ENV LAB - 18CVL67 - Manual

Environmental Engineering Laboratory
Subject Code : 18CVL67 I.A. Marks : 40

Hours/Week : 1I + 2P Exam Hours : 03
Total Hours : 40 Exam Marks : 60
Credits - 02 Total Marks : 100
COURSE SYLLABUS:
01. Determination of pH, Acidity and Alkalinity.
02. Determination of Calcium, Magnesium and Total Hardness.
03. Determination of Dissolved Oxygen.
04. Determination of BOD.
05. Determination of Chlorides
06. Determination of percentage of available chlorine in bleaching powder,
07. Determination of Residual Chlorine.
08. Determination of Solids in Sewage: Total Solids, Suspended Solids, dissolved Solids,
VTUPulse.com
Volatile Solids, Fixed Solids, Settable Solids.
09. Determination of Turbidity by Nephelometer.
10. Determination of Optimum Dosage of Alum using Jar Test apparatus.
11. Determination of sodium and potassium by Flame Photometer.
12. Determination Nitrates by spectrophotometer.
13. Determination of Iron and Manganese.
14. Determination of COD ( Demonstration ).
REFERENCE BOOKS:
1. Lab Manual, ISO 14001 Environmental Management, Regulatory Standards for Drinking
Water and Sewage disposal
2. Clair Sawyer and Perry McCarty and Gene Parkin, “Chemistry for Environmental
Engineering and Science” , McGraw-Hill Series in Civil and Environmental Engineering
Scheme of Examination:
Question paper pattern:
1. Two experiments shall be asked from the above set
2. One experiment to be conducted and for the other student should write detailed procedure.
CLO’s and CO’s:
ENVIRONMENTAL ENGINEERING LAB
Subject Code : 18CVL67 I.A. Marks : 40

Hours/Week : 1I + 2P Exam Hours : 03
Total Hours : 40 Exam Marks : 60
EXPERIMENT 1:
Determination of pH Acidity and Alkalinity.
Objectives: To determine the pH, acidity and alkalinity of a given water sample
Generic Skills / Outcomes: After Performing, one can judge that the given water sample
is acidic or basic in nature and able to calculate acidity and alkalinity of water sample
EXPERIMENT 2:
Determination of Calcium, Magnesium and Total Hardness.
Objectives: To determine Calcium, Magnesium and Total hardness of given water

sample
Generic Skills / Outcomes: After performing the experiment one can validate that the
given water sample is hard or soft.
EXPERIMENT 3:
Determination of Dissolved Oxygen
VTUPulse.com
Objectives: To determine the DO of water sample
Generic Skills / Outcomes: After performing one can estimate the percentage of
dissolved oxygen present in the given water sample.
EXPERIMENT 4:
Determination of Chlorides by Electrical Conductivity Meter.
Objectives: To determine the amount of chlorides in a given water sample
Generic Skills / Outcomes: After performing the experiment one can validate the
amount of chloride is in the permissible range or not in a given water sample
EXPERIMENT 5:
Determination of percentage of available chlorine in bleaching powder.
Objectives: To determine the amount of chlorine in bleaching powder for a given water
sample.
Generic Skills / Outcomes: After performing, one can validate the amount of chlorine
present in bleaching powder which is usually added to disinfect the water
EXPERIMENT 6:
Determination of Solids in Sewage: Total Solids, Suspended Solids, dissolved Solids,
Volatile Solids, Fixed Solids, Settable Solids.
Objectives: To Determination of Solids in Sewage: Total Solids, Suspended Solids,
dissolved Solids, Volatile Solids, Fixed Solids, Settable Solids.
Generic Skills / Outcomes: After conduction, one can validate whether the amount of
dissolved, volatile, fixed and Settleable solids is in the permissible range or not for a
given water sample
EXPERIMENT 7:
Determination Sodium and Potassium by Flame Photometer
Objectives: To determine sodium and Potassium present in given sample by flame
photometer
Generic Skills / Outcomes: One can validate the amount of sodium and potassium
present in given water sample
EXPERIMENT 8:
Determination of Iron and Manganese by Spectrophotometer.
Objectives: To determine the amount of iron present in the given water sample by
phenantheroline method
Generic Skills / Outcomes: After performing, one can estimate the amount of iron
present in given water sample
EXPERIMENT 9:
Determination of COD.
Objectives: To determine the COD value of given water sample
Generic Skills / Outcomes: After performing the experiment one can validate whether it
is permissible range or not.
QUESTION PAPER PATTERN:
One lab experiment to be conducted for 60 marks in 3 hours duration
OBJECTIVES:
1. To determine the amount of total solids present in waste water.
2. To determine the amount of pH, Calcium and Magnesium carbonates, chlorides, iron, Manganeses,.
3. To determine the value of DO, BOD and COD.
Generic Skills / Outcomes:
1. One can able to estimate the amount of chemicals present in the water.
2. After performing the experiments one can able to validate that the given water sample is whether it
VTUPulse.com
fit for drinking or not based on permissible values.
3. Based on DO, BOD and COD values of waste water, one can decide the type of disposal either to
water or land based on permissible value before or after treatment
Prerequisite: Environmental Engineering - I

CONTENT LIST
SL. PAGE
EXPERIMENT NAME
NO. NO.
Determination of pH, Acidity and Alkalinity.

1.
Determination of Calcium, Magnesium and Total Hardness.

2.
Determination of Dissolved Oxygen

3.
Determination of Chlorides by Electrical conductivity,

4.
Determination of percentage of available chlorine in bleaching
5. powder
Determination of Solids in Sewage: Total Solids, Suspended

Solids, dissolved Solids, Volatile Solids, Fixed Solids, Settable
6.
Solids.
VTUPulse.com
7.
8.
Determination of Iron by Spectrophotometer.
Determination of Manganese by Spectrophotometer.
Determination of Sodium by Flame Photometer.

9.
Determination of Potassium by Flame Photometer.

10.
Determination of COD . ( Demonstration)

11.
Environmental Engineering Laboratory 18CVL67
Experiment : Determination of Alkalinity, Acidity and pH
Aim: To conduct pH, acidity and alkalinity test on water.

Objective: To determine the acidity, alkalinity, pH of the given water sample.
Apparatus: Pipette, burette, titration flask, Beaker, pH meter
Reagents: NaOH, HCl, Methyl orange and Phenolphthalein indicators.
Theory:
pH is the negative logarithm of hydrogen ion concentration which measures the acidic or
alkaline condition of a solution. pH of natural waters lie between of 4 to 9. Several processes like
softening, coagulation, adsorption, dewatering sludge’s or oxidizing substances like cyanide are pH
dependent. Very low and very high pH values are not suitable for biological metabolism and bacterial
growth. For public water, pH should be close to 7. Acidic water cannot be used in construction as it
can increase the rate of corrosion of metal used. Acidity of water is due to the presence of dissolved
carbon dioxide (bicarbonates), weak organic acids (formic, acetic acid) due to microorganisms and
VTUPulse.com
strong mineral acid (Sulphuric, hydrochloric, nitric acid) due to industrial wastes. Alkalinity of water
is its capacity to neutralize acids. Alkalinity in water is mainly due to the presence of hydroxides
(hydroxyl alkalinity), carbonates and Bicarbonates. The high pH of water is due to hydroxyl alkalinity.
The amount of basicity in water can be determined by titrating it with strong acids.
PROCEDURE:
Preparation of standard acid or base:
Collect the acid/base from the stock solution (note down the volume and concentration
given)and make it upto 100ml using distilled water. Calculate its normality as given.
pH meteric : Standardize the instrument against temperature and two buffer solutions of known pH
prepared using buffer tablets. After standardization the electrode is dipped in the water samples whose
pH is to be determined. The pH displayed is noted down. Every time before the electrode is put into a
different sample, it is rinsed with distilled water and wiped using an absorbent like tissue paper.
Acidity: Pipette out 25ml of water sample into a conical flask. Titrate against standard Sodium
hydroxide solution using methyl orange indicator. The endpoint is confirmed by the change of orange
red to yellow colour note down the volume of NaOH consumed (V1). Then to the same solution add 2-
3 drops of phenolphthalein indicator to the same solution and continue the titration till the colour
changes from yellow to pink. And note down the volume of the NaOH consumed (V2). Repeat the trail
for concordant values. Calculate the respective acidity of water sample using volume of NaOH
consumed.
Department of Civil Engineering, ATMECE
Alkalinity: Pipette out 25ml of water sample into a conical flask. Titrate against standard
Hydrochloric acid using phenophthalein indicator. The endpoint is confirmed by the change of pink
red to colourless, note down the volume of HCl consumed (V3). Then to the same solution add 2-3
drops of methyl orange indicator to the same solution and continue the titration till the colour changes
from yellow to red. Note down the volume of the HCl consumed (V4). Repeat the trail for concordant
values. Calculate the respective alkalinity of water sample using volume of HCl consumed.
Result and discussion.
Observation and calculation
Normality of NaOH= NNaOH (given) = N, Volume of NaOH= VNaOH (given) = _ ml
Normality of acid = NHCl (given) = N, Volume of acid= VHCl (given) = ml
Acidity Alkalinity
Burette Standard base Standard Acid
Conical
25ml of water sample 25ml of water sample
flask
VTUPulse.com
First Methyl orange and then First phenolphthalein and Then Methyl
Indicator
phenolphthalein orange
End point 1. Orange red to yellow colour. (M) 1. Pink to colourless (P)
2. Yellow to pink colour. (P) 2. Orange to red colour (M)
Acidity Alkalinity
Trial number 1 2 1 2
M P M P P M P M
Final Burette Reading (ml)
Initial Burette Reading (ml)
Volume run down (ml)
Volume consumed VM = , VP = VP = , VM =
Acidity calculation :
1000 cm3 of 1N NaOH = 50 g of CaCO3 (Eq. wt of CaCO3)
Methyl orange endpoint = acidity due to mineral acid
Phenolphthalein endpoint = total acidity of water

Alkalinity Calculation:
1000 cm3 of 1N NaOH = 50 g of CaCO3 (Eq. wt of CaCO3)
Phenolphthalein endpoint = alkalinity due to Hydroxide and Carbonate
Methyl orange endpoint = total alkalinity of water
Total acidity of water sample = mg/L of CaCO3

Total alkalinity of water sample = mg/L of CaCO3
Viva Questions
1. Define (i) acidity (ii) alkalinity (iii) pH..
2. Which is the indicator used for titration in determination of acidity?
3. Which is the major acidic component in surface water?
4. Discuss the source and nature of acidity.
VTUPulse.com
5. Discuss the significance of carbon dioxide and mineral acidity.
6. Can the pH of a water sample be calculated from a knowledge of its acidity? Why?
7. Can the carbon dioxide content of a wastewater sample known to contain significant concentrations of
acetic acid be determined by the titration procedure? Why?
8. What is the combination for mixed indicator?
9. Which is the main component for imparting alkalinity to natural water?
10. What is ppm?
11. What is standard solution? Why do we take 0.02 N H2SO4 for the titration?
12. Which is the major form of alkalinity? How is it formed?
13. What is excess alkalinity? How do you express it?
14. The water where algae are flourishing is alkaline. Why? Will there be diurnal variation in pH?
15. Why does the pH change on aerating the water?
16. For efficient coagulation the water must be alkaline. Why?
17. What is the pH of neutral water?
18. What is the acceptable value of pH for portable water?
19. What is acidic buffer and basic buffer?
20. What is the range of pH scale?
Outcome:
After Performing, one can judge that the given water sample is acidic or basic in nature and able to calculate
alkalinity and acidity of water sample.

EXPERIMENT : CALCIUM, MAGNESIUM AND TOTAL HARDNESS
Aim: To conduct Hardness test on water.

Objective: To determine Calcium, Magnesium & total hardness in given water sample.
Apparatus: Pipette, burette, titration flask
Reagents: EDTA, Buffer Solution, 1N NaOH, Erichrome Black T (EBT) & Murexide
(Ammonium purpurate) indicator.
Theory:
Hardness of water is its resistance to the production of lather with soap and ability to
produce scale in pipes and boilers. Calcium and magnesium salts produce hardness in water.
The hardness of water reflects the nature of geological formations with which it has been in
contact.
Hardness is of two types: Permanent hardness due to completely soluble salts of Ca
and Mg like Chlorides, sulphates, nitrates, etc. Temporary hardness due to carbonate and
bicarbonate salts of Ca and Mg. Excessive hardness may cause the accumulation of Ca and
VTUPulse.com
Mg in human body which may lead to kidney stones, paralysis attack and also cardiac arrest.
Consumes excess of soap during washing. It imparts saline taste to water. Boiling and cooling
of hard water in boiler forms scale and incrustation of pipes. Hardness of water can be
reduced by: Boiling, Lime soda, Zeolite or Base Exchange, Ion exchange processes.
Permissible limits: Calcium = 75 mg/L, Magnesium = 125 mg/L, Total hardness = 200 mg/L
Principle:
EDTA forms complex with Ca & Mg present in water (Total), Ca alone is determined
by precipitating Mg using sodium hydroxide ant pH 12-13.
Preparation of standard EDTA:

Collect the EDTA from the stock solution (note down the volume and concentration
given) and make it up to 100 ml using distilled water. Calculate its normality.
Procedure:
(1) Determination of Total Hardness
Pipette out 25ml of the given water sample into a clean conical flask. Add
approximately 3-5 ml of NH3-NH4Cl buffer (To maintain pH 10) and a pinch of Erichrome
black – T (EBT). Titrate against Standard Na2EDTA solution till the color of the solution

changes from wine red to clear blue. Note the volume of Na2EDTA solution consumed.
Repeat the titration for concordant values. Calculate the total hardness of the water sample
using volume of Na2EDTA consumed.
(2) Determination Hardness due to Calcium

The titration is repeated by adding 3-5 ml 1N NaOH & Murexide indicator to 25 ml
given water sample and titrate it against standard Na2EDTA solution till the colour changes
from pink to purple. Calculate the amount of Calcium present in the water sample using
volume of Na2EDTA consumed. The difference in Total hardness and calcium gives the
amount of Mg present in water.
Removal techniques:
Softening techniques such as boiling, lime soda process, Zeolite process and Ion exchange
process may be used for removal of excess Calcium and Magnesium.
 Observation and calculation
VTUPulse.com
Weight of the given Na2EDTA salt, W1 = ............... gm
Normality & Volume of given Na2EDTA = N = ………………………
Normality (N) = [(Weight of Na2EDTA salt X 1000) /(Equivalent wt of Na2EDTA salt X 100)]
 [Equivalent weight of Na2EDTA is 372.24]
Total hardness Calcium hardness
Trial number
1 2 3 1 2 3
Initial Burette Reading (ml )
Volume of EDTA run down (ml)
Volume consumed VT = VCa =
𝑉𝑇∗𝑍∗𝑀𝑜𝑙𝑚𝑎𝑠𝑠𝑜𝑓𝐶𝑎𝐶𝑂3 ∗1000
 Total Hardness as mg/L CaCO3 =
𝑚𝑙𝑜𝑓𝑤𝑎𝑡𝑒𝑟𝑡𝑎𝑘𝑒𝑛
=.................................................mg/L of CaCO3
 [Molecular mass of CaCO3 = 100]

 Calcium Hardness =
∗∗𝐴𝑡𝑜𝑚𝑖𝑐𝑚𝑎𝑠𝑠𝑜𝑓𝐶𝑎∗1000
𝑚𝑙𝑜𝑓𝑤𝑎𝑡𝑒𝑟𝑡𝑎𝑘𝑒𝑛
= .......................................... mg/L
 [Atomic mass of Ca = 40]
(𝑉𝑇 −
−𝑉𝐶𝑎)∗𝑍∗𝐴𝑡𝑜𝑚𝑖𝑐 𝑚𝑎𝑠𝑠𝑜𝑓𝑀𝑔∗1000
Magnesium Hardness =
𝑚𝑙 𝑜𝑓𝑤𝑎𝑡𝑒𝑟 𝑡𝑎𝑘𝑒𝑛
= ............................................... mg/L
 [Atomic mass of Mg = 24.3]
 Results
Total Hardness mg/L of CaCO3
Hardness due to Calcium mg/L of Ca
Hardness due to Magnesium mg/L of Mg
VTUPulse.com
 Environmental Significance
Advantages:



Absolutely soft water is tasteless. Eg: Distilled water.
Moderate hard water is preferred to soft water for irrigation purpose.
Scales are formed on inner coating of pipelines and hence prevent corrosion.
 Absolutely soft water is corrosive and dissolves metals.
 More cases of cardiovascular diseases are reported in soft waters.
 Hard water is useful to growth of children due to presence of calcium.
Disadvantages:
 Hard water causes excessive consumption of soap user for cleaning purposes.
 Scales formed act as insulation in case of pipelines and cause enormous loss in boilers.
 Scales formed in distribution mains reduce their carrying capacity.
 Magnesium hardness (associated with sulphate ions) has a laxative effect on persons
unaccustomed to it.
 Makes food tasteless.

 Viva Questions
1. Define Hardness
2. What is permissible value of Calcium that should be present in water?
3. Which are salts of Calcium impart hardness to water?
4. What is permissible value of Magnesium that should be present in water?
5. Which are salts of Magnesium impart hardness to water?
6. What are the processes for removing hardness of water?
7. Which water produces more lather?
8. Which are salts responsible for hardness of water?
9. What is EDTA?
10. What is the need of buffer in titration process?
 Outcome
After performing the experiment one can validate that the given water sample is hard or soft.
VTUPulse.com

Experiment : Determination of Percentage of Available Chlorine

in Bleaching Powder
Aim: To determine percentage available Chlorine content of the given Bleaching powder
sample.
Apparatus: Pipette, burette, titration flask,
Reagents: Bleaching powder, Potassium Iodide (Powder), Sodium Thiosulphate (Na 2S2O3)
reagent, Glacial acetic acid, Starch indicator.
Theory:
Chlorine is a strong oxidizing agent hence added to water as disinfectant in the form
of bleaching powder (BP) to destroy pathogenic organisms in drinking water. Commercial
BP contains 25 – 30 % chlorine, this chlorine content reduces when the powder is exposed to
atmosphere or stored for a long period. The strength of bleaching powder is determined by
percentage of available chlorine in it.
Bleaching powder is Calcium hypochlorite [Ca(OCl)2] which combines with water
liberating hypochlorite ion (OCl-), which further forms hypochlorous acid (HOCl) and acts as
VTUPulse.com
disinfectant. Percentage of chlorine in bleaching powder can be determined by iodometric
method or by Orthotoulidine method. This experiment is useful to assess the quality of
bleaching powder and also useful to estimate the amount of bleaching powder required for
effective disinfection of water.
The amount of chlorine consumed for oxidation and disinfections is known as
chlorine demand. Chlorine demand is the difference between the amount of chlorine added
to water and the amount residual chlorine after a specified contact time. Water which yields
residual chlorine of about 0.2mg/L at the end of 10 minutes contact period is considered as
the optimum dosage. During rainy season and break out of epidemics higher residual chlorine
is maintained (up to 1 mg/L). A larger brine residual causes bad taste while a smaller residual
is not reliable.
Principle of iodometric method:

The chlorine present in the bleaching powder gets reduced with time. So, to find the exact
quantity of bleaching powder required, the amount of available chlorine in the sample must
be found out. Chlorine will liberate free iodine from potassium iodide solution when its pH is
8 or less. The iodine liberated, which is equivalent to the amount of active chlorine, is titrated
with standard sodium thiosulphate solution using starch as indicator.

Preparation of standard Sodium Thiosulphate solution:

Collect Sodium Thiosulphate salt or stock solution (note down the volume and concentration
given) and make up it to 100 ml using distilled water. Then calculate its normality.
Preparation of chlorine water from bleaching powder:

Weigh 1g of bleaching powder and make it into a paste by adding small quantity of distilled
water. Add some water stir it and allow it to settle for a few minutes. Decant the supernatant
solution and dilute to 1000ml with distilled water in a volumetric flask and stopper it. This is
called chlorine water/ standard chlorine solution.
Procedure:
Collect the stock chlorine solution, transfer 25 ml solution to a titration flask, add 5m1 acetic
acid (acidic pH). Add 10 ml of 10 % potassium Iodide and add 15 m
mll distilled water. Titrate
the reaction mixture against standard Na2S2O3 till pale yellow colour is obtained. Add 2 to 3
drops of starch indicator and continue titration till the blue colour completely disappears.
Repeat the titration for concordant values.
 OBSERVATIONS AND CALCULATIONS:
VTUPulse.com
 mg/L of bleaching powder = ............................... mg/L
Normality of given Sodium thiosulphate solution = N =
NS = Normality of Stock Sodium thiosulphate solution

NS * VS
V
= ............ N
VS = Volume of Stock Sodium thiosulphate solution given =............ ml
V = Volume of Sodium thiosulphate solution prepared = ........... ml
Burette Standard Na2S2O3 solution

Conical flask 25 ml chlorine solution + 5 ml acetic acid + 10ml KI + 1 Test tube H2O
Indicator 2-3 drops of starch solution near the end point
End point Complete disappearance of blue colour
Trial number 1 2 3
Volume of Na2S2O3 solution run down (ml)
Volume of sodium thiosulphate solution consumed V = ....................... ml

V * N * Atomic mass of chlorine * 1000

 mg/L of chlorine = ml of sample = .......................... mg/L
 [Atomic mass of chlorine = 35.5]
mg /L of chlorine
 % chlorine in Bleaching powder = *100
mg /L of bleaching
powder
 RESULT: Percentage of available chlorine in bleaching powder = .
 Environmental Significance
1. This test is useful to assess the quality of bleaching powder.
2. It is useful to estimate the bleaching powder required for effective disinfection of water.
1. What do you means by disinfection?
2. For what purpose, bleaching powder is added to water?
VTUPulse.com
3. What is portable water?
4. What is the amount of residual chlorine that should be present in water?
 Outcome
After performing, one can validate the amount of chlorine present in bleaching powder which
is usually added to disinfect the water.

Experiment : DISSOLVED OXYGEN (DO)

Aim: To Conduct DO test on water.
Objective: To determine Dissolved Oxygen content of the given water sample.
Apparatus: BOD bottle, pipette, burette, titration flask, measuring jar.
Reagents: MnSO4, Alkali Iodide Azide, con H2S04, Sodium Thiosulphate reagent, Starch
indicator
Theory:
Gaseous oxygen is present in water in dissolved state called dissolved oxygen (DO); it
ranges from 14.6 – 7 mg/L in pure water. The survival of fish and other aquatic life is
dependent on DO present in water. Organic impurities present in water are oxidized by
aerobic organism with the aid of DO. The solubility of DO reduces in impure waters and at
higher temperatures. Critical conditions occur during summer when solubility of Oxygen is
low and rate of biological activity is high.
A minimum of 4 mg/L DO must be present in streams for aquatic life. Discharge of
organic pollutants (wastes) to water drops the DO level to zero. This is known as Oxygen sag.
VTUPulse.com
DO test is used for monitoring water pollution and also the BOD. Absence of DO indicates
anaerobic conditions. All aerobic wastewater treatment processes depend upon the presence
of DO. Drinking water should be rich in DO concentration for good taste. DO test is used to
evaluate the pollution strength of domestic and industrial wastes. DO may cause corrosion of
Iron and steel.
Azide Modification of Winkler’s method for determination of DO:
Principle:
DO in water oxidizes Manganese ions to its higher oxidation state in alkaline medium,
which further oxidizes potassium iodide releasing free iodine gas in acidic condition. The
amount of free iodine released is equivalent to DO present which is measured by titrating
with std. sodium thiosulphate solution. Interference due to nitrites is over come by using
azide modified Winkler’s method.
Preparation of standard Sodium Thiosulphate solution:

Collect the Sodium Thiosulphate (Na2S2O3 ) salt or stock solution (note down the volume and
concentration given) and make up it to 100 ml using distilled water. Calculate its normality.

Procedure:
Take 300ml water sample in BOD bottle. Add 2ml MnSO4 solution and 2 ml alkali iodide
azide reagent and stopper the flask mix well. A reddish brown gelatinous precipitation forms.
Allow the precipitation to settle for 15 min, and then add 2 ml conc. H2S04, replace stopper
and mix till dissolution is complete.
Measure out 101 ml of above solution into a clean 250ml conical flask and titrate against
standard sodium thiosulphate reagent till a pale yellow colou
colour,
r, is obtained. Add a 2 - 3 drops
of starch indicator and continue titration till the blue colour completely disappears. Repeat the
titration for concordant values.(101 ml solution corresponds to 100 ml sample after correction
for loss of 1 ml sample by displacement with reagents.)
 OBSERVATIONS AND CALCULATIONS:
𝑵𝑺∗𝑽𝑺
Normality of given Sodium thiosulphate solution = N =
𝑽
NS = Normality of Stock Sodium thiosulphate solution = ............ N
VS = Volume of Stock Sodium thiosulphate solution given =............ ml
V = Volume of Sodium thiosulphate solution prepared = ............ ml
VTUPulse.com
Burette
Conical flask
Indicator
Standard Solution of Sodium thiosulphate
101 ml of water sample
Starch near the end point
End point Complete disappearance of blue colour
Trial number 1 2 3
Volume of Na2S2O3 solution run down (ml)
Volume of Na2S2O3 solution Consumed V= ml
V∗N∗Atomic mass of oxygen ∗1000


DO mg/L = ml of sample =................ mg/L
[ Atomic Mass of Oxygen = 8 ]

RESULT : Amount of Dissolved Oxygen in given water sample = .................. mg/L
 Environmental Significance:
 The oxygen remains in water in dissolved form depending upon the temperature of water.
As the temperature increases, the solubility of D.O in water decreases.
 The organic matter present in the waste water poses a Biochemical Oxygen Demand. This
demand is met with the Dissolved Oxygen present in the fresh body of water. If the
organic load (volume x BOD) of the waste water is more than the asset (volume x DO)
the whole of the oxygen is depleted. This causes the death of fish and other aquatic
animals and plants and they being organic matter further increase the demand of oxygen
for the degradation.
 Aerobic bacteria thrive when free oxygen is available in plenty. Aerobic conditions
prevail when sufficient DO is available in water. End products of aerobic metabolism are
stable and not foul smelling.
 Higher temperature, biological impurities, ammonia, nitrites, ferrous iron, chemicals such
as hydrogen sulphide and organic matter reduces DO values.

VTUPulse.com
Drinking water should be rich in DO for good taste. However higher value of DO in
water may cause corrosion of iron and steel.
DO test is used to evaluate the pollution strength of industrial and domestic waste.
1. Define DO?
2. Winkler titration method is based on which property of DO?
3. DO depends on which property of water?
4. What DO will impart to portable water?
5. What should be the minimum DO to be present in water for the survival of aquatic life?
6. Discuss the environmental significance of dissolved oxygen.
7. Draw the oxygen saturation curve.
 Outcome
After performing one can estimate the percentage of dissolved oxygen present in the given
water sample.

Experiment : SOLIDS IN SEWAGE

Aim: To determine the concentrations of different types of solids in given wastewater
Objective: Determination of Solids in Sewage: Total Solids, Suspended Solids, dissolved
Solids, Volatile Solids, Fixed Solids, Settable Solids.
Apparatus: Porcelain dish, Filter Paper (or Hersh funnel or Gooch crucible), Imhoff cone,
Drying oven, Analytical balance, muffle furnace, Desiccator, suction apparatus or vacuum
pump.
Theory:
The concentrations of different types of solids present in water help in determining its
strength, scheme of treatment and design of various treatment units. It also helps in deciding
the method for disposal of wastewater.
Significance:
Solids in water may be settleable, suspended, dissolved, volatile and fixed, this
together constitutes total solids.
VTUPulse.com
1. The settleable solids are those, which are capable of settling when, placed in a quiescent
condition.
2. The suspended solids are those which are not soluble in water and remain in suspension
for a long period. These solids impart turbidity to the water.
3. The dissolved solids impart color, and odor to water.
Procedure:
a) Total Solids, volatile solids and fixed solids:

Determine the initial weight of a clean dry empty evaporating dish. Take 50 ml of well mixed
sewage sample in the dish and evaporate water content by applying heat. Determine the
weight of the dish with solid residue after cooling to room temperature in a desiccator. Keep
the dish in the muffle furnace at 550°C for 15 minutes. Cool to room temperature in a
desiccator and determine the final weight of dish with fixed residue.
b) Suspended and dissolved solids:

Determine the initial weight of a clean dry empty Hersh funnel. Filter 50 ml sewage sample
through the funnel-applying vacuum to reduce the time of filtration. Keep the funnel in the
oven at 103°C to remove the water content and dry the solid residue. Cool to room
temperature in desiccators and find the final weight of funnel.

c) Settleable solids:
Fill an Imhoff cone up to 1000ml mark with a thoroughly mixed sample and keep in a stand.
Allow settling for 45 minutes. Gently rotate the cone to dislodge solids sticking to sides of
cone. Allow the contents to settle for a further period of 15 minutes. At the end of settling
note the volume of sludge settled at the bottom of cone in ml. Record the volume of settleable
matter in the cone as ml/litre.
 Observation & Calculation:

A. Determination of total Solids, volatile solids and fixed solids:
Weight of dry empty crucible = W1 = g

Weight of crucible with solid residue after evaporation = W 2 = g
Weight of crucible after removing from muffle furnace = W3 = g
𝑊2 − 𝑊1
Total Solids =
𝑚𝑙𝑜𝑓𝑤𝑎𝑡𝑒𝑟 *106 = ................................ mg/L
𝑊3−𝑊1
Fixed Solids = * 106 = ............................... mg/L
VTUPulse.com
𝑚𝑙𝑜𝑓𝑤𝑎𝑡𝑒𝑟
Volatile solids = Total solids - Fixed solids = mg/L
B. Determination of Suspended and Dissolved solids:

Weight of dry Hersh Funnel = W4 = g
Weight of Hersh funnel with solid residue = W5 = g
𝑊5−w4
Suspended Solids = *106 = ............................ mg/L
𝑚𝑙 𝑜𝑓𝑤𝑎𝑡𝑒𝑟
Dissolved solids = Total solids - Suspended solids = mg/L
C. Determination of Settleable Solids:

Volume of Settlable impurities = ml/L

 Results:
Sl. No Item Values
1 Total Solids …………………(mg/L)
2 Suspended Solids …………………(mg/L)
3 Dissolved Solids …………………(mg/L)
4 Volatile Solids …………………(mg/L)
5 Fixed Solids …………………(mg/L)
6 Settlable Solids …………………(ml/L)
1. Define Total Solids.

2. Define Suspended Solids
3. Define Volatile Solids
VTUPulse.com
4. Define Dissolved Solids
5. Define Fixed Solids
6. Define Settleable Solids.
7. What is the normal size of colloids in water?
8. What methods are available for the removal of organic dissolved solids in water and
waste water?
 Outcome
After conduction, one can validate whether the amount of dissolved, volatile, fixed and
Settleable solids is in the permissible range or not for a given water sample.

Experiment : DETERMINATION OF MANGANESE

Aim: To determine the manganese content in the water sample by Spectrophotometer.
Objective: To determine the amount of manganese present in the given water sample by
Spectrophotometer instrument.
Instrument: Spectrophotometer, Beaker of 250ml, Volumetric flask of 100ml & 25ml
capacity, burette.
Reagents: Manganese sulphate, Orthophosphoric acid, potassium periodate.
Principle: Manganese is an essential nutrient at about 2.5-5mg/day, but overexposure can

potentially cause serious health issues. Long term exposure to manganese cam cause toxicity
to nervous system and Parkinson’s like symptoms. Infants cannot breakdown manganese in
their bodies as effectively as adults, which can cause issues in early brain development.
Commonly used method for the determination of trace manganese involves the oxidation of
Mn2+ to pink coloured Mn5+ using potassium periodate in presence of orthophosphoric acid.
This can be spectrophotometrically measured at 520nm and correlated using standard.
VTUPulse.com
Procedure:
Part A: Preparation of standard Mn2+ solution

5ml of the stock manganese sulphate (Mn2+) solution is transferred to 250ml beaker and 30ml
of distilled water is added to it. Add 10ml of orthophosphoric acid and 5ml of potassium
periodate solution and place it on a heating mantle for boiling. The colour of the solution
changes to pink. If the pink colour doesn’t appear add 5ml of potassium periodate and
continue boiling. The coloured solution is completely transferred to 100ml volumetric flask.
Care should be taken while boiling and transferring the solution. Even a small spillage,
experiment must be repeated from the beginning.
Part B: Determination of trace manganese in water

Draw out 5, 10, 15 & 20ml of the above manganese solution into separate 25ml volumetric
flask. Make upto the mark using distilled water and mix well. After 10 minutes measure the
absorbance at 520 nm against blank solution (use distilled water as the blank for calibration).
Repeat the same with the given unknown sample and measure the absorbance. Plot a graph of
concentration of Manganese (X-axis) and Absorbance (Y-axis).

 Observations and calculations

Concentration of stock Mn2+ = ppm
Volume of stock solution given = V = ml
𝑉∗30
Concentration of Mn2+ in diluted solution = a = = ............... ppm
100
Volume of Mn2+ Concentration of Iron Transmittance
VTUPulse.com
Sl. No. A = 2-log t
Taken (Z) = (Z X a) mg/L (t)
1 5
2 10
3 15
4 20
5 Test solution
 Result: Amount of manganese in the given water sample = mg/L.
 Environmental significance
In explorations of new water supplies, particularly from underground sources, iron and
manganese determinations are important considerations. Supplies may be rejected on this
basis alone. When supplies containing amounts in excess of 0.3 mg/L iron and 0.05 mg/L
manganese are developed, the engineer must decide whether treatment is justified, and if so,
which is the best method. The efficiency of treatment units is determined by routine tests of
iron and manganese.

 Outcome:
After performing the experiment, one can estimate the amount of iron present in given water
sample.
 Viva questions
1. What is the environmental significance of manganese in water supplies?
2. Discuss briefly how manganese get into underground water supplies?
3. What analytical methods area generally used for measuring the concentration of
manganese in water supplies?
VTUPulse.com

EXPERIMENT : DETERMINATION OF IRON
Aim: To conduct iron test by Spectrophotometer

Objective: To determine the amount of iron present in the given water sample by
phenantheroline method.
Reagents: Ferrous ammonium sulphate (FAS), Sulphuric acid (H2SO4), Hydroxylamine
hydrochloride, 1,10 Phenonthroline, Sodium acetate.
Principle: Iron is only toxic at very high concentrations; it acts as a useful surrogate for other
heavy metals, whose presence in drinking water is a real danger to public health. Amount of
iron in municipal drinking water should be less than 0.3 ppm (0.3 mg/L).
Commonly used method for the determination of trace iron involves the complexation of Fe 2+
with phenanthroline to produce an intensely red-orange colored complex. This can be
spectrophotometrically measured at 510 nm.
Procedure:
VTUPulse.com
Part A: Preparation of Mohr's salt solution
Weigh about 2 g ferrous ammonium sulphate (FAS) & transferred into 100 ml volumetric
flask. Add 2ml of 2.5M H2SO4 to avoid hydrolysis. Dissolve the crystals and make up the
solution up to the mark and mix well. Transfer 1ml of stock FAS solution to 100 ml standard
flask and dilute up to the mark using distilled water. Calculate the normality of FAS solution.
Part B: Determination of trace iron in water

Draw out 1, 2, 3, 4 & 5ml of FAS solution into 5 separate 50 ml volumetric flasks. Add 1 ml
of hydroxylamine hydrochloride, 4ml of sodium acetate , 5ml of Phenonthroline, and make
up to the mark using distilled water and mix well. After 10minutes Measure the absorbance at
510 nm against blank solution. Repeat the same with the given unknown sample and measure
the absorbance. Plot a graph of concentration of iron (X-axis) and Absorbance (Y-axis).

 Observations and Calculations:

Normality of Stock FAS = N = N
Volume of FAS given = VF = ml
N∗VF
Concentration of FAS in 100 ml = Z = = ............. M
100
VTUPulse.com
Sl.
No.
1
Volume of FAS
(V) ml
1
Concentration of Iron =
(V X a) mg/L
Transmittance
(t)
A = 2-log t
2 2
3 3
4 4
5 5
6 Test solution
(Y)
To determine ‘a’:
1000ml of 1M FAS = 55.85g of Iron
1ml of Z M FAS = a g of Iron = a g of iron
𝒁∗55.1
a= =.......................... mg
𝟏

 Result: Amount of iron in the given water sample = mg /L.
 Environmental significance:
 Iron content of the water is important in determining the suitability of water for domestic
and industrial purposes.
 Determination of iron is useful to select the treatment unit and design of treatment units
 The ratio of iron to manganese is a characteristic factor that determines the type of
treatment unit used as well as the amount of organic matter present in the water.
 It is also used to aid in the solution of problems in distribution systems where iron fixing
bacteria are troublesome.
 The iron determination is helpful in assessing the extent of corrosion and aiding in control
of corrosion.
 Outcome:
After performing the experiment, one can estimate the amount of iron present in given water
sample.
VTUPulse.com
 Viva Questions
1. How iron is removed from water?
2. Explain the significance of Fe in environmental engineering.

EXPERIMENT : DETERMINATION OF SODIUM BY FLAME

PHOTOMETER
Aim: Flame photometric estimation of sodium in the given water sample.

Objective: To conduct flame photometer test for determination of sodium present in given
water sample.
Apparatus: Flame Photometer, Compressor and 50ml Standard Flask.
Theory: When a solution containing the Metal ion is aspirated to flame a vapour of metal ion
is formed, which absorb heat energy and gets excited to higher energy level. The excited
metal ion returns back to its ground state by emitting the absorbed energy in the form of
radiation. The intensity of emitted radiation is directly proportional to the concentration of the
metal ion in solution.
 Procedure:
Fill the burette with given sodium chloride (Stock solution). Draw 5 of the solution
VTUPulse.com
into 50ml standard flask and make the solution upto the mark with distilled water and mix
well. Calibrate the instrument using the 10 ppm and 100 ppm standard solution prepared. The
readings of the unknown samples are obtained by aspirating solution to the flame. (Aspirate
distilled water between each run) Aspirate the given test solution into the flame and note
down the reading. Construct the calibration curve by plotting volume/concentration of
solution along x-axis and emission intensity along y-axis.
Using the graph identify the volume/concentration of sodium in given test solution

 Observations and calculations:
 Estimation of Na+
Weight of Na in the stock solution x = 10,000 ppm
Volume of Na given = VNa = ml
VNa
Weight of Na/100ml of the solution, a = X10000
100
VTUPulse.com

Volume of Wt of Na/50 ml Emission Response

Nacl = (VNacl * a)/50
Result:
 The given water sample contains……. mg of sodium
 Outcome:
After performing the experiment, one can validate the amount of sodium present in
givenwater sample
VTUPulse.com
 Viva Questions
1. Explain the principle involved in flame photometer.

2. What should be the permissible amount of sodium in water

EXPERIMENT : ELECTRICAL CONDUCTIVITY CONDUCTOMETRIC ,

DETERMINATION OF CHLORIDES
Aim: Conductometric determination of Chlorides.
Objective: To determine the amount of chlorides in a given water sample.
Apparatus: Conductivity meter, beakers, volumetric flask, Microburette.
Reagents: Silver Nitrate (AgNO3), Barium Chloride (BaCl2)
Theory:
Conductivity of water is a measure of its ability to conduct electric current and varies with
the number and type of ions present. It is expressed in specific conductivity, which is defined as
“the reciprocal of electrical resistance in ohm (), the unit is given in Siemens per cm (S.cm-1).
Water with high TDS level may have other water quality problems and / or may be unpleasant to
drink.
Chlorides: Natural water contains chloride in the form of NaCl, CaCl2 and other dissolved salts.
VTUPulse.com
Chlorides above 250 mg/L. give a salty taste to water and hence are not permitted. Otherwise
chlorides are not harmful. Presence of excessive chlorides in water also indicates possible
sewage combination. Chlorides salt of Calcium and Magnesium produces permanent hardness in
water. Excess chlorides can also corrode concrete by extracting calcium in the form of calcite.
 Procedure to find conductance of water

Rinse the conductivity electrode with deionized water and dip the electrode in 50 ml
given water sample. Record the conductivity of water in micro-Siemens (µS) /cm.
Preparation of standard acid or base:

Collect the stock water (note down the volume and concentration given) and make it up
to 50 ml using distilled water.
Conductometric determination of chlorides:

Fill the Std. AgNO3 solution into micro-burette. Transfer out 50 ml given water into clean 100
ml beaker. Immerse the conductivity cell and note down the initial Conductance, record the
change in conductance after subsequent addition of 0.5 ml of AgNO3. Plot a graph of volume of
AgNO3 in x-axis and conductance along y-axis Extrapolate the graph as shown in figure.

Using volume A calculate the amount of chloride present in the given water.
 Observation & Calculation:

Normality of Silver Nitrate = NAg =
Tabulation:
VTUPulse.com AgNO3,
VAg (cm3)
Determination of Chlorides
Conductance
(mili mhos)
AgNO3,
VAg (cm3)
Conductance
(mili mhos)
0.0 7.5
0.5 8.0
1.0 8.5
1.5 9.0
2.0 9.5
2.5 10.0
3.0 10.5
3.5 11.0
4.0 11.5
4.5 12.0
5.0 12.5
5.5 13.0
6.0 13.5
6.5 14.0
7.0 14.5

From graph, VAg =
 Chloride Calculation:
Volume of AgNO3 Consumed by given water sample = VAg =.......................... ml
V Ag ∗N Ag ∗Atomic wt of chlorine ∗1000

Chloride mg/L = = ............... mg/L
Volume of water sample
Atomic weight of chlorine = 35.5
 Result: Amount of Chloride in the given water sample = _ mg/L
 Outcome:
After performing the experiment one can validate the amount of chloride is in the permissible
range or not in a given water sample
VTUPulse.com
1. Define resistance.
2. State Ohm’s law.
3. Define conductance.
4. What is the unit of conductance?
5. Define conductivity.
6. Conductivity is maximum for which water?
7. Using conductivity cell we can measure which type of solution?
8. Conductivity experiment leads to a measurement of which type of solids?
9. What is the limit of chlorides in drinking water?
10. Chlorides can corrode which type of pipe?
11. What will be the chloride concentration in sewage water?
12. Explain the significance of high chloride in water.
13. What are the sources of chloride in water?
14. What are the methods of determination of chlorides?

ENV LAB - 18CVL67 - Manual

Uploaded by

Document Information

Original Description:

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

ENV LAB - 18CVL67 - Manual

Uploaded by

Copyright:

Available Formats

Environmental Engineering Laboratory

Subject Code : 18CVL67 I.A. Marks : 40

01. Determination of pH, Acidity and Alkalinity.

02. Determination of Calcium, Magnesium and Total Hardness.

03. Determination of Dissolved Oxygen.

04. Determination of BOD.

05. Determination of Chlorides

06. Determination of percentage of available chlorine in bleaching powder,

07. Determination of Residual Chlorine.

10. Determination of Optimum Dosage of Alum using Jar Test apparatus.

11. Determination of sodium and potassium by Flame Photometer.

12. Determination Nitrates by spectrophotometer.

13. Determination of Iron and Manganese.

14. Determination of COD ( Demonstration ).

Question paper pattern:

1. Two experiments shall be asked from the above set

ENVIRONMENTAL ENGINEERING LAB

Subject Code : 18CVL67 I.A. Marks : 40

Objectives: To determine Calcium, Magnesium and Total hardness of given water

QUESTION PAPER PATTERN:

One lab experiment to be conducted for 60 marks in 3 hours duration

Prerequisite: Environmental Engineering - I

Determination of pH, Acidity and Alkalinity.

Determination of Calcium, Magnesium and Total Hardness.

Determination of Dissolved Oxygen

Determination of Chlorides by Electrical conductivity,

Determination of Solids in Sewage: Total Solids, Suspended

Determination of Manganese by Spectrophotometer.

Determination of Sodium by Flame Photometer.

Determination of Potassium by Flame Photometer.

Determination of COD . ( Demonstration)

Experiment : Determination of Alkalinity, Acidity and pH

Aim: To conduct pH, acidity and alkalinity test on water.

Volume run down (ml)

Phenolphthalein endpoint = total acidity of water

Department of Civil Engineering, ATMECE

Methyl orange endpoint = total alkalinity of water

Total acidity of water sample = mg/L of CaCO3

Department of Civil Engineering, ATMECE

EXPERIMENT : CALCIUM, MAGNESIUM AND TOTAL HARDNESS

Aim: To conduct Hardness test on water.

Preparation of standard EDTA:

Department of Civil Engineering, ATMECE

(2) Determination Hardness due to Calcium

 Observation and calculation

Final Burette Reading (ml)

Initial Burette Reading (ml )

Volume of EDTA run down (ml)

Volume consumed VT = VCa =

 [Molecular mass of CaCO3 = 100]

Department of Civil Engineering, ATMECE

 [Atomic mass of Mg = 24.3]

Department of Civil Engineering, ATMECE

Department of Civil Engineering, ATMECE

Experiment : Determination of Percentage of Available Chlorine

Principle of iodometric method:

Department of Civil Engineering, ATMECE

Preparation of standard Sodium Thiosulphate solution:

Preparation of chlorine water from bleaching powder:

 OBSERVATIONS AND CALCULATIONS:

NS = Normality of Stock Sodium thiosulphate solution

Burette Standard Na2S2O3 solution