricity . When an
electrical potential difference is created across a conductor , its ions starts
flow , giving rise to an electric current
2. What is unit for conductivity of water ?
μmho/cm or siemen . It is reciprocal of resistivity of sample .
3. What is conductivity of standard KCl solution is ?
1412 μmho/cm
4. Which water has more conductivity?
Sea water . because it contains more salt contains chloride cntent , it
leads to high conductivity
5. What is limit of conductivity in water ?
50-1500 μmho/cm
6. How will you determine the conductivity of sample ?
Conductivity = Conductance * cell constant (K)
7. How to find TDS of conductivity ?
TDS = o.64 * electrical conductivity
2 DETERMINATION OF HARDNESS
1. Define hardness ?
It is defined as property of water which prevents the formation of lather
with soap
2. What are types of hardness ?
a) Carbonate hardness
b) Non Carbonate hardness
3. Which method is used to find hardness of water ?
EDTA method – Ethylene Di-amine Tetra Acetic acid
4. Which is used as indicator of determining hardness ?
Eriochrome Black T
89
5. Which colour is obtained at end point ?
Wine red to Deep blue
6. What is the hazard value of hardness in water sample ?
>180mg/lt
7. Define total hardness ?
It is defined as equivalent of calcium and magnesium ions hardness
3A) DETERMINATION OF ALKALINITY
1. Define alkalinity ?
It is defined as the capacity of water a way of measuring acid neutralizing
. To maintain relative constant pH
2. What are types of alkalinity ?
a) Carbonate alkalinity
b) Bicarbonate alkalinity
c) Hydroxide alkalinity
3. What is the colour of phenolphthalein and methyl orange indicator ?
Lavender , Deep Orange
4. Which colour defines the end point of the water sample in hardness
determination ?
Pale yellow
5. Which equivalent is used as Hardness ?
CaCO3
6. Which solution is used as titrant ?
N/50 standard sulphuric acid
7. What is the limit of total alkalinity in water sample ?
20-200mg/lt
3B) DETERMINATION OF ACIDITY
1. Define Acidity ?
It is defined as property that has state of acid
2. What are types of Acidity ?
a)Total acidity b) Mineral acidity
3. Which instrument can be used for determination of acidity ?
Spectrometer
90
4. What is pH of phenolphthalein acidity and methyl orange acidity?
8.3 , 3.7
5. Which solution is used as titrant ?
Standard NaOH
6.What is limit of acidity in water sample ?
0-50mg/lt
4)DETERMINATION OF CHLORIDE
1.What is role of chloride in water ?
Chloride is the one of the inorganic matter in water sample . The chloride
content in raw water is slight highly .
2.Which method is used to determine the chloride content ?
It can be determined by Mohr’s method
3.What is normality of AgNO3 solution ?
0.014
4.What is equivalent value of chlorides in water ?
35.5
5.What is indicator of the chloride content ?
Red brown
6.Which solution is used as indicator ?
AgNO3 , K2CRO4
7.What is limit of chlorides in water sample ?
<250mg/lt
5A) DETERMINATION OF PHOSPHATES
1. Which method is used to determine the phosphates in water ?
Stannous chloride method
2. What are reagents used in determining phosphates ?
Ammonium Molybdate , Stannous chloride
91
3. Which instrument is used to determine the phosphates in water ?
Spectrophotometer
4. What is end point of the determining phosphates in water sample ?
Blue colour solution
5. Which is used as titrant ?
Ammonium Molybdate
6. What is limit of phosphates in water sample ?
0.1mg/lt
7. What is the name of holder ?
Cuvette
5.B)DETERMINATION OF SULPHATES
1. Which method is used as sulphates determination ?
Gravimetric method
2. What are reagents used in this determination ?
BaCl , MgSO4
3. Which is used as titrant ?
BaCl
4. What is end point of this experiment ?
Colourless
5. What is limit of sulphates in water sample ?
1000mg/lt
6A)DETERMINATION OF IRON
1. What is role of iron in water ?
Iron is only toxic at very high concentrations , it acts as a useful
surrogate for other heavy metals
2. What are reagents used in this experiment ?
Hydroxyammonium chloride , Phenanthroline
3. Which solution is used as titrant ?
NaOH
4. What is end point of this solution ?
Brownish orange colour
5. What is limit of iron in water sample ?
0.03mg/lt
92
6B)DETERMINATION OF FLUORIDES
1. Which method used to determine the fluoride content in water sample ?
Spands method
2. What are reagents used in this experiment ?
Spands Tri-sodium salt solution , Zinconyl acid reagent , sodium
arsenite solution ,
3. Which solution is used as titrant ?
Standard Spands solution
4. What is end point of this experiment ?
Pure Blood red colour
5. What is limit of fluorides in water sample ?
0.05mg/lt
7)DETERMINATION OF OPTIMUM COAGULANT DOSAGE
1. Which method is used to determine the coagulant dosage ?
Jar test
2. Which is mostly used as Coagulant ?
Alum (Al2SO4)3 . 18H2O
3.What is speed rate of pedals for mixing ?
20-120 revolutions
4.What is limit of coagulant dosage ?
10-15ml
5.Why coagulants are used ?
Raw water contains some suspended impurities . Some of these can be
removed by sedimentation and some of them cannot be easily removed . So we
have do the coagulation process . Optimum dose of coagulant is the minimum dose
of the coagulant that will be remove the maximum turbidity in water
93
8)DETERMINATION OF CHLORINE
1. Define chlorination ?
It is done by determining chlorine content in water sample to find
disinfection. It is called chlorination .
2. What are reagents used in water sample ?
KI , starch indicator
3. Which solution is used as titrant ?
Sodium Thiosulphate
4. What is limit of residual chlorine?
0.1-0.2ppm of residual chlorine at consumers end
5. Define residual chlorine ?
It is low amount of chlorine remaining in water after a certain period
after its initial precipitation
6.What are methods used to determine the chlorine in water ?
a) Starch iodide test , b) DPD test , c)Residual chlorine kit
7. What is end point of this experiment ?
From yellow to blue , till Disappearance of blue colour
9)DETERMINATION OF OIL AND GREASE
1.Which method is used to measure Oil and Grease ?
Partially Gravimetric method
2.What are reagents used in this experiment ?
Sulfuric acid
Ethyl alcohol
Petroleum ether
5. What is limit of oil and grease in water sample ?
75-100mg/lt
94
10)DETERMINATION OF SETTLEABLE , SUSPENDED ,
VOLATILE AND FIXED SOLIDS
1. Define Settleable solids ?
It refers to any material that will not remain suspended or dissolved in
water tank excludes TDS and TSS
5. Define suspended solids ?
It refers to small solid particles remain in suspension in water as a
colloidal or due to motion of water
6. Define volatile solids ?
It refers to substance that can easily transform from its solid state in to
vapour state without goes to liquid state
7. Define fixed solids ?
It refers to summation of dissolved solids and suspended solids
8. What is limit of solids in water ?
500mg/lt
11)DETERMINATION OF DO AND BOD OF THE GIVEN SAMPLE
1. Define dissolved oxygen ?
It is defined as measure of how much oxygen is dissolved in water
2. Define BOD ?
BOD is briefly called as Biochemically Oxygen Demand .. The amount
of dissolved oxygen that bacteria need for consumption of organic matter in a
sample. It can be neither CBOD (Carbonaceous) or NBOD (Nitrogenous)
3. Which instrument used for this experiment ?
Potentiometer
4. What is limit of BOD in water sample ?
<8mg/lt
95
12)DETERMINATION OF COD OF THE GIVEN SAMPLE
1. Define COD ?
COD is briefly known as Chemically Oxygen Demand . It is defined as
amount of oxygen need to oxidize the organic carbon completely to CO2 , H2O
and ammonia
2.What are reagents used in this experiment ?
FAS (ferrous ammonium sulphate ) salt , potassium dichromate , ferrine
indicator
3.Why here we need blank titration ?
It is needed when all chemicals are working based on suitable places , so we
have to deduct this water sample . This is called blank titration
4.What is end point of this experiment ?
Brick Brown colour
5.What is limit of COD in this water sample ?
500-1500mg/lt
13.DETERMINATION OF SVI OF BILOGICAL SLUDGE AND
MICROSCOPIC EXAMINATION
1. Define SVI ?
SVI means Sludge Volume Index is defined as settling characteristics of
sludge in aeration tank in activated sludge process
2.Define Activated sludge ?
It is thick soft substance used for removing pollutants from waste water
by a biological reaction that involves oxygen
3.What is limit of SVI in waste water sample ?
50-150ml/g
96
14)DETERMINATION OF MPN INDEX FOR GIVEN WATER SAMPLE
1.Define MPN ?
MPN is briefly known as Most Probable Number . It is the index used to
estimate the concentration of viable microorganisms in a sample by means of
replicable liquid broth growth in tenfold dilutions
2. What is limit of MPN index
200MPN/100ml
<<<<<<<<<<<<<<<<<<<<<<<<<THE END>>>>>>>>>>>>>>>>>>>>>>>>>>
97
CONCLUSION
COURSE OUTCOMES
1.The students will have the required knowledge in the area of testing of both
drinking water and waste water components of experiments experimentally

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CE8512-WATER AND WASTE WATER ANALYSIS LABORATORY.pdf

  • 1. LABORATORY MANUAL Mr. SATHISHKUMAR A.S Mr. VETRISUBAM Prepared By WATER AND WASTE WATER ANALYSIS LABORATORY LAB MANUAL Academic Year : 2022 - 2023 Subject Code : CE8512 Regulations : R21 Class : V Semester (CE) DEPARTMENT OF CIVIL ENGINEERING SBM COLLEGE OF ENGINEERING AND TECHNOLOGY SBM Nagar, Thamaraipadi, Dindigul - 624 005 Registration Number : ____________________________________ Name of the Student : ____________________________________ Assistant Professor Assistant Professor
  • 2. 2 CE8512 - WATER AND WASTE WATER ANALYSIS LABORATORY LIST OF EXPERIMENTS 1.Determination of pH , Turbidity , Conductivity 2.Determination of Hardness 3.Determination of Alkalinity and Acidity 4. Determination of Chlorides 5.Determination of Phosphates and Sulphates 6.Determination of Iron and Fluoride 7.Determination of Optimum Coagulant dosage 8.Determination of residual chlorine and available chlorine in bleaching powder 9.Determination of oil and Grease 10.Determination of suspended , settleable , volatile and fixed solids 11.Determination of Dissolved oxygen and BOD for given sample 12.Determination of COD for given sample 13.Determination of SVI of biological sludge and microscopic examination 14.Determination of MPN index of given sample .
  • 3. 3 CONTENTS S.No Experiments Name Pg No 1 Determination of pH , Turbidity , Conductivity a) Ph 6 b) Turbidity 9 c) Conductivity 12 2 Determination of Hardness 16 3 Determination of Alkalinity and Acidity a) Alkalinity 20 b) Acidity 23 4 Determination of Chlorides 27 5 Determination of Phosphates and Sulphates a) Phosphates 31 b) Sulphates 36 6 Determination of Iron and Fluoride a) Iron 40 b) Fluoride 44
  • 4. 4 7 Determination of Optimum Coagulant dosage 49 8 Determination of residual chlorine and available chlorine in bleaching powder 53 9 Determination of oil and Grease 57 10 Determination of suspended , settleable , volatile and fixed solids 61 11 Determination of Dissolved oxygen and BOD for given sample a) DO 66 b) BOD 68 12 Determination of COD for given sample 73 13 Determination of SVI of biological sludge and microscopic examination 79 14 Determination of MPN index of given sample 83 VIVA VOCE QUESTIONS 87 CONCLUSION 97
  • 5. 5 EXP NO 1 DETERMINATION of pH, TURBIDITY AND CONDUCTIVITY
  • 6. 6 1.a) DETERMINATION OF pH :- AIM :- To determine the pH of the given waste water sample. APPARATUS REQUIRED 1. pH meter with pH electrodes. 2. Thermometer. ACIDS / REAGENTS REQUIRED 1. Buffer solution. 2. pH tablets no = 4, 7, 10
  • 7. 7 SAMPLES TAKEN : 2 Beakers a) first = pH buffer tablet no 4 ( colorless ) b) second = pH buffer tablet no 7 ( colorless ) PROCEDURE:- 1. Calibrate the electrodes with two standard buffer solution of pH 4 and 9 buffer solution. It is a solution offering resistances. 2. The sample temperature is determined at the same time and is entered into the meter to allow for a temperature correction. 3. Raise the electrodes thoroughly mix it with ionized distilled water and carefully wipe it with a tissue paper. 4. Dip the electrode into the sample solution wait upto 1 min for steady reading the pH meter reading within ±0.1 pH unit will be adequate for such work. 5. The reading is taken and the indicator value remains constant for about 9 minutes pH= log10 [ 𝟏 𝑯+ ]
  • 8. 8 TABULATION :- Description of sample Temperature Ph Blank 4.0 7.0 END POINT :- RESULT The pH value of the given waste water sample is ____________
  • 9. 9 1b. DETERMINATION OF TURBIDITY :- AIM :- To determine the turbidity of the given sample of waste water using nephelometric turbidity meter.(20NTU) PRINCIPLE :- Nephelo turbidity meter operator on the principle of light passing through a substance of light passing. In this a strong light beam is passing upward APPARATUS REQUIRED 1. Nepheolo turbidity water meter GLASSWARE REQUIRED :-  Cuvette  Measuring Cylinder  Beaker  Rinser
  • 10. 10 ACIDS / REAGENTS REQUIRED :-  H2SO4 ( colorless ) SAMPLES TAKEN : Beaker :- H2SO4 ( Colorless ) PROCEDURE: 1. Switch ON the instrument and let the instrument warm for 15-20 minutes. 2. Insert the cell with distilled water into the cell holder. Cover the cell with light shield. 3. Select the sang [ 1-100 NTU] as yield by range on panel meter with the help of “Set Zero” control knobs. 4. Select the range for use insert the all with standards solution [20 NTU] cell holder. Adjust standardized control to set to 20 on the panel. 5. Insert cell rider in 100 NTU range and adjust to panel meter. 6. Repeat step 3 and 4 till you get zero and standard control. 7. Now insert all the sample solution and note the reading. 8. The meter scale is marked from 0-100 for NTU range read 100 as 20 NTU. (A). In 100 NTU range inserts cell riser first, insert the cell will distilled water and adjust to zero. (B). Always adjust zero in highest sensitivity to set better adjustment. H2SO4  H2 + SO4
  • 11. 11 TABULATION :- Sample Range selected Turbidity NTU END POINT :- RESULT :- Turbidity of given sample ________________ NTU
  • 12. 12 1.c) DETERMINATION OF ELECTRICAL CONDUCTIVITY :- AIM :- To determine the electrical conductivity of given water sample PRINCIPLE :- Electrical conductivity of water is the ability to conduct an electric current . Salts and other chemicals that dissolve in water can break down in to positively and negatively charged ions . It depends upon the concentration of the ions. Conductivity is the reciprocal of resistance . Its unit is μmho/cm G= k (A/L) Where k is the conductivity or specific conductance APPARATUS REQUIRED :- 1. Conductivity meter with conductivity cell
  • 13. 13 GLASSWARES REQUIRED :-  Beaker  Rinser  Measuring Cylinder ACIDS / REAGENTS REQUIRED :-  KCl ( colorless ) SAMPLES TAKEN :  Beaker – KCl ( colorless solution ) PRINCIPLE :- 1.Calibarte the conductivity meter as per the directions were given by the manufacturer’s manual using standard solutions 2. Rinse the cell with the sample , measure the sample resistance or conductivity PROCEDURE :-  Take 50ml of water sample  Add 2g of KCl in it and mix properly  Switch ON the conductivity meter and warm it in for 5minutes  Keep the Calibration control as it by constant it will shows green light  Set the temperature at 27°C  Turn it in to Calibration control again it will shows red light  Rinse the electrode in prepared KCl solution and note down the proper reading KCl  K+ + Cl-
  • 14. 14 TABULATION :- Sample details Conductivity measured corrected CALCULATION :- Conductivity of cell = Measured value * cell constant * Correction factor = ------ μmho/cm Where , Cell constant – 1.02 Correction factor – 1.05 RESULT :- Electrical conductivity of the water = -------- μmhos/cm
  • 16. 16 Exp No 2 DETERMINATION OF HARDNESS AIM :- To determine the total hardness of water PRINCIPLE:- Hardness in water is that characteristics which prevents the formation of sufficient foam or lather when such hard waters are mixed with soap . It is usually caused by presence of Ca and Mg salts present in water , which forms scum by reaction with soap . Bicarbonates and carbonates of Ca and Mg ions are called temporary while sulphates , nitrates , chlorides of Ca and Mg The total hardness of the given sample of water be easily computed by titration method by using EDTA solution either in a solution or salt . The indicator dye which is found to be serve an excellent indicator to show all hardness ions is called Eriochrome Black T having blue colour is added to water with pH of 10 ,. It combined with divalent metallic ion having wine red in colour S.No Category Hardness 1 Soft 0-75 2 Moderately Hard 75-150 3 Hard 150-300 4 Very hard >300 GLASSWARES REQUIRED :- 1. Conical flasks 2. Burette 3. Pipette 4. Beakers
  • 17. 17 ACIDS / REAGENTS REQUIRED :- 1. Standard N/50 EDTA solution (Colorless) 2. EBT indicator( Black) 3. Ammonia buffer (Colorless) SAMPLES TAKEN : Beaker = Water sample with EBT indicator added ( wine red solution ) Burette = EDTA solution ( Colorless ) Final = Solution ( Sky blue colour ) PROCEDURE:- 1. Take 100ml of water sample in conical flask 2. Add 1ml of ammonia buffer to flask 3. Add 6 drops of EBT indicator in to flask . Wine red colour will be developed 4. Titrate it with EDTA solution till the colour changes from wine red to deep blue 5. Hardness in mg/lt = 𝑚𝑙 𝑜𝑓 𝐸𝐷𝑇𝐴 𝑢𝑠𝑒𝑑∗ 𝑁 50 ∗50∗1000 𝑚𝑙 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 as CaCO3 TABULATION :- Sample No ml of water sample used in flask (2) Initial burette reading (3) Final burette reading (4) ml of N/50 EDTA used in ml (5) Hardness mg/lt CaCO3 = (5/2)*1000
  • 18. 18 END POINT :- RESULT :- Hardness of the given water sample = ------------ mg/lt
  • 20. 20 3.a) DETERMINATION OF ALKALINITY :- AIM :- To measure alkalinity by using indicators to find phenolphthalein alkalinity and total alkalinity PRINCIPLE :- Alkalinity is due to presence of salts of weak acids . It is a classified as in three forms . They are Hydroxide alkalinity , carbonate alkalinity, Bicarbonate alkalinity. Among these Bicarbonate alkalinity is major constituent . It is measure on CaCO3 scale as mg/lt of CaCO3 . APPARATUS REQUIRED :- 1. Burette 2. Conical flask 3. Measuring cylinder 4. Beakers ACIDS / REAGENTS REQUIRED :- 1. Phenolphthalein indicator ( colorless ) 2. Methyl orange indicator ( red orange ) 3. Standard N/50 sulphuric acid ( colorless ) SAMPLES TAKEN :- 2Beakers a) 1st = Phenolphthalien with water sample ( light pink ) b) 2nd = methyl orange with water sample ( light orange ) Burette = H2SO4 ( Colorless ) Final a) 1st = colorless b) 2nd = light orange
  • 21. 21 PROCEDURE :- 1) Fill the burette with H2SO4 solution up to mark 2) Take 100ml of sample which is to be tested in measuring cylinder and filled in to conical flaks and note down the initial reading 3) Now 3-4 drops of Phenolphthalein in to this solution and mixed thoroughly and it turns to pink colour and titrate it with H2SO4 solution 4) Open the cock of burette with constant rate when the pink colour disappears and note down the reading as final reading as of phenolphthalein indicator 5) Then add 1 drop of methyl orange indicator in the same solution and it is titrated with H2SO4 till it gets appearance of light orange colour and note down the final reading as of methyl orange indicator 6) Repeat the procedures for 3-4 trails 7) To find the H2SO4 volume , to deduct the final reading from initial reading 8) Then find the total volume by adding both values ( phenolphthalein and methyl orange of sample TABULATION :- a)As a phenolphthalein indicator S.No Sample volume (ml) Initial reading Final reading Volume of H2SO4 used (ml) b)As a Methyl Orange indicator S.No Sample volume (ml) Initial reading Final reading Volume of H2SO4 used (ml)
  • 22. 22 END POINT OF PHENOLPTHALEIN :-  END POINT OF METHYL ORANGE :-  CALCULATIONS :- a)Phenolphthalein alkalinity = (P*1000) /( ml of sample) = ---------mg/lt b)Total alkalinity = (T*1000)/ (ml of sample ) = ----- mg/lt RESULT :- Phenolphthalein alkalinity = ----- mg/lt Total alkalinity = ------ mg/lt
  • 23. 23 3.b) DETERMINATION OF ACIDITTY :- AIM :- To measure acidity by using mineral and phenolphthalein acidity PRINCIPLE :- Acidity is the caused by CO2 and mineral acids , sulphates of iron and aluminium . It is measure on CaCO3 scale as mg/lt of CaCO3 . GLASSWARES REQUIRED : 1. Burette 2. Conical flask 3. Measuring cylinder 4. Beakers ACIDS / REAGENTS REQUIRED :- 1. Methyl orange ( red orange solution ) 2. Phenolphthalein indicator ( colorless ) 3. Standard N/50 NaOH solution (colorless) SAMPLE TAKEN : Beaker :- a) First beaker – light orange ( sample with methyl orange ) b) Second beaker – colorless ( sample with phenolpthalien ) Final = orange to pink / lavender PROCEDURE :- 1) Fill the burette with NaOH solution up to mark 2) Take 100ml of sample which is to be tested in measuring cylinder and filled in to conical flaks and note down the initial reading 3) Add 1 drop of methyl orange indicator in the same solution and it is titrated with NaOH till it gets appearance of light orange colour
  • 24. 24 4) Then add 0.5ml of Phenolphthalein in to this solution and mixed thoroughly and it is colourless 5) Note the initial reading of both indicator values 6) Now these can be titrated with NaOH solution , it turns to lavender colour . It is end point . Now it is persist for 30seconds 7) Note the final reading END POINT :-  TABULATION :- a)As a phenolphthalein indicator S.No Sample volume (ml) Initial reading Final reading Volume of NaOH used (ml)
  • 25. 25 b)As a Methyl Orange indicator S.No Sample volume (ml) Initial reading Final reading Volume of NaOH used (ml) CALCULATIONS :- a) Mineral acidity mg/lt = 𝑚𝑙 𝑜𝑓 𝑁𝑎𝑂𝐻 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 𝑢𝑠𝑒𝑑 𝑤𝑖𝑡ℎ 𝑚𝑒𝑡ℎ𝑦𝑙 𝑜𝑟𝑎𝑛𝑔𝑒 𝑚𝑙 𝑠𝑎𝑚𝑝𝑙𝑒 b) Total acidity mg/lt = 𝑚𝑙 𝑜𝑓 𝑁𝑎𝑂𝐻 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 𝑢𝑠𝑒𝑑 𝑤𝑖𝑡ℎ 𝑝ℎ𝑒𝑛𝑜𝑙𝑝ℎ𝑡ℎ𝑎𝑙𝑒𝑖𝑛 𝑚𝑙 𝑠𝑎𝑚𝑝𝑙𝑒 RESULT :- Mineral acidity = -----------mg /lt Total acidity = ---------- mg/lt
  • 27. 27 Exp NO 4 DETERMINATION OF CHLORIDES AIM :- To determine the chloride content in given water sample PRINCIPLE :- Chloride is the one of the inorganic matter in water sample . The chloride content in raw water is slight highly . So this can be determined by Mohr’s method uses silver nitrate solution with normality of 0.014 which is titrated against the standard sodium chloride solution . But the indicatr KMnO4 is added to realize the end point of this experiment AgNO3 + NaCl  NaNO3 + AgCl This AgCl is substance which is in milky white which denotes end point of this experiment . It is limited up to 250mg/lt – 600mg/lt APPARATUS REQUIRED :- 1. Beaker 2. Burette 3. Pipette ACIDS / REAGENTS REQUIRED :- 1. KMnO4 as indicator ( Dark Yellow ) 2. Silver nitrate solution ( Colorless ) 3. NaCl (Colorless) SAMPLE TAKEN : Burette = Silver nitrate ( Colorless) Beaker = Pale yellow solution ( KMnO4 + sample ) Final = Brickish red solution
  • 28. 28 PROCEDURE :- 1) Take 20ml of water sample in measuring cylinder and pour in it without air bubbles and this is transfer in to conical flask 2) Take 5ml of NaCl solution in cylinder and add this also in to flask 3) Now take silver nitrate solution in to burette up to mark 4) Now take indicator KMnO4 as in 4-5 drops in to prepared conical flask solution 5) Now flask solution is titrated with burette solution until it turns in to pale yellow colour which denotes the chloride in water sample 6) The Silver nirate reacts with potassium chromate which gives a final solution as silver chromate which is in a red brown colour TABULATION :- S.No Sample volume (ml) Initial reading Final reading Volume of AgNO3 used (ml) CALCULATION :- Chloride ion concentration (mg/lt) = (A*N*35.45*1000) / Volume of sample (V) = --------- mg/lt AgNO3 + K2CrO4  Ag2CrO4 + 2KNO3 Ag2CrO4 denotes the red brown colour
  • 29. 29 END POINT  RESULT :- Chloride content = ------- mg/lt
  • 31. 31 5.a) DETERMINATION OF PHOSPHATES :- AIM :- To Determine the phosphates content in water sample by spectrophotometer. PRINCIPLE :- Phosphates in acidic condition reacts with ammonium molybdate to form molybdophosphoric acid which is then reduced to molybdenum blue by adding stannous chloride. The intensity of the blue colored complex is measured spectrophotometrically,which is directly proportional to the concentration of phosphate present in the sample. APPARATUS REQUIRED :- 1. Spectrophotometer GLASSWARES REQUIRED :- 1) Pipettes 2) Measuring cylinder 3) Glass-rod 4) Beakers 5) Dropper.
  • 32. 32 ACIDS / REAGENTS REQUIRED :- 1. Ammonium molybdate solution 2. Stannous chloride solution 3. Standard Phosphate Solution SAMPLES TAKEN :- Beaker = Ammonium Molybdate ( creamy white / creamy green solution ) Stannous Chloride solution ( colorless ) Burette = Standard phosphate solution ( Colorless solution ) Final = Sky blue solution REAGENTS PREPARATION :- 1.Ammonium molybdate solution In 175 ml of distilled water, add 25 g of ammonium molybdate. Now add 280 ml of conc.sulphuric acid in 400 ml of distilled water and cool it. Make the volume upto 1 litres with distilled water which gives faint green solution 2. Stannous chloride solution Dissolve 2.5 g of stannous chloride in 100 ml glycerol by heating in a water bath 3. Standard Phosphate Solution Dissolve 4.388 g of anhydrous potassium hydrogen phosphate in 1000 ml distilled water. Dilute this solution to 100 times (10ml-1000ml).This solution contains 10 mg P/l (1ml = 0.01 mg P) which is used as standard phosphate solution.
  • 33. 33 PROCEDURE :- 1. Switch ON the spectrophotometer and allow 20 minutes for warm up and set 410 nm by adjusting the wavelength knob. 2. For calibration of the instrument take distilled water in the cuvette holder and place in the compartment on the light path and close the compartment. 3. Press the mode button to set transmittance mode and set 100 % T. 4. Again press the mode button to set it for absorbance to read 0.00. 5. Fill the prepared standard solutions in the cuvette holders and place in the compartment. 6. Read the colour developed on the display and note down the peak value. 7. Take 25 ml of filtered and clear sample. 8. Add 1 ml of ammonium molybdate solution and 2 drops of stannous chloride which gives faint green solution 9. Measure the blue color developed at 690 nm on a spectrophotometer using a distilled water blank with the same chemicals. 10.Note down the readings of spectrophotometer after 5 minutes but before 12 minutes of the addition of the last reagent. 11.Find out the concentration of the phosphate with the help of the standard curve. TABULATION :- S No Initial volume Final volume Volume of ammonium molybdate solution
  • 34. 34 END POINT :- MODEL GRAPH :- Display Readings Phosphate concentration in mg 
  • 35. 35 RESULT :- The amount of phosphates determined from the given sample is ________mg/l.
  • 36. 36 5.b)DETERMINATION OF SULPHATES AIM :- To determine the sulphates of the sample by spectrophotometer method APPARATUS REQUIRED :- 1)Spectrophotometer ACIDS / REAGENTS REQUIRED :- 1. Barium Chloride 2. Magnesium sulphate SAMPLES TAKEN : Beaker – a) Barium shloride solution ( colourless ) b) Magnesium sulphate solution ( colourless ) Final = Greenish Solution
  • 37. 37 PROCEDURE :- 1. Set the meter to zero and calibrate it without keeping at air passing place 2. Take Barium chloride powder is added in to magnesium sulphate sample of 10ml and mixed well which gives greenish solution BaCl2 + MgSO4  BaSO4 + MgCl2 3. Place the cuvette in holder of the meter and rotate it to stand in position 4. Press READ button for 3 seconds and count down will starts from 5 minutes 5. This resultant value is shown in spectrophotometer screen TABULATION :- Sample No Initial reading (mg/lt) Final reading (mg/lt) Volume of barium chloride used (mg/lt)
  • 38. 38 END POINT : RESULT :- Amount of sulphates = ----- mg/lt
  • 40. 40 6.a) DETERMINATION OF IRON :- AIM :- To determine the iron content in water sample by spectrophotometer method PRINCIPLE :- Iron is only toxic at very high concentrations , it acts as a useful surrogate for other heavy metals . So it is limit up to 0.3ppm APPARATUS REQUIRED :- 1. Spectrophotometer GLASSWARES REQUIRED :- 2. Volumetric flasks 3. Beakers 4. Flasks 5. Volumetric flask ACIDS / REAGENTS REQUIRED :- 1. Standard iron solution 2. Unknown solution 3. Hydroxyammonium chloride 4. Phenanthroline indicator
  • 41. 41 SAMPLES TAKEN : Pipette – Iron solution ( Green solution ) 6 Volumetric flasks a) 1st volumetric flask – blank( colorless ) b) 2nd volumetric solution – 2.5ml of iron solution ( light orange ) c) 3rd volumetric solution – 5ml of iron solution ( slight orange ) d) 4th volumetric solution – 7.5ml of iron solution ( thin orange ) e) 5th volumetric solution – 10ml of iron solution ( thickish dark orange ) Phenonthraline indicator ( thick red colour ) Beaker – Light orange solution PROCEDURE :- 1. Take 200ppm of iron solution and pipette it with 25ml 2. Add it to 500ml A grade Volumetric flask and add distilled water about of its half 3. Shake well and finalize the volume with 500ml up to mark of flask and add distilled water up to this mark 4. Shake well and intermediate iron solution of 10ppm is ready Take membrane filter unit to find dissolved iron in water sample by closing filter base with filter paper and close it tightly 5. Add sample water and connects suction pump and give such pressure by sucking out 6. Calibration standard from blank , 0.1ppm , 0.5ppm,1.0ppm,1.5ppm,2ppm iron and take each beaker for each solution 7. Pipette 50ml of sample water after filter unit 8. Add 0.5ml to prepare 0.1ppm Fe , 2.5ml to prepare 0.5ppm Fe , 5ml to prepare 1ppm Fe , 7.5ml to prepare 1.5ppm Fe , 10ml to prepare 2ppm Fe 9. Add 1+1 Hl is pipette and add 2ml to each beaker to reduce interference by organic matter 10. 1ml of hydroxyammonium chloride to each beaker and it is used as reducing agent to reduce ferric ions to ferrous ions 11.Then add 50ml distilled water to each beaker except in sample
  • 42. 42 12.Now Heat all beakers in hot plate inside fume hood to digest heat until volume reduced to 10-20ml 13.After cooling this residual volume 14.Transfer each in to 50ml A grade volumetric flask is labeled as 0.1-2ppm Fe and sample and rinse properly 15. Then take ammonium acetate and pipette it with 10ml to each flask which is used to maintain pH about 3.5 for complete complexation of ferrous ions with phenanthroline and shake it well 16.Finally add phenonthroline in each beaker of 4ml with ferrous ions to give pale orange complex 17.Add 50ml of distilled water in each flask as final volume reading and shake well Fe + 3 Phen  Fe(Phen)3 END POINT :-
  • 43. 43 MODEL GRAPH Fe abs 0 0.5 1 1.5 2 2.5 3 3.5 Concentration (ppm)  RESULT : Iron Content = ------- mg/lt
  • 44. 44 6.b)DETERMINATION OF FLUORIDE AIM :- To determine the fluoride content in given water sample by spands method ACIDS / REAGENTS REQUIRED :- 1. Spands Tri-sodium salt solution 2. Zinconyl acid reagent 3. Sodium arsenite solution GLASSWARES REQUIRED :- 1. Burette 2. Pipette 3. Conical flask
  • 45. 45 SAMPLES TAKEN : 6 Volumetric flasks a) First flask = blank ( colorless ) b) Second flask = 0.5ml of SPADNS solution ( thinnish red ) c) Third flask = 1ml of SPADNS solution ( slight thickish red ) d) Fourth solution = 1.5ml of SPADNS solution ( thickish red ) e) Fifth solution = 2ml of SPADNS solution ( normal red solution ) f) Sixth solution = 2.5ml of SPADNS solution ( blood red solution ) Pipette – zirconyl chloride solution ( colorless ) Flask – Sodium arsenite solution ( colourless ) Final = Blood red solution PROCEDURE :- a)Preparation of sample :- 1. Take Spadns tri-sodium salt of 0.3g in 500ml volumetric flask and half of the distilled water to that flask and shake well 2. It is in beetroot red colour solution and store it in a amber glass bottle protected from direct sunlight 3. To prepare Zinconyl acid reagent by adding conc .HCl and Zinconyl chloride octahydrate of 0.133g zinconyl chloride in 500ml volumetric flask and add 25ml of distilled water in it , also add 350ml conc . HCl slowly and carefully upto mark 4. It is store in a reagent glass bottle 5. Mix equal volume of both spadns solution and zinconyl acid solution 6. Sodium arsenite NaASO2 is prepared by this salt weighed of 2.5gm in volumetric flask 7. Add distilled water up to half of the flask and shake well b)Test procedure :- 1. Pipette 10ml of spadns solution and add in 250ml volumetric flask and then add 100ml distilled water 2. Take 3ml of distilled water in measuring cylinder and 7ml of Conc HCl is in it carefully and safely And add this in to standard Spadns solution
  • 46. 46 3. It is thick blood red colour 4. To find the fluoride content in this sample , add sodium fluoride of 0.2gm in 1000ml volumetric flask and add distilled water to half of flask , shake well of fluoride 10ppm by knowing blank , 0.5ppm , 1.0ppm , 1.5ppm and sample solution 5. Add 10ml of zinconyl acid + spadns solution in this each flask , shake well and add distilled water in it to half level END POINT :-
  • 47. 47 TABULATION :- Sample no Initial reading Final reading Volume of spands solution Volume of zinconyl acid solution RESULT :- Fluorides Content = -----mg/lt
  • 49. 49 Exp No 7 DETERMINATION OF OPTIMUM COAGULANT DOSAGE AIM :- To determine the optimum coagulant dosage by using jar test PRINCIPLE :- Raw water contains some suspended impurities . Some of these can be removed by sedimentation and some of them cannot be easily removed . So we have do the coagulation process . Optimum dose of coagulant is the miminum dose of the coagulant that will be remove the maximum turbidity in water by using jar test APPARATUS REQUIRED :- 1. Jar test – Having 6 pedals can be independently move up or down , electric motor operates the jar , speed control , time control , platform transparent sheet with tube light , Counter measures number of rotation GLASSWARES REQUIRED :- 1) 6 glass jars of 1lt capacity 2) Measuring cylinder of 1lt 3) Pipette of 10ml 4) Bucket Raw water of 20-25lt
  • 50. 50 ACIDS S/ REAGENTS REQUIRED :- 1) Coagulants – Alum / Ferric Chloride / Hydrated lime SAMPLES TAKEN : 8 GLASS JAR BEAKERS a) First : Blank solution ( colorless) b) Second : 5ml of alum solution ( colorless) c) Third : 10ml of alum solution ( colorless) d) Fourth : 15ml of alum solution ( colorless) e) Fifth : 20ml of alum solution ( colorless) f) Sixth : 25ml of alum solution( colorless) g) Seventh : 30ml of alum solution ( colorless) h) Eight : distilled water sample mixing ( colorless) PROCEDURE :- 1. Pour raw water up to mark in measuring cylinder and pass in to all beakers 2. Here we use alum is the main coagulant to determine the coagulant dosage 3. To get Alum / Ferric Chloride / Hydrated lime solution by adding 1 gm of Alum / Ferric Chloride / Hydrated lime in 1 liter of distilled water 4. Adding 5ml of solution is pipetted in to first beakers and add 5ml increment of each subsequent beakers 5. Place each beaker on platform of jar test 6. Load the pedals and locked them in position which is submerge in to solution 7. Stir the sample by rotating speed control from 100-120rpm for 1-2minutes and reduce speed to 20rpm and free for 20minutes 8. Observe the extent of removal of turbidity in all beakers by putting tube light
  • 51. 51 TABULATION :- Volume of sample = 1 liter Beaker No Coagulant dosage ml Floc formation designation Color Turbidity pH Akalinity Blank - 1 5 2 10 3 15 4 20 5 25 6 30 END POINT :- RESULT :- Optimum coagulant dosage = -------- ml
  • 52. 52 Exp No 8 DETERMINATION OF RESIDUAL CHLORINE AND AVAILABLE CHLORINE IN BLEACHING POWDER
  • 53. 53 Exp No 8 DETERMINATION OF RESIDUAL CHLORINE NAD AVAILABLE CHLORINE IN BLEACHING POWDER AIM :- To determine the residual chlorine and available chlorine in bleaching powder sample PRINCIPLE :- It is done by determining chlorine content in water sample to find disinfection. It is called chlorination . It is 0.1-0.2ppm of residual chlorine at consumers end ACIDS / REAGENTS REQUIRED :- 1. Bleaching powder 2. Sodium thiosulphate solution 3. Potassium iodide 4. Starch Indicator GLASSWARES REQUIRED :- 1) Burette 2) Pipette 3) Conical flask 4) Beaker 5) Measuring cylinder
  • 54. 54 SAMPLES TAKEN : Beaker = dark blue solution a) Bleaching powder solution ( colorless) b) Pottasium iodide ( yellowish colour ) c) Starch indicator ( black colour ) Burette = sodium thiosulphate solution ( colorless ) Final = colourless solution PROCEDURE : 1. Weigh a 1gm of bleaching powder in paper in weighing balance 2. Add make this in to powder form by mortaring it until it gets fine powder 3. Take 100ml of distilled water in measuring cylinder and transfer in to beaker 4. Add another 100ml of distilled water in measuring cylinder again add it in to beaker 5. Now , Prepared bleaching powder mix is transferred in to beaker by mixing it thoroughly and shake well 6. Take 25ml of this sample is in conical flask and add 2ml of acetic acid in it 7. Add pinch of potassium iodide crystal powder in that solution , add 2 drops of starch solution in it 8. Take sodium thiosulphate solution in burette 9. This is titrated with flask solution until colour changes to colourless 10.The mark of the place which denotes the residual chlorine content in bleaching powder
  • 55. 55 TABULATION :- Volume = 200ml S.No Initial reading Final reading Ml of sodium thiosulphate added CALCULATION :- Residual chlorine = V1*N*34540/V2 = -------- mg/lt V1 – volume of sodium thiosulphate used V2 – volume of sample N – Normality of sodium thiosulphate – 1/100 RESULT :- Chlorine content = ------ mg/lt
  • 57. 57 Exp No 9 DETERMINATION OF OIL AND GREASE AIM :- To determine the oil and grease content in water sample by partition gravimetric method APPARATUS REQUIRED :- 1. Sulfuric acid 2. Ethyl alcohol 3. Petroleum ether GLASSWARES REQUIRED :- 1. Volumetric flask 2. Conical flask 3. Pipette ACIDS/ REAGENTS REQUIRED : a) H2SO4 b) Petroleum ether c) Ethyl alchohol SAMPLE TAKEN : Burette = Petroleum ether Beaker = Dirty colourless ( water + petroleum ether ) Final = Swelly colourless solution PROCEDURE :- 1. Add 250ml of the water sample in beaker 2. This is added to petroleum ether in beaker in two layers of about 200ml in beaker 3. This will form in 2 layers after the settling of about 1hour
  • 58. 58 4. The water is discard in bottom of from funnel and petroleum ether on top is drained through filter paper 5. It is poured in to filter paper to ensure no oil and grease stuck in paper 6. The conical flask is placed in hot bath and allows petroleum ether to evaporate and allowed to cool 7. Add 10ml of sulfuric acid , 50ml of petroleum ether , 3ml of ethyl alcohol are added to sample prepared and well shake END POINT :- TABULATION :- Volume = 250ml SAMPLE NO Volume of Ether added Volume of sample after hot bath Volume of Ethyl alcohol
  • 59. 59 CALCULATION :- Oil content = { 1000 * (Wa-Wb) } / V Where Wa- weight of conical flask and reside after hot bath Wb- Weight of sample conical flask after hot bath V- Volume of sample – 250ml RESULT :- Oil and grease content = -------- mg/lt
  • 60. 60 EXP no 10 DETERMINATION OF SUSPENDED , SETTLEABLE , VOLATILE AND FIXED SOLIDS
  • 61. 61 Exp no 10 DETERMINATION OF SUSPENDED , SETTLEABLE , VOLATILE AND FIXED SOLIDS AIM :- To determine the suspended , settleable , volatile and fixed solids in given water sample PRINCIPLE :- Generally water contains solids and impurities . The given water sample also contains suspended , settleable , volatile , fixed solids . APPARATUS REQUIRED :- 1. Hot Air Oven 2. Weighing Balance GLASSWARES REQUIRED :- 1) Imhoff cone 2) China dish
  • 62. 62 PROCEDURE :- A)Total solids :- 1. Ignite the evaporating dish in muffle furnace for 30minutes at 550C and cool in dessicator 2. Note down the empty weight of dish (W1) 3. Pour a measured portion of 50-100ml in to dish and contents by placing dish to oven 4. Transfer the dish to oven maintained a 103-105ᵒC and dry it for 1 hour 5. Allow dish to cool briefly in air before placing it , while still warm in dessiccator to complete in dry atmosphere 6. Weigh the dish , it has completely cooled (W2) 7. Weigh of residue = W2-W1 in mg B)Total Fixed solids :- 1. Keep the dish used for determining the total residue in muffle furnace for 1 hour at 550C 2. Allow the dish to partially cool in air until the most of heat has been dissipated 3. Weight dish as soon as it has cooled W3 4. Weigh of total fixed residue = W3-W1 in mg C)Total Dissolved solids :- 1. Filter a measured portion of mixed sample of 50-100ml through filter paper 2. Repeat he steps from 3-6 in total solids 3. Weight of dissolved solids = W5-W4 mg Where W4- weight of empty evaporating dish W5- weight of empty dish + residue left after evaporating the filtrate in mg D)Total suspended solids :- 1.Total solids – Total dissolved solids E)Total volatile solids :- 1.Total solids – Total fixed solids
  • 63. 63 F)Fixed dissolved solids 1. Keep the evaporating dish used in determining TDS in muffle furnace for 1 hour at 550C 2. Repeat the 2-3 in total fixed solids 3. Weight of fixed dissolved solids = W6-W4 in mg Where W6-weight of empty evaporating dish + fixed solids left after ignition G)Volatile dissolved solids 1. Total fixed solids – TDS H)Fixed suspended solids 1. Total fixed solids – Volatile dissolved solids I)Volatile suspended solids 1.Total volatile solids – Volatile dissolved solids J) Settleable solids 1.Fill imhoff cone to 1lt with thoroughly mixed sample and settle for 45minutes 2. Gently stir the sides of cone with rod 3. Settle for 15minues
  • 64. 64 TABULATION :- Item Sample 1 Sample 2 Volume of sample Weight of empty evaporating dish W1 Weight of dish + total solids W2 Total solids W2-W1 Weight of dish + fixed solids W3 Fixed solids W3-W1 Weight of empty evaporating dish W4 Weigh of dish + total dissolved solids W5 Total dissolved solids W5-W4 Weight of dish + fixed dissolved solids W6 Fixed dissolved solids W6-W4 Total solids Fixed solids Dissolved solids Suspended solids Volatile solids RESULT :- i) Suspended solids =------- m/l ii) Settleable solids = -------m/l iii) Volatile solids = ------ m/l iv) Fixed solids = ------- m/l
  • 65. 65 EXP No 11 DETERMINATION OF DISSOLVED OXYGEN AND BOD OF THE GIVEN SAMPLE
  • 66. 66 11.a) DETEMINATION OF DISSOLVED OXYGEN :- AIM :- To determine the DO for the given water sample by winkler’s method APPARATUS REQUIRED :- 1. DO meter or potentiometer with electrodes which is silver anode and gold cathode GLASSWARES REQUIRED :- 1) Burette 2) Pipette 3) Conical flask ACIDS / REAGENTS REQUIRED :- 1. Distilled water 2. Sodium sulphate 3. Potassium chloride 4. Starch , 5. Conc sulphuric acid
  • 67. 67 SAMPLES TAKEN : Beaker = NaSO4 ( Colorless) KCl ( yellow colour ) Starch indicator ( thick blue ) Conc Sulphuric acid ( colorless ) Final = PROCEDURE :- 1. Add KCl in electrolyte cell and slowly insert the electrode and wipe it cleanly 2. Put cell in sodium sulphate solution 3. Switch ON the meter by allowing it to stand in warm up condition 4. Temperature is also controlled at same time by temperature probe 5. Adjust the reading to 0 6. Take out cell and clean with distilled water 7. Dip the probe in solution and stirred it gently until correct reading observes . Note down the reading OBSERVATION :- Sample details = tap water Instrument used = potentiometer DO observed i) at initial stage = ------- mg/lt ii) At 5 days = -------mg/lt RESULT :- DO )1= ---------mg/lt DO)5 = -------- mg/lt
  • 68. 68 11.b)DETERMINATION OF BOD AIM :- To determine the BOD for given sample by inhibited BOD test PRINCIPLE :- BOD is briefly called as Biochemically Oxygen Demand .. The amount of dissolved oxygen that bacteria need for consumption of organic matter in a sample. It can be neither CBOD (Carbonaceous BOD ) or NBOD (Nitrogenous BOD) . Criteria Need :- A) It must be free from chlorine B) pH range from 6.5-7.5 C) Adequate microbial population APPARATUS REQUIRED :- 1. Incubator
  • 69. 69 GLASSWARES REQUIRED :- 1. BOD Bottle 2. Burette 3. Pipette 4. Flask ACIDS / REAGENTS REQUIRED :- 1. 2 chloro 6 Trichloromethyl Pyridine PROCEDURE :- 1. Add 2 chloro 6 Trichloromethyl Pyridine at final concentration of 10mg/lt for nitrification inhibition . It has been that chemical does not suppress the organic matter oxidation 2. First we have to collect the water sample 3. First of all about , we have already determining the amount of DO in 11.a) , to determine the BOD at each day . i.e BOD at first day is (BOD)1 4. Here we have usually to find BOD of the given sample at more of 5 days (BOD)5 5. Organic matter + micro organism + nutrients - CO2 + H2O + micro organisms 6. BOD (mg/lt) = (DO)1 – (DO)5
  • 70. 70 TABULATION :- Day Volume of sample (ml) Initial burette reading Final burette reading Volume of titrant used sodium thiosulphate (ml) DO(mg/lt) CALCULATION :- DO)1 = ---------mg/lt DO)5 = ----------mg/lt BOD = DO)1 – DO)5 = ---- mg/lt
  • 71. 71 GRAPH :- Nitrogen BOD BOD5 carbon BOD BOD 0 5 10 15 Incubation days RESULT :- BOD for given water sample = ------ mg/lt
  • 72. 72 Exp No 12 DETERMINATION OF COD FOR GIVEN WATER SAMPLE
  • 73. 73 Exp No 12 DETERMINATION OF COD FOR GIVEN WATER SAMPLE AIM :- To determine the COD for given water sample PRINCIPLE :- COD is briefly known as Chemically Oxygen Demand . It is defined as amount of oxygen need to oxidize the organic carbon completely to CO2 , H2O and ammonia . It requires rapid test of 2-4hours GLASSWARES REQUIRED :- 1. Burette 2. 2 Pipettes of 250ml 3. Flask 4. weighing bottle APPARATUS REQUIRED :- 1. Incubator
  • 74. 74 ACIDS / REAGENTS REQUIRED :- 1. FAS (ferrous ammonium sulphate ) salt 2. Potassium dichromate 3. 1:1 sulphuric acid 4. Dilute sulphuric acid 5. Ferrion indicator SAMPLES TAKEN Beaker a) FAS ( whitish blue solution ) b) Dil H2SO4 ( colorless ) c) K2CR2O7 ( yellow colour ) d) Ferroin indicator ( green colour ) Burette – distilled water ( colorless ) Final = Reddish brown solution PROCEDURE:- 1. Fill the weighing bottle with FAS salt as W1 2. This is transferred in to flask and take the empty weighing bottle as W2 3. W1-W2 = we get the weight of the salt 4. We have to add half of the test tube is filled with dilute sulphuric acid and added to flask solution and shake well 5. First , we have to fill burette with distilled water 6. Then add distilled water up to neck of flask and its remaining portion will be titrated with distilled water solution from burette to flask mark , mix them in 5-6 minutes , which is colourless 7. The water in burette is washed out and add prepared FAS solution in it 8. Take another flask and 25ml of water sample is pipette in to it and transferred in to flask’ 9. Take 25ml of potassium dichromate solution by pipette it in to flask which is yellow colour
  • 75. 75 10.Add 1;1 sulphuric acid in this prepared solution and add also 3 drops of ferrine indicator 11.This solution is mixed will until it gets turns from yellow to green colour 12. Now this solution is totally titrated with burette FAS solution until the green colour to reddish brown colour 13.Now we prepare the solution only for given sample . It is called as back titration 14.But , we have also calculate the blank titration without using water sample by repeating steps 6-12 except that no distilled water can be added END POINT :-
  • 76. 76 TABULATION :- S.No Initial burette reading Final burette reading Volume of FAS solution 1 2 3 GRAPH :- 800 600 400 200 0.1 0.2 0.3
  • 77. 77 CALCULATION :- a) NORMALITY , N= ( Weight of FAS *4 ) / Equivalent weight of b) COD of given sample = ( 10*(V1-V2)*N* 8*1000 ) / Vs Where 8 – constant N – Normality Vs- Volume of sample RESULT :- COD = ------ mg/lt
  • 78. 78 EXP No 13 DETERMINATION OF SVI OF BIOLOGICAL SLUDGE AND MICROSCOPIC EXAMINATION
  • 79. 79 Exp No 13 DETERMINATION OF SVI OF BIOLOGICAL SLUDGE AND MICROSCOPIC EXAMINATION AIM :- To determine the SVI of biological sludge by microbiological examination PRINCIPLE :- SVI is the sludge volume index . It is the indicator of sludge settleability between the water content between flocs and SVI . It is the measure of activated sludge to separate from mixed liquor in order to achieve adequate sludge recycle and final efficient with low suspended solids concentration . It is defined as volume occupied by 1 g of sludge after 30minutes settling in a 1liter unstirred cylinder GLASSWARES REQUIRED :- 1. Burette 2. Pipette 3. Conical flask 4. Gradual water sample of volume 1 liter 5. Stirrer for SSVI test 6. Sludge sample PROCEDURE :- 1. Measure the concentration of sludge sample with TSS test 2. Fill 1Liter of gradual cylinder with sludge sample and allow sample to settle 3. But it is not easy to settle 4. So we have to add supernatent liquid to settle it quickly 5. After 30 minutes of settling , read the volume occupied by sludge from graduated cylinder (SV30 in ml ) 6. Calculate the SVI from relation with Xrss being measured sample concentration in gL-1
  • 80. 80 TABULATION :- S.No Volume of sludge (V1) Volume of sludge (V2) Total volume (V) (Xrss) 1 2 3 CALCULATION :- SSVI = SVss / Xrss = ---- ml g-1 Where Xrss - concentration of sludge sample – V2-V1 SVss - volume of sludge occupied by cylinder
  • 81. 81 END POINT :- RESULT :- SVI = --------- ml g-1
  • 82. 82 Exp No 14 DETERMINATION OF MPN INDEX OF THE GIVEN SAMPLE
  • 83. 83 Exp No 14 DETERMINATION OF MPN INDEX OF THE GIVEN SAMPLE AIM :- To Determine the MPN index of the given sample PRINCIPLE :- MPN is briefly known as Most Probable Number . It is the index used to estimate the concentration of viable microorganisms in a sample by means of replicable liquid broth growth in tenfold dilutions . It is most commonly applied for quality testing of water sample . That is the whether the water is safe or not . It is mainly tested for coli-forms bacteria present in water GLASSWARES REQUIRED :- 1. Burette 2. Pipette 3. 12 Test tubes 4. 3 Lactose broth test tubes PROCEDURE :- 1. Take drinking water sample 2. This is accounts in to 3 samples of 12 lactose broth test tubes 3. Take 10ml of water sample and passed in to each broths in 1st sample 4. Take 1ml of same sample in to each broths in 2nd sample 5. Take 0.1ml of same in to each broths in 3rd sample 6. All these samples are kept in incubator at 37ᵒC for 1 day 7. After this , these can be colour changes from colourless to dirty state , but not bin all broths , in 1 or 2 broths of sample definitely 8. We have see the number of broths which have colour changes to dirty , for example , In first sample , only 4 broths have colour changed and in 2nd , 3 are coloured and 3rd 1 is changed 9. From this results , By consult reference table pattern of most probable number for this sample is 4:3:1 ( for eg ) ., MPN value = 33 /ml
  • 85. 85 END POINT :- RESULT :- MPN = -------- /ml
  • 87. 87 1A)DETERMINATION OF pH 1. Define pH ? pH is the measure of alkalinity and acidity of the water sample by concentration of H+ ions in solution 2. Define the full form of pH ? pH means potential of Hydrogen ions 3. What are methods available for determining pH ? a) Indicator method , b) Electrode method , c)pH meter , d) pocket pH meter 4. What are conditions needed for test sample ? It depends upon type of pH sensor , holder material , room temperature 5. Which solution is immersed inside the solution of pH glass electrode ? AgCl , where Ag acts as cation and Cl acts as anion 6. What is permissible limit of pH in water ? 6.5-7.5 for potable water 7.What is the unit of pH ? It has no unit 1B) DETERMINATION OF TURBIDITY 1. Define Turbidity ? Turbidity is measure of cloudiness and haziness f water caused by large number of individual particles that are generally invisible to naked eye 2. What are methods available to determining turbidity ? Nepheleometric Turbidity meter , Jackson Candle Turbidity Meter , Bayli Turbidimeter , turbidity rod 3. What is the unit of Turbidity ? If nepheleometric turbidity meter is used , it is as NTU while jackson turbidity candle turbidity meter is used , it is used as JTU 4. What are causes for turbdity ? It is caused by suspended particles dissolved in water that scatter light making the water appear cloudy or milky 5. The material which is sued for determination of nepheleomteirc turbidity meter ? Silica
  • 88. 88 6. What is light source for nepheleomtric turbidity meter ? Tungsten Vapour lamp 7. What is limit of turbidity in water ? 5-10 NTU 1C)DETERMINATION OF CONDUCTIVITY 1. Define conductivity ? It is defined as the ability of conducting heat , electricity . When an electrical potential difference is created across a conductor , its ions starts flow , giving rise to an electric current 2. What is unit for conductivity of water ? μmho/cm or siemen . It is reciprocal of resistivity of sample . 3. What is conductivity of standard KCl solution is ? 1412 μmho/cm 4. Which water has more conductivity? Sea water . because it contains more salt contains chloride cntent , it leads to high conductivity 5. What is limit of conductivity in water ? 50-1500 μmho/cm 6. How will you determine the conductivity of sample ? Conductivity = Conductance * cell constant (K) 7. How to find TDS of conductivity ? TDS = o.64 * electrical conductivity 2 DETERMINATION OF HARDNESS 1. Define hardness ? It is defined as property of water which prevents the formation of lather with soap 2. What are types of hardness ? a) Carbonate hardness b) Non Carbonate hardness 3. Which method is used to find hardness of water ? EDTA method – Ethylene Di-amine Tetra Acetic acid 4. Which is used as indicator of determining hardness ? Eriochrome Black T
  • 89. 89 5. Which colour is obtained at end point ? Wine red to Deep blue 6. What is the hazard value of hardness in water sample ? >180mg/lt 7. Define total hardness ? It is defined as equivalent of calcium and magnesium ions hardness 3A) DETERMINATION OF ALKALINITY 1. Define alkalinity ? It is defined as the capacity of water a way of measuring acid neutralizing . To maintain relative constant pH 2. What are types of alkalinity ? a) Carbonate alkalinity b) Bicarbonate alkalinity c) Hydroxide alkalinity 3. What is the colour of phenolphthalein and methyl orange indicator ? Lavender , Deep Orange 4. Which colour defines the end point of the water sample in hardness determination ? Pale yellow 5. Which equivalent is used as Hardness ? CaCO3 6. Which solution is used as titrant ? N/50 standard sulphuric acid 7. What is the limit of total alkalinity in water sample ? 20-200mg/lt 3B) DETERMINATION OF ACIDITY 1. Define Acidity ? It is defined as property that has state of acid 2. What are types of Acidity ? a)Total acidity b) Mineral acidity 3. Which instrument can be used for determination of acidity ? Spectrometer
  • 90. 90 4. What is pH of phenolphthalein acidity and methyl orange acidity? 8.3 , 3.7 5. Which solution is used as titrant ? Standard NaOH 6.What is limit of acidity in water sample ? 0-50mg/lt 4)DETERMINATION OF CHLORIDE 1.What is role of chloride in water ? Chloride is the one of the inorganic matter in water sample . The chloride content in raw water is slight highly . 2.Which method is used to determine the chloride content ? It can be determined by Mohr’s method 3.What is normality of AgNO3 solution ? 0.014 4.What is equivalent value of chlorides in water ? 35.5 5.What is indicator of the chloride content ? Red brown 6.Which solution is used as indicator ? AgNO3 , K2CRO4 7.What is limit of chlorides in water sample ? <250mg/lt 5A) DETERMINATION OF PHOSPHATES 1. Which method is used to determine the phosphates in water ? Stannous chloride method 2. What are reagents used in determining phosphates ? Ammonium Molybdate , Stannous chloride
  • 91. 91 3. Which instrument is used to determine the phosphates in water ? Spectrophotometer 4. What is end point of the determining phosphates in water sample ? Blue colour solution 5. Which is used as titrant ? Ammonium Molybdate 6. What is limit of phosphates in water sample ? 0.1mg/lt 7. What is the name of holder ? Cuvette 5.B)DETERMINATION OF SULPHATES 1. Which method is used as sulphates determination ? Gravimetric method 2. What are reagents used in this determination ? BaCl , MgSO4 3. Which is used as titrant ? BaCl 4. What is end point of this experiment ? Colourless 5. What is limit of sulphates in water sample ? 1000mg/lt 6A)DETERMINATION OF IRON 1. What is role of iron in water ? Iron is only toxic at very high concentrations , it acts as a useful surrogate for other heavy metals 2. What are reagents used in this experiment ? Hydroxyammonium chloride , Phenanthroline 3. Which solution is used as titrant ? NaOH 4. What is end point of this solution ? Brownish orange colour 5. What is limit of iron in water sample ? 0.03mg/lt
  • 92. 92 6B)DETERMINATION OF FLUORIDES 1. Which method used to determine the fluoride content in water sample ? Spands method 2. What are reagents used in this experiment ? Spands Tri-sodium salt solution , Zinconyl acid reagent , sodium arsenite solution , 3. Which solution is used as titrant ? Standard Spands solution 4. What is end point of this experiment ? Pure Blood red colour 5. What is limit of fluorides in water sample ? 0.05mg/lt 7)DETERMINATION OF OPTIMUM COAGULANT DOSAGE 1. Which method is used to determine the coagulant dosage ? Jar test 2. Which is mostly used as Coagulant ? Alum (Al2SO4)3 . 18H2O 3.What is speed rate of pedals for mixing ? 20-120 revolutions 4.What is limit of coagulant dosage ? 10-15ml 5.Why coagulants are used ? Raw water contains some suspended impurities . Some of these can be removed by sedimentation and some of them cannot be easily removed . So we have do the coagulation process . Optimum dose of coagulant is the minimum dose of the coagulant that will be remove the maximum turbidity in water
  • 93. 93 8)DETERMINATION OF CHLORINE 1. Define chlorination ? It is done by determining chlorine content in water sample to find disinfection. It is called chlorination . 2. What are reagents used in water sample ? KI , starch indicator 3. Which solution is used as titrant ? Sodium Thiosulphate 4. What is limit of residual chlorine? 0.1-0.2ppm of residual chlorine at consumers end 5. Define residual chlorine ? It is low amount of chlorine remaining in water after a certain period after its initial precipitation 6.What are methods used to determine the chlorine in water ? a) Starch iodide test , b) DPD test , c)Residual chlorine kit 7. What is end point of this experiment ? From yellow to blue , till Disappearance of blue colour 9)DETERMINATION OF OIL AND GREASE 1.Which method is used to measure Oil and Grease ? Partially Gravimetric method 2.What are reagents used in this experiment ? Sulfuric acid Ethyl alcohol Petroleum ether 5. What is limit of oil and grease in water sample ? 75-100mg/lt
  • 94. 94 10)DETERMINATION OF SETTLEABLE , SUSPENDED , VOLATILE AND FIXED SOLIDS 1. Define Settleable solids ? It refers to any material that will not remain suspended or dissolved in water tank excludes TDS and TSS 5. Define suspended solids ? It refers to small solid particles remain in suspension in water as a colloidal or due to motion of water 6. Define volatile solids ? It refers to substance that can easily transform from its solid state in to vapour state without goes to liquid state 7. Define fixed solids ? It refers to summation of dissolved solids and suspended solids 8. What is limit of solids in water ? 500mg/lt 11)DETERMINATION OF DO AND BOD OF THE GIVEN SAMPLE 1. Define dissolved oxygen ? It is defined as measure of how much oxygen is dissolved in water 2. Define BOD ? BOD is briefly called as Biochemically Oxygen Demand .. The amount of dissolved oxygen that bacteria need for consumption of organic matter in a sample. It can be neither CBOD (Carbonaceous) or NBOD (Nitrogenous) 3. Which instrument used for this experiment ? Potentiometer 4. What is limit of BOD in water sample ? <8mg/lt
  • 95. 95 12)DETERMINATION OF COD OF THE GIVEN SAMPLE 1. Define COD ? COD is briefly known as Chemically Oxygen Demand . It is defined as amount of oxygen need to oxidize the organic carbon completely to CO2 , H2O and ammonia 2.What are reagents used in this experiment ? FAS (ferrous ammonium sulphate ) salt , potassium dichromate , ferrine indicator 3.Why here we need blank titration ? It is needed when all chemicals are working based on suitable places , so we have to deduct this water sample . This is called blank titration 4.What is end point of this experiment ? Brick Brown colour 5.What is limit of COD in this water sample ? 500-1500mg/lt 13.DETERMINATION OF SVI OF BILOGICAL SLUDGE AND MICROSCOPIC EXAMINATION 1. Define SVI ? SVI means Sludge Volume Index is defined as settling characteristics of sludge in aeration tank in activated sludge process 2.Define Activated sludge ? It is thick soft substance used for removing pollutants from waste water by a biological reaction that involves oxygen 3.What is limit of SVI in waste water sample ? 50-150ml/g
  • 96. 96 14)DETERMINATION OF MPN INDEX FOR GIVEN WATER SAMPLE 1.Define MPN ? MPN is briefly known as Most Probable Number . It is the index used to estimate the concentration of viable microorganisms in a sample by means of replicable liquid broth growth in tenfold dilutions 2. What is limit of MPN index 200MPN/100ml <<<<<<<<<<<<<<<<<<<<<<<<<THE END>>>>>>>>>>>>>>>>>>>>>>>>>>
  • 97. 97 CONCLUSION COURSE OUTCOMES 1.The students will have the required knowledge in the area of testing of both drinking water and waste water components of experiments experimentally