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FOREWORD
Global Academy of Technology strives to inculcate environmental consciousness among its
student community. This course- Environmental Engineering Laboratory (15CVL76) as prescribed by
VTU, Belagavi will aid in its fulfilment.
Environmental Engineering involves planning, design, construction and operation of
equipment, systems, and structures for the protection and enhancement of the environment. Although
traditionally a significant part of the Environmental Engineering encompassed water and waste water
collection, treatment and disposal to ensure sanitary living conditions for the public, in recent times, its
scope has grown abundantly covering additionally aspects of air pollution control, waste water
treatment/water pollution control, hazardous waste management, and solid waste management.
Environmental site assessments for property and environmental impact assessments for projects
and activities also form a significant part of the job of environmental engineers. Another concern
regarding the environment is, soil and groundwater contamination, which is being addressed by
Environmental engineers. Today, environmental engineers work on all the above subjects with more
intensive land and resource usage, along with cleaning up past pollution, and integrating with multi-
disciplinary teams to develop alternate energy sources, and more.
The current manual is prepared to equip students with information required to conduct
experiments necessary to analyse the quality of water and wastewater along with basic principles of the
working of experiment. The environmental significance of each parameter is incorporated for better
understanding of students.
The regulatory standards for drinking water as per World Health Organisation (WHO) and
Bureau of Indian Standards(BIS) is incorporated in the manual to train student in understanding the
standard requirements by the authorities and check the water’s compatibility for consumption or other
usage by comparing it with the prescribed Central Pollution Control Board (CPCB), BIS and WHO
standards. With this, the student will be able to apply the gained knowledge for the design of water and
waste water treatment units considering environmental and public protection.
The manual was prepared considering the guidelines given by CPCB and APHA standards, thus
ensuring the quality of the information given herewith.
Ms. Khushbu.K.Birawat
Assistant Professor
Mrs. Vidyashree D
Assistant Professor
M3. Inculcate ethical values and environmental consciousness through holistic education programs
MISSION
M1. Create a favourable environment for learning, teaching & continuous improvement for
implementation of various civil engineering facilities.
M2. Promote professionalism, innovation and research through collaboration with industries to
realize cost & resource effective, stable, quality structures.
M3. Inculcate environmental consciousness and ethical values through interconnected training
programs to ensure sustainability and client satisfaction.
The program educational objectives of Civil Engineering are to enable students in,
PEO-1: Developing careers in government and private civil engineering organizations and other
professionally related domains
PEO-2: Pursuing higher studies, and research to develop innovative solutions and technologies in
civil engineering and other multi disciplinary areas
PEO-3: Improving professional and personal traits aligned to professional ethics and environmental
compulsions
PEO-4: Professional leadership and Successful entrepreneurship
PSO-1: Comprehend, analyze and design alternatives for execution of civil engineering facilities
PSO-2: Apply Standard Codes of Practices and schedule of rates for planning, design, quality
control, estimating & costing of civil engineering projects.
PSO-3: Evaluate the buildings for resource conservation.
PROGRAM OUTCOMES-PO’s
Contents
FOREWORD ................................................................................................................................................... i
VISION OF THE INSTITUTE ....................................................................................................................ii
MISSION OF THE INSTITUTE.................................................................................................................ii
DEPARTMENT OF CIVIL ENGINEERING ................................................................................................ii
PROGRAM EDUCATIONAL OBJECTIVES-PEO’s ................................................................................. iii
PROGRAM SPECIFIC OUTCOMES-PSO’s .............................................................................................. iii
PROGRAM OUTCOMES-PO’s................................................................................................................... iii
GOVERNING REGULATIONS ..................................................................................................................vii
COURSE DETAILS ................................................................................................................................... viii
COURSE OUTCOMES .............................................................................................................................. viii
EVALUATION SCHEME (2015) .................................................................................................................. x
LABORATORY GUIDELINES.................................................................................................................... xi
EVALUATION SHEET ............................................................................................................................. xiii
IMPORTANCE OF ENVIRONMENTAL ENGINEERING LAB ............................................................. xiv
COLLECTION AND PRESERVATION OF SAMPLES ............................................................................ xv
GENERAL INFORMATION ...................................................................................................................... xix
QUALITY STANDARDS FOR MUNICIPAL OR DOMESTIC SUPPLIES ............................................. xx
WATER QUALITY CRITERIA AS PER CPCB NORMS ......................................................................... 24
WATER TREATMENT PLANT- FLOWCHART ...................................................................................... 25
WASTE WATER TREATMENT PLANT- FLOWCHART ....................................................................... 27
DETERMINATION OF pH OF WATER .................................................................................................... 30
DETERMINATION OF ACIDITY OF WATER ......................................................................................... 35
DETERMINATION OF ALKALINITY OF WATER ................................................................................. 40
DETERMINATION OF TEMPORARY HARDNESS, PERMANENT HARDNESS AND TOTAL
HARDNESS ................................................................................................................................................. 46
DETERMINATION OF DISSOLVED OXYGEN (DO) ............................................................................. 52
DETERMINATION OF BIOCHEMICAL OXYGEN DEMAND (BOD) .................................................. 56
DETERMINATION OF CHLORIDE CONTENT IN THE GIVEN SAMPLE........................................... 60
DETERMINATION OF PERCENTAGE OF AVAILABLE CHLORINE IN BLEACHING POWDER .. 63
TO DETERMINE THE RESIDUAL CHLORINE....................................................................................... 67
DETERMINATION OF SOLIDS ................................................................................................................ 71
DETERMINATION OF TURBIDITY OF A GIVEN SAMPLE ................................................................. 78
Department of Civil Engineering – 15CVL76 v
GLOBAL ACADEMY OF TECHNOLOGY
GOVERNING REGULATIONS
ATTENDANCE REQUIREMENT
Each semester is considered as a unit and the candidate has to put in a minimum attendance
of 85% in each subject with a provision of condonation of 10% of the attendance by the
Vice-Chancellor on the specific recommendation of the Principal of the college where the
candidate is studying, showing some reasonable cause such as medical grounds, participation
in University level sports, cultural activities, seminars, workshops and paper presentation,
etc.
The basis for the calculation of the attendance shall be the period prescribed by the
University by its calendar of events.
The students shall be informed about their attendance position periodically by the colleges so
that the students shall be cautioned to make up the shortage.
A candidate having shortage of attendance in one or more subjects shall have to repeat the
whole semester and such candidates shall not be permitted to take admission to next higher
semester. Such students shall take readmission to the same semester in the subsequent
academic year.
INTERNAL ASSESSMENT MARKS
There shall be a maximum of 20 Internal Assessment Marks in each practical papers, the IA
marks shall be based on the laboratory journals/reports and one practical test.
A candidate failing to secure a minimum of 50% of the IA marks (10/20) in Practical, 50%
of marks in project work, shall not be eligible for the practical / project in the University
examination. For a pass in a Practical/Project/Viva-voce examination, a candidate shall
secure a minimum of 40% of the maximum marks prescribed for the University Examination
in the relevant Practical/ Project/ Viva-voce.
COURSE DETAILS
Course Name : ENVIRONMENTAL ENGINEERING LABORATORY
Course Code : 15CVL76
Course Pre-requisite : Water supply and Treatment Engineering
COURSE OUTCOMES
Upon successful completion of this course, students will be able to
2 Conduction 56
3 Viva Voce 12
TOTAL 80
LABORATORY GUIDELINES
EVALUATION SHEET
Marks allotted
Page Faculty
SN Date Experiment Total
No. Conduction Record Viva Sign
(4) (4) (4)
1 Determination of pH
2 Determination of Acidity
3 Determination of Alkalinity
Determination of Calcium,
4
Magnesium and Total Hardness
5 Determination of DO
6 Determination of BOD
7 Determination of Chlorides
Determination of percentage of
8 available chlorine in bleaching
powder
Determination of Residual
9
Chlorine
Determination of Solids in
10
Sewage
11 Determination of Turbidity
Determination of Optimum
12
Dosage of Alum
13 Determination of sodium
14 Determination of potassium
15 Determination Nitrates
16 Determination of Iron
17 Determination of Manganese
18 Determination of COD
19 Air Quality Monitoring (Demo)
Determination of Sound by
20
Sound level meter (Demo)
Average (A) -12
Internal Assessment Marks (B) - 08
Total Marks (A + B) -20
Two hydrogen atoms and one oxygen atom forms a molecule of water. This pure water is
practically impossible to have in nature or in laboratory. The precipitation, at the instant of its
formation contains no impurities, but during its course of reaching earth through the atmosphere,
dissolves many gases, mineral traces and other substances. Once it reaches the earth’s surface, the
rain water may get physically, chemically or biologically contaminated.
The impurities which the water picks up or dissolves may render the water more useful and
potable for public uses or it may sometimes render it harmful and unfit for further use. For example,
certain minerals such as iron, calcium, magnesium, fluorine, etc., in small quantities may be useful
and good for health of the people. But, if the same and other materials are in large quantities or
different combinations, the water might become unfit or municipal or industrial use. For example,
water may contain pathogenic bacteria, which may cause diseases like cholera, typhoid, dysentery,
etc. Thus, to ensure safety to public, economy and utility in industries, it is essential to thoroughly
check, analyse, and treat the raw available water to safe and permissible limits, before supplying to
the public, used for irrigation or in industries.
The raw or treated water can be checked and analysed by studying and testing their physical,
chemical and biological characteristics. Thus, the experiments conducted in Environmental
engineering laboratory helps us in determining the contents of water and waste water and thereby
help us to decide on the degree of treatment required.
Experiments such as conductivity, determination of chlorides etc. can be used to determine
the type of desalination unit required which can be employed in coastal areas, where, there is acute
shortage of drinking water. Experiments such as determination of chlorides, sulphates, acidity,
alkalinity, pH value helps us determine whether the given water is suitable for human consumption.
Department of Civil Engineering – 15CVL76 xiv
GLOBAL ACADEMY OF TECHNOLOGY
The determination of hardness present in water is important in pharmaceutical and textile industries.
Determination of BOD is the one of the parameters that gives us an idea about the biodegradability
of any sample and the purification capacity of rivers and streams. The COD test is useful to assess
the strength of waste which contains toxins and biologically resistant organic substances.
The importance of each characteristic and its environmental significance is given in detail with the
experimental procedure.
To conclude, this laboratory provides us with the facilities required to assess the quality of
the raw and treated water and sewage, which is imperative to maintain the successful operation of
the treatment units along with safe supply of water to public and disposal into the environment.
SAMPLING:
SIGNIFICANCE OF SAMPLING:
The value of any laboratory analysis and tests depends upon the method of sampling.
Failure to observe proper precautions in securing a representative sample may result in an
analysis which is of little use since it may condemn good water or certify bad water as
satisfactory.
3. SORBENT SAMPLING:
Use of solid sorbents, particularly membrane-type disks, is becoming more frequent.
Rapid, inexpensive method, if the analytes can be adsorbed and desorbed efficiently and the
water matrix is free of particulates that plug the sorbent.
GENERAL INFORMATION
In water and wastewater analysis, the results are usually reported in terms of mg/L of a particular
ion, element or compound. It shall be convenient to have the standard titrating agent of such
strength, that 1mL is equivalent to 1mg of material being measured. Thus 1 litre of the standard
solution is usually equivalent to 1g of the standard substance.
Normality
The desired normality of the titrant is obtained by the relationship of 1 to the equivalent weight of
the measured material. Thus normality of acid solution to measure ammonia, ammonia nitrogen, and
alkalinity as CaCO3
The normality of silver nitrate to measure chloride and sodium chloride is:
Most materials subjected to the analysis of water and wastewater fall in the realm of dilute solutions
i.e., a few mg in a litre. So the results are normally expressed in mg/L or ppm. Parts per million
(ppm) is a weight ratio; but mg/L is a weight by volume ratio.
The relationship is given as follows:
If concentrations are less than 0.1 mg /L, express them in μg/L (micrograms per litre).
If concentrations are more than 10,000 mg/L, they are expressed in percentages.
Turbidity, NTU,
v)
Max 1 5 Part 10 —
Total dissolved
vi)
solids, mg/l, Max 500 2 000 Part 16 —
Sl Requirem
No. Characteristic ent Permissible Method of Test, Remarks
(Acceptabl
e Limit in the Ref to
Limit) Absence of
Alternate
Source
(1) (2) (3) (4) (5) (6)
Typical water treatment flowchart: Raw water from a surface water lake or reservoir is drawn into
the plant through intake structures. Large debris like logs is prevented from entering. Smaller debris
like fish, vegetation and garbage are removed from the raw water by protective bar and travelling
screens before the water enters the low lift pumps. These pumps lift the water to flow through the
treatment processes by gravity. First, pre-oxidation and primary disinfection is done, where
Disinfectants or other oxidants are added to disinfect or control tastes and odours. The specific
processes used are determined by the chemical and biological raw water characteristics. Next during
coagulation, coagulants, rapidly add electrochemical charges that attract the small particles in water to
clump together as a “floc”. This initial charge neutralization process allows the formed floc to
agglomerate but remain suspended. During flocculation, by slower mixing, turbulence causes the
flocculated water to form larger floc particles that become cohesive and increase in mass. This visible
floc is kept in suspension until large enough to settle under the influence of gravity.
The selection of unit operations and unit processes for the treatment of sewage depends on
several factors such as characteristics of raw sewage, degree of purification required, disposal
facilities available, cost involved including cost of installation, maintenance and operation, ease of
construction and maintenance, benefits derived from better environmental sanitation, location,
availability of land and topographical conditions.
Typically, there are four stages of sewage treatment:
1. Sewage treatment begins with preliminary treatment, which involves removal of floating
material, settleable inorganic solids like sand and oily substances like grease. Equipments like
screens, grit chambers and skimming tanks are used to aid in removal of above impurities.
2. In the next stage, primary treatment is aimed at the removal of fine suspended organic solids that
cannot be removed in the preliminary treatment. Primary treatment basically involves the process of
sedimentation or settling. In the normal process of sewage treatment, sedimentation is usually carried
out twice- once before the secondary treatment, referred to as primary sedimentation, and then after
The most important suspended-growth biological treatment systems used for the removal of organic
matter are:
1. Activated sludge process
2. Aerated lagoons
3. Sequencing batch reactor
4. Aerobic digestion.
Among these, activated sludge process is the most widely used for the secondary treatment of
sewage.
The commonly used attached-growth processes are listed:
1. Trickling filters
2. Roughing filters
3. Rotating biological contractors
4. Packed bed reactors.
Among these, trickling filter is most widely used.
4. Next, tertiary treatment or advanced treatment is sometimes needed for the removal of suspended
and dissolved substances, after the conventional primary and secondary treatments. In general, the
effluent of the sewage obtained after secondary treatment can be conveniently disposed without
causing any nuisance.
However, tertiary treatment is needed under the following circumstances:
1. When the quality of the effluent to be discharged does not meet the standard requirements.
2. When there is a necessity to reuse the sewage/ waste water (reclamation of water is quite
expensive, but is required in certain situations of water shortage).
3. For the removal of nitrogen and phosphorus compounds.
Tertiary treatment process broadly involves the removal of suspended and dissolved solids, nitrogen,
phosphorus and pathogenic organisms.
With this brief understanding on water and waste water treatment plant, let us start with the
experiments essential for analysing the quality of water/ wastewater.
DETERMINATION OF pH OF WATER
Aim: To determine the pH of the given sample of water using 1) pH paper, and 2) digital pH meter.
Introduction:
pH is the term used to express the acidic or alkaline condition of a solution. It expresses
hydrogen-ion concentration in water and concept of pH was put forward by Sorenson (1909). Acids
and bases were originally distinguished by their difference in taste and later by the manner in which
they affected certain materials that came to be known as indicators. With the discovery of hydrogen,
it soon became apparent that all acids contained the element hydrogen. Chemists found that
neutralization reactions between acids and bases always produced water. From this and other related
information, it was concluded that bases contained hydroxyl groups.
In 1887, Arrhenius announced his theory of ionization. Since that time acids have been considered to
be substances that dissociate to yield hydrogen ions or protons, and bases have been considered to be
substances that dissociate to yield hydroxide ions (also called hydroxyl ions). According to the
concepts of Arrhenius, strong acids and bases are highly ionized and weak acids and bases are poorly
ionized in aqueous solution.
The pure water dissociates to yield a concentration of hydrogen ions equal to about 10–7 mol/l.
H2O H+ + OH–
The amount of hydroxyl ions is equal to the hydrogen ions, so 10–7 mol of hydroxyl ion is produced
simultaneously. The equilibrium equation gives
{H+} {OH–}/H2O = K
As the concentration of water is so extremely large and is diminished so much little by the slight
degree of ionization it may be considered as constant and the above equation can be written as:
{H+} {OH–} = Kw
For pure water at 25oC,
{H+} {OH–} = 10–7 × 10–7 = 10–14
This is known as the ion product or ionization constant for water. When an acid is mixed in water it
ionizes in the water and the H+ ion activity increases. Consequently the OH- ion activity must
decrease according to the ionization constant.
For example, if acid is added to increase the {H+} to 10–2, the {OH–} must decrease to 10–12
10–2 × 10–12 = 10–14
Similarly if a base is added to increase the {OH–} to 10–3, the {H+} decreases to 10–11. However the
{H+} or the {OH–} can never be reduced to zero no matter how basic or acidic the solution may be.
Designating the hydrogen ion concentration in terms of molar concentration is cumbersome and to
overcome this difficulty, Sorenson gave such value in terms of their negative logarithms as pH. So,
pH = – log {H+}
Or pH = log 1/ {H+}
The pH scale is represented as ranging from 0 to 14 with pH 7 at 25oC designating absolute
neutrality. pH lesser than 7 is acidic and more than 7 is a basic solution. pH is used in the calculation
of carbonate, bicarbonate and CO2, corrosion and stability index etc. While the alkalinity or acidity
measures the total resistance to the pH change or buffering capacity, the pH gives the hydrogen ion
activity.
Principle:
1) Using pH Papers
Results:
Discussion:
Environmental Significance:
Questions:
1. pH is defined as
(i) Logarithm of Hydrogen ions (ii) Negative logarithm of Hydrogen ions
(iii) Hydrogen ion concentration (iv) OH ion concentration
2. For pure water at 25°C, the product of H+ and OH– ions is
(i) 10–7 (ii) 10–14 (iii) 10 (iv) 107
3. The acceptable value of pH of potable water is
(i) 7.0 to 8.5 (ii) 6.5 to 9.5 (iii) 6 to 8.5 (iv) 6.5 to 10
4. The alum is most effective as a coagulant in the pH range of
(i) 6.5 to 8.5 (ii) 6 to 9.0 (iii) 6.5 to 9.5 (iv) 7.0 to 7.5
5. Discuss the relationship between (a) pH and hydrogen ion concentration (b) pH and hydroxide
ion concentration?
6. A decrease in pH of 1 unit represents how much of an increase in hydrogen ion concentration?
7. Why is it necessary to maintain the pH of water nearly 7?
8. What is a buffer solution? Give examples.
Marks Obtained:
B. Phenolphthalein acidity:
1. Take 25 ml of the given sample in a conical flask.
2. Add few drops of phenolphthalein indicator.
3. If the solution turns to pink in colour, it indicates that acidity is absent in the sample.
Department of Civil Engineering – 15CVL76 Page 36
GLOBAL ACADEMY OF TECHNOLOGY
4. If the solution does not give any colour (i.e. acidity is present), titrate with 0.02 N NaOH till
the solution turns pink, indicating end point.
5. Record the volume of titrant consumed in ml.
Observation:
Description of Initial Burette Final Burette Volume of 0.02N
SN Experiment
sample(volume) reading Reading NaOH used
Methyl Orange
1.
acidity
Phenolphthalein
2.
acidity
Calculation:
Where,
V = mL of NaOH titrant consumed
N = Normality of NaOH
Result:
1. Methyl Orange Acidity in mg/L as CaCO3 = ………………………
2. Phenolphthalein acidity in mg/L as CaCO3 = ………………………….
Discussion:
Environmental Significance:
Acids contribute to corrosiveness and influence chemical reaction rates, chemical speciation and
biological processes.
Acid waters are of concern because of their corrosive characteristics and the expense involved in
removing or controlling the corrosion-producing substances. The corrosive factor in most waters
is carbon dioxide, but in many industrial wastes it is mineral acidity.
Where biological processes of treatment are used, the pH must ordinarily be maintained within
the range of 6 to 9.5. This criterion often requires adjustment of pH to favourable levels, and
calculation of the amount of chemicals needed is based upon acidity values in most cases.
Carbon dioxide determinations are particularly important in the field of public water supplies. In
the development of new supplies, it is an important factor that must be considered in the
treatment method and the facilities needed.
Many underground supplies require treatment to overcome corrosive characteristics resulting
from carbon dioxide. The amount present is an important factor in determining whether removal
by aeration or simple neutralization with lime or sodium hydroxide will be chosen as the
treatment method. The size of equipment, chemical requirements, storage space, and cost of
treatment all depend upon the amounts of carbon dioxide present.
Carbon dioxide is an important consideration in estimating the chemical requirements for lime or
lime-soda ash softening.
Most industrial wastes containing mineral acidity must be neutralized before they may be
discharged to rivers or sewers or subjected to treatment of any kind. Quantities of chemicals,
size of chemical feeders, storage space, and costs are determined from laboratory data on acidity.
Questions:
1. Acidity of water means
a. pH of water in acidic range
b. pH of water in alkaline range
c. base neutralizing capacity of water
d. acid neutralizing capacity of water
Marks Obtained:
Procedure:
Phenolphthalein Alkalinity:
1. Take 25ml of sample in a conical flask.
2. Add 3-4 drops of phenolphthalein indicator. If the pH of sample is above 8.3, sample turns
pink.
3. Titrate with 0.02 N H2SO4 in a burette till the colour disappears.
4. Note down the volume of H2SO4 added (V1)
Total Alkalinity:
1. Take 25ml of sample in a conical flask.
2. Add 3-4 drops of Methyl orange indicator. The sample turns yellow.
3. Titrate it against 0.02N H2SO4 till the colour of the sample turns orange.
4. Note down the total volume of H2SO4 added (V2)
Observation:
Phenolphthalein
1.
alkalinity
2. Total Alkalinity
Calculation:
Where,
V = mL of H2SO4 titrant consumed
N = Normality of H2SO4
The types of alkalinities present in the samples are calculated using the equations given in the
following table and the results are tabulated.
Environmental Significance:
Highly alkaline water in usually unpalatable and the consumer tends to seek other supply.
Chemically treated water sometimes has rather high pH values which have met with some
objection by consumers.
Large amounts of alkalinity impacts bitter tastes to water.
Chemicals used for coagulation of water and wastewater react with water to form insoluble
hydroxide precipitates. The hydrogen ions released react with the alkalinity of the water. Thus,
the alkalinity acts to buffer the water in a pH range where the coagulant can be effective.
Alkalinity must be present in excess of that destroyed by the acid released by the coagulant for
effective and complete coagulation to occur.
Water softening: To find out quantity of lime and soda ash required for the removal of hardness,
alkalinity should be computed.
Alkalinity aids in corrosion control.
Buffer Capacity: | Alkalinity measurements are made as a means of evaluating the buffering
capacity of wastewaters and sludges. They can also be used to assess a natural water’s ability to
resist the effects of acid rain.
Influence of waste water: waste water containing excess caustic (hydroxide) alkalinity is not to
be discharged into natural water bodies or sewers. Excess alkalinity in water is harmful for
irrigation which reduces crop yield. Alkalinity less than 250 mg/L is desirable for domestic
consumption and RCC Works.
Questions:
1. What is meant by alkalinity in water and waste water.
2. 2000ml of a sample of water required 20 ml of N/50 H2SO4 using methyl orange as indicator but
did not produce any coloration with phenolphthalein. What type of alkalinity is present in the
sample?
3. What effect does the addition of carbon dioxide have on the total alkalinity of water?
4. On analysis, a series of samples was found to have the following pH values: 5.5,3.0, 11.2, 8.5,
7.4, and 9.0. What can you conclude regarding the possible presence of a significant bicarbonate,
carbonate, or hydroxide alkalinity in each sample?
5. What causes alkalinity in water?
6. At what pH range alkalinity is present in water?
7. How alkalinity is removed from water?
8. What is the permissible limit of alkalinity in drinking water?
9. Which is the major form of alkalinity? How is it formed?
10. What is excess alkalinity? How do you express it?
11. Why do we take 0.02 N H2SO4 for the titration?
12. Calculate the Phenolphthalein and total alkalinities of the following samples: (a) A 50-mL
sample required 5.3 mL 0.020 N H2S04 to reach the Phenolphthalein end point and a total of 15.2
mL to reach the methyl orange end point. (b) A 100-mL sample required 20.2 mL of 0.020 N
H2S04 to reach the Phenolphthalein end point and a total of 25.6 mL to reach the methyl orange
end point.
13. The water where algae are flourishing is alkaline. Why? Will there be diurnal variation in pH?
14. Why does the pH change on aerating the water?
15. For efficient coagulation the water must be alkaline. Why?
Marks Obtained:
Hardness test of water is important in determining suitability of water for domestic and industrial
use. Also the determination of hardness serves as a basis for finding the most economical method
of softening water.
Principle:
When the hardness is numerically greater than the sum of the carbonate alkalinity and the
bicarbonate alkalinity, the amount of hardness, which is equivalent to the total alkalinity, is called
carbonate hardness; the amount of hardness in excess of this is called non-carbonate hardness.
When the hardness is numerically equal to or less than the sum of carbonate and bicarbonate
alkalinity all of the hardness is carbonate hardness and there is no noncarbonate hardness. The
hardness may range from zero to hundreds of milligrams per litre in terms of calcium carbonate,
depending on the source and treatment to which the water has been subjected.
Ethylenediamine tetra-acetic acid and its sodium salts (EDTA) form a chelated soluble
complex when added to a solution of certain metal cations. If a small amount of a dye such as
Eriochrome black T is added to an aqueous solution containing calcium and magnesium ions at a pH
of 10 ± 0.1, the solution will become wine red. Then when the solution is titrated against EDTA, it
forms complex with the calcium and magnesium ions. After sufficient EDTA has been added to
complex all the magnesium and calcium, the solution will turn back from wine red to blue. This is
the end point of the titration.
Reagents:
1. Hardness Buffer Solution
2. Eriochrome Black T indicator
3. Standard EDTA Solution 0.01M
Apparatus:
1. Burette; 2. Pipette; 3. Conical Flask
Procedure:
1. Take 25 ml sample in a conical flask.
2. Add 1 ml of Hardness buffer solution.
3. Add 2-3 drops of Eriochrome Black T indicator. Wine red colour is observed.
4. Titrate with standard EDTA solution till wine red colour changes to blue.
5. Note down the volume of EDTA run down (A)
Observations:
Total Hardness:
Description of Initial Burette Final Burette
SN Volume of EDTA (mL)
sample(volume) reading Reading
Calculations:
Permanent Hardness:
Calculations:
Calcium as mg/L =
Calcium = ………………
Results:
1. Total hardness = ………………….mg/L as CaCO3
2. Permanent hardness = …………….. mg/L as CaCO3
3. Temporary hardness = ...…………. mg/L as CaCO3
4. Calcium Hardness = ………………. mg/L as CaCO3
5. Magnesium Hardness = ………………. mg/L as CaCO3
6. Calcium = ………..mg/L
7. Magnesium = ………..mg/L
Discussion:
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.
Magnesium hardness (associated with sulphate ions) has a laxative effect on persons
unaccustomed to it.
Makes food tasteless.
Questions:
1. What is degree of hardness? How will you classify water in terms of degree of hardness?
2. What is pseudo-hardness?
3. Explain the significance of determination of hardness of water in environmental engineering.
4. How can you remove permanent hardness from water?
5. Can you determine temporary hardness and permanent hardness separately? If yes, how?
6. What are the principal cations causing hardness in water and the major anions associated
with them?
7. How is hardness classified?
8. Why is softening of water necessary? What are the advantages of soft water?
9. Among finished drinking water, raw wastewater and de-ionized water, which water is
expected to have the highest carbonate hardness and why?
10. A sample has 50mg/L Ca2+,150mg/L Mg2+, 50 mg/L Na+, 20 mg/L Cl- and 100 mg/L
glucose. Calculate its total hardness, carbonate and non-carbonate hardness?
11. Define hardness with respect to water.
12. What are the constituents that cause hardness in water?
13. How do you classify the water based on hardness in water?
14. Which method is the best for hardness determination in water and why?
Marks Obtained:
Introduction:
Dissolved Oxygen (D.O.) levels in natural and wastewaters are dependent on the physical, chemical
and biochemical activities prevailing in the water body. The analysis of D.O. is a key test in water pollution
control activities and waste treatment process control.
The presence of oxygen is essential for the survival of aquatic life in water. This oxygen is especially
required by aerobic bacteria and other micro-organisms for degradation and stabilization of organic
constituents in waste water. A rapid fall in DO level in river water is one of the first indications of organic
pollution. Thus it is one of the important parameters for accessing the quality of water, water bodies and
plays a key role in water pollution control activities.
The major inputs of DO to natural water are from atmosphere and photosynthetic reaction. The
solubility to oxygen in water depends on pressure, temperature, altitude and chloride concentration etc.
The solubility of atmosphere oxygen in fresh water varies from 14.6 mg/lt at 0 o C to about 7 mg/lt at
35o C under 1 atmospheric pressure. Low DO in water can kill fish and many other organisms in water. For
example, fish requires 2 mg/lt to 5 mg/lt of DO in water.
Principle:
Improved by various techniques and equipment and aided by instrumentation, the Winkler
(iodometric) test remains the most precise and reliable titrimetric procedure for D.O. analysis. The test is
based on the addition of divalent manganese solution, followed by strong alkali to the water sample in a
glass-stoppered bottle. D.O. present in the sample rapidly oxidises in equivalent amount of the dispersed
divalent manganous hydroxide precipitate to hydroxides of higher valency states. In the presence of iodide
ions and upon acidification, the oxidised manganese reverts to the divalent state, with the liberation of
iodine equivalent to the original D.O. content in the sample. The iodine is then titrated with a standard
solution of thiosulphate.
Apparatus:
1. BOD Bottle- 300 ml Capacity; 2. Conical Flask; 3. Burette; 4. Measuring Jars
Reagents:
1. Manganous Sulphate
Department of Civil Engineering – 15CVL76 Page 52
GLOBAL ACADEMY OF TECHNOLOGY
2. Alkali Iodide-Azide Solution
3. Starch Indictor
4. Standard Sodium Thio Sulphate (0.025 N)
5. Concentrated Sulphuric Acid
Results:
Discussion:
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. For example the maximum D.O at 20 oC
is 9.17 mg/l where as at 25oC it is 8.38 mg/l. A minimum of 4 mg/L D.O is essential for the aquatic life.
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 D.O ) 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. So it is necessary to find out the D.O of water to maintain sanitary
conditions. It can be achieved by the treatment of waste water. Treatment means the reduction of BOD
below the allowable limits. The limit is 30 mg/l for disposal of wastewater (sewage) in water.
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.
Algae group in water may release oxygen during its photosynthesis and DO may even shoot up to 300
mg/lt.
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 necessary for all aerobic biological waste treatment process to control rate of aeration.
DO test is used to evaluate the pollution strength of industrial and domestic waste.
Questions:
1. The concentration of Dissolved Oxygen in water is mainly dependent on
1. The temperature
2. Chloride concentration
Marks Obtained:
OF WASTE WATER
Aim: To determine the amount of BOD (Biochemical Oxygen Demand) exerted by a given sample of waste
water.
Introduction:
The Biochemical Oxygen Demand (B.O.D.) of sewage or of polluted water is the amount of oxygen
required for the biological decomposition of dissolved organic matter to occur under aerobic condition and
at the standardised time and temperature. Usually, the time is taken as 5 days and the temperature 20°C as
per the global standard. The B.O.D. test is among the most important method in sanitary analysis to
determine the polluting power, or strength of sewage, industrial wastes or polluted water. It serves as a
measure of the amount of clean diluting water required for the successful disposal of sewage by dilution.
The test has its widest application in measuring waste loading to treatment plants and in evaluating the
efficiency of such treatment systems.
Principle:
The test consists in taking the given sample in suitable concentrations in dilute water in B.O.D. bottles.
Two bottles are taken for each concentration and three concentrations are used for each sample. One set of
bottles is incubated in a B.O.D. incubator for 5 days at 20°C; the dissolved oxygen (initial) content (D1) in the
other set of bottles will be determined immediately. At the end of 5 days, the dissolved oxygen content (D2) in
the incubated set of bottles is determined.
Then, mg/L B.O.D. =
2. Manganous Sulphate
3. Alkali- Iodide- Azide Solution
4. Concentrated Sulphuric Acid
5. Starch Indicator
6. Phosphate Buffer Solution
7. Magnesium Sulphate Solution
8. Ferric Chloride Solution
9. Calcium Chloride Solution
Procedure:
1. Preparation of aerated distilled water: Place desired volume of distilled water in a 5 litre flask. Aeration
is done by bubbling compressed air through water.
2. Add 1 ml each of phosphate buffer, magnesium sulphate solution, calcium chloride solution and ferric
chloride solution for every litre of distilled water.
3. In the case of waste water which is not expected to have sufficient bacterial population, add seed to the
diluted water. Generally 2 ml of settled domestic sewage is sufficient for 1000 ml of dilution water.
4. Highly acidic or alkaline sample are to be neutralized to a pH of 7.
5. Take the sample and dilute it with distilled water and mix contents well.
6. Take diluted sample into 2 BOD bottles.
7. Fill the other two BOD bottles with dilution water alone.
8. Find DO of diluted waste water and dilution water and note them down.
9. Incubate the other two BOD bottles in a BOD Incubator for 5 days at 200C. They are to be tightly
stoppered to prevent any air entry into the bottles.
10. Determine DO content in the incubated bottles at the end of 5 days.
11. Calculate the B.O.D. of the given sample.
Note: The procedure for determining the dissolved oxygen content is same as described in the experiment
under “Determination of dissolved oxygen”.
Sample
IBR FBR VR (DO)0 IBR FBR VR (DO)5
Sewage sample
Blank solution
Calculations:
Where:
DO = DO of diluted wastewater sample on 0th day
D5 = DO of diluted waste water sample on 5th day
BO = DO of blank solution before incubation
B5 = DO of blank solution after incubation of 5 days
Results:
The BOD of sample is ________________mg/L
Discussion:
Environmental Significance:
The most widely used test indicating organic pollution of both wastewater and surface water is the
5-day BOD (BOD5). This determination involves the measurement of the dissolved oxygen used by
microorganisms in the biochemical oxidation of organic matter. BOD5 is the total amount of
oxygen consumed by microorganisms during the first five days of biodegradation. Oxygen demand
is associated with the biodegradation of the carbonaceous portion of wastes and oxidation of
Marks Obtained:
Signature of Course Co-ordinator
Principle:
In neutral or slightly alkaline water potassium chromate can indicate the end point of the silver
nitrate. Silver chloride precipitated quantitatively before red silver chromate precipitate is formed.
Apparatus:
1. Burette; 2. Pipette; 3. Conical flask
Reagents:
1. Chloride free distilled water
2. Potassium chromate indicator.
3. Standard silver nitrate (0.0141N)
4. Standard sodium chloride (0.0141N)
Procedure:
1. Take 25ml of sample in conical flask.
2. Adjust its pH between 7.0 and 8.0 either with sulphuric acid or sodium hydroxide solution.
Otherwise AgOH is formed at high pH level.
3. Add 1ml of potassium chromate to get light yellow colour.
4. Titrate with standard silver nitrate solution till colour change from yellow to brick red.
5. Note down the volume of silver nitrate added (A).
6. If more quantity of potassium chromate is added, silver chromate may form too soon or not soon
enough.
7. For better accuracy, titrate distilled water in the same manner.
8. Note the volume of silver nitrate added for distilled water (B).
Observation:
Burette: 0.0141N silver nitrate solution
Conical flask: 25ml of sample
Indicator: Potassium chromate
End Point: Yellow to Brick red
A=
Blank solution
B=
Calculations:
Result:
Chloride content of the given sample is = ………………………… mg/lt
Discussion:
Environmental significance:
Chlorides determination in natural waters is useful in the selection of water supplies for human use.
Chlorides determination is used to determine the type of desalting apparatus to be used.
The chloride determination is used to control pumping of ground water from locations where intrusion
of sea water is a problem.
Questions:
1. What is the need to adjust the pH of the sample to 7-8 in chlorides estimation?
2. What is the effect of temperature in the determination of chlorides?
3. What is meant by indicator blank correction?
4. What process is to be used to remove excess chlorides in water?
Marks Obtained:
Signature of Course Co-ordinator
Reagents:
1. Standard sodium thiosulphate solution (0.025N)
2. Potassium iodide
3. Starch indicator
4. Iodine solution (0.025 N).
5. Glacial Acetic Acid
Procedure:
1. 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.
2. Place 5 mL glacial acetic acid in an Erlenmeyer flask and add about 1g potassium iodide
crystals. Pour 25 mL of bleaching powder solution prepared above and mix with a stirring rod.
Wait for 15 to 20 minutes.
Department of Civil Engineering – 15CVL76 Page 63
GLOBAL ACADEMY OF TECHNOLOGY
3. Titrate with 0.025N Sodium Thio-Sulphate solution until a pale yellow colour is obtained. (Deep
yellow changes to pale yellow.)
4. Add 1 mL of starch solution. The solution becomes blue in colour.
5. Continue the titration till the blue colour disappears. Note down the volume of sodium Thio-
Sulphate run down(V1).
6. Take a volume of distilled water corresponding to the sample used.
7. Add 5 mL acetic acid, 1g potassium iodide and 1 mL starch solution.
8. If blue colour occurs, titrate with 0.025 N sodium thiosulphate solution until the blue colour
disappears.
9. Record the volume of sodium thiosulphate solution added (A1).
10. If no blue colour occurs, titrate with 0.025 N iodine solution until a blue colour appears. Note
down the volume of iodine (A2).
11. Then, titrate with 0.025 N sodium thiosulphate solution till the blue colour disappears. Record
the volume of sodium thiosulphate solution added (A3). Note down the difference between the
volume of iodine solution and sodium thiosulphate as A4(A4=A2 – A3).
Note: Blank titration is necessary to take care of the oxidising or reducing reagents’ impurities.
Observations:
Volume
Initial Burette Final Burette
Trial No. Sample Rundown
Reading (IBR) Reading (FBR)
VR =FBR - IBR
2. Distilled water
Volume
Initial Burette Final Burette
Trial No. Sample Rundown
Reading (IBR) Reading (FBR)
V =FBR - IBR
Calculations:
Results:
The available chlorine content in the given bleaching powder sample is = ………….mg /L
Percentage of chlorine available in bleaching powder = ____________
Discussion:
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.
Marks Obtained:
Signature of Course Co-ordinator:
Principle:
Chlorine present in water reacts with potassium iodide and iodine is liberated. When starch is used as
indicator, the presence of blue colour indicates the presence of iodine.
Apparatus:
1. Burette; 2. Pipette; 3. Conical flask; 4. Beaker
Procedure:
1. Take 6 beakers with increasing dosage of standard chlorine solution. Add 100ml of Tap water to each
beaker and mix well.
2. To this add 5ml of glacial acetic acid and pinch of potassium iodide and place it aside for 10 minutes.
3. Titrate the solution from each beaker against 0.025 N Sodium Thio-sulphate to pale yellow colour, by
adding add 1 ml of starch solution until the solution turns from blue to colourless.
4. Note down the burette reading and calculate the amount of residual chlorine present.
Observation:
1 5
2 10
3 15
4 20
5 25
6 30
Calculations:
Where,
VR= Volume of Sodium thio-sulphate Run-down
N = Normality of sodium thio-sulphate.
Results:
The residual chlorine present in the sample = ……………………… mg/lt
Discussion:
Environmental Significance:
1. The chlorination of water supplies and polluted waters serves primarily to destroy or
deactivate disease-producing micro-organisms. A secondary benefit, particularly in treating
drinking water, is the overall improvement in water quality resulting from the reaction of chlorine
with ammonia, iron, manganese, Sulphide and some organic substances.
2. Determination of residual chlorine is used to control chlorination of domestic and industrial
waste water.
3. Determination of chlorine residual is used universally in disinfection practice to control the
chlorine so as to ensure effective disinfection without waste.
4. Determination of chlorine residual in water distribution is useful to find the source of
contamination or leakage point so as to supply wholesome water to consumer.
5. Residual chlorine should be present in drinking water within range of 0.1 to 0.2 mg/ltr.
However excess chlorine content may give out bad odour and may change even taste of water.
6. Excess chlorine is said to be carcinogenic.
7. Residual chlorine should be present in the drinking water within range of 0.1 to 0.2mg/ltr.
However excess chlorine content may give out bad odour and may changes even taste of water.
8. Excess chlorine is said to be carcinogenic.
Questions:
1. What is chlorination?
2. Explain the reactions occurring during chlorination while disinfection of water.
Marks Obtained:
Signature of Course Co-ordinator:
DETERMINATION OF SOLIDS
Aim: To determine the total solids, fixed solids, volatile solids, settleable solids, suspended solids,
and dissolved in a given sample.
Introduction:
Normally the sewage water sample contains 99.9 % water and 0.1% solids. The term solids in
water and waste water for a sanitary engineer refers to as the matter which remains as a residue after
evaporation and subsequent drying at specified temperature of 100 to 105o C. the total solids is
considered as the sum of dissolved solids and suspended solids.
1) Total Solids: They indicate both organic and inorganic matter. Organic solids are also called
as volatile solids and inorganic solids are also called non-volatile solids.
2) Suspended Solids: These are of two types: settleable and non-settleable solids. Settleable
solids are those which will settle down in the sedimentation tank with a usual detention
period of 1 to 3 hours. Non-settleable solids will not settle down and are usually volatile in
nature.
3) Dissolved Solids: They are present in dissolved state and can be determined indirectly.
4) Fixed Solids: The residue obtained in total solids test is heated to 550 ± 50o C in a muffle
furnace at a constant rate for about 1 hour. The volatile solid vaporizes and the residue that
remains is the fixes solids.
Apparatus:
6. Evaporating Dish (Gooch Crucible); 2. Oven (103o C); 3. Muffle Furnace (550 ± 50o C);
4. Weighing Balance
1. Take a clean crucible and make it completely dry in oven, cool it and take its initial weight as
W1
1. The crucible which contains total solids will be used in this experiment.
2. Place the crucible in a muffle furnace at 550 ± 50o C for 15 to 20 minutes.(At 550 ± 50o C
all the volatile matter will burn out leaving behind only fixed solids or inorganic solids)
3. Allow the dish to cool and note down the weight as W3.
3. Place the dish along with the filtrate in an oven at 100 to 103o C and evaporate the filtrate
sample. (Under any circumstance the sample should not be boiled).
Apparatus:
Procedure:
1. Mix thoroughly the given waste water sample
2. Place the Imhoff Cone on the stand
3. Pour the thoroughly mixed sample into the imhoff cone upto 1 Ltr Mark.
4. Gently Stir the sides of the cone with a rod or by spinning.
5. Allow the sample to settle at least for 45 to 60 minutes.
6. At the end of 45 minutes note down the settleable solids in cone in ml/ltr.
Observations:
Total Solids
W2 = Weight of gooch crucible + water sample (after Oven dry 103- 105o C) =
………………… mg
= ………………………….. mg/lt
Fixed Solids
= ………………………………… mg
= ……………………………… mg/lt
= …………………………. mg/lt
Suspended Solids
= ………………………………..mg/lt
Dissolved Solids
=……………………………mg/lt
Results:
Total solids of waste water sample = ………………………….. mg/lt
Discussion:
Environmental Significance:
1. The suspended solids parameter is used to measure the quality of waste water influent and
effluent and also extremely valuable in analysis of polluter water.
2. It is used to evaluate strength of the domestic waste water.
3. Dissolved substances are undesirable in water. Dissolved Minerals, gasses and organic
constituents may produce aesthetically displeasing color, taste and odor.
4. Some dissolved organic chemicals may deplete the dissolved oxygen in receiving water and
some may also be carcinogenic.
5. Water with higher solid continent often has a Laxative effect and sometimes the reverse
effect on people whose bodies are not adjusted to them.
6. High concentration of dissolved solid of about 3000 mg/lt may also produce distress and
livestock. In industries the use of water with high amount of dissolved solids may lead to
scaling in boilers, corrosion and degraded quality of product.
7. Water consisting of high volatile solids is not suitable for drinking purpose. It indicates that
the water may have been polluted by domestic wastes and other organic waste. In general
groundwater is free from volatile Solids. Surface water may have high volatile solids due to
disposal of domestic and other wastes.
10. Biologically active suspended solids may include disease causing organisms as well as
organisms such as toxin producing algae.
Questions:
Marks Obtained:
Signature of Course Co-ordinator:
Nephlometric turbidity meter is generally used for samples with low turbidity and expressed as
NTU or mg/ltr. For portable water allowable turbidity is between 5 to 10 mg/ltr.
Apparatus:
1. Nephlo turbidity meter; 2. Sample Tubes
Procedure:
1. Switch on the instrument and allow sufficient warm-up period.
2. Take distilled water or bank solution in the test tube holder and close the lid. Make sure that
the mark on the test tube coincides with mark on the panel.
3. Select required range for measurement.
4. Adjust the displayed to ‘000’ by adjusting set zero knob.
5. Remove the test tube containing distilled water and insert another test tube containing standard
solution (say 100 NTU or 400 NTU). Place it in test tube holder.
6. Adjust the calibrate knob so that the display reach the standard solution value.
7. Again check ‘0’ display with distilled water. The instrument is now calibrated.
Observations:
Results:
The turbidity of the given sample is = ……………… NTU
Discussion:
Environmental Significance:
1. Turbidity is objectionable because of aesthetic and engineering considerations.
Questions:
1. What are the causes of turbidity in water?
2. What units are used for measuring turbidity?
3. What is the difference between visual method and instrumental method in turbidity
measurement?
4. What is meant by coefficient of fineness? Mention its importance.
5. What is the basic difference in principle involved in Jackson turbid meter and
Nephelo turbidity meter?
6. What is the general coagulant used for removal of turbidity in water?
Marks Obtained:
Signature of Course Co-ordinator:
Reagents:
1. Alum Solution
2. H2SO4
Procedure:
1. Take 6 beakers containing 1 ltr of sample
2. Check the initial pH, turbidity, alkalinity of the given sample. If pH is low add soda ash or
lime make up the pH between 6.5 - 8.5.
3. Add the coagulant alum for the beakers in increasing order.
4. With the help of flash mixer go for the process of coagulation with the speed between 80-
100 rpm for 15 minutes.
5. After 15 minutes, slow down the speed between 20-30 rpm and stir for 5-10 minutes.
6. After all the above process keep the beaker for a detention period of 20-30 min for efficient
settling of flocks.
7. Take out the supernatant liquid without disturbing the sediment and check the final
turbidity and alkalinity of all the beakers.
1 2
2 4
3 6
4 8
5 10
6 12
From the graph; we can conclude that whichever will give maximum turbidity removal, that
dosage of alum will be the optimum dosage of coagulant.
Results:
Optimum dosage of coagulant to be added for the given water sample is …………. ml
Discussion:
Environmental Significance:
Coagulants are used in water treatment plants
(i) to remove natural suspended and colloidal matter,
(ii) to remove material which do not settle in plain sedimentation, and
(iii) to assist in filtration.
To maintain the cost of operation and maintenance, optimum dosage quantity is essential
to be determined.
Questions:
Marks Obtained:
Signature of Course Co-ordinator:
Reagents:
1. Deionised distilled water
2. Stock sodium solution
3. Intermediate solution
4. Standard sodium solution
5. Standard lithium solution.
Procedure:
1. Prepare a blank and sodium calibration standards in stepped amounts in any of the following
applicable ranges 0 to 1.0, 0 to 10 or 0 to 100 mg/L.
2. Starting with the highest calibration standard and working towards the most dilute, measure
emission at 589 nm.
3. Repeat the operation with both calibration standards and samples enough limes to secure a
reliable average reading for each solution.
4. Construct a calibration curve from the sodium standards.
5. Determine sodium concentration of sample from calibration curve.
Procedure:
For Bracketing Approach:
1. From the calibration curve, select and prepare sodium standards that immediately bracket the
emission intensity of the sample.
2. Determine emission intensities of the bracketing standards (one sodium slightly less and other
slightly greater than the sample) and the sample as nearly simultaneously as possible.
3. Repeat the determination on bracketing standards and sample.
Calculations:
For direct reference to the calibration curve:
Mg Na/l = (mg Na/l in portion) * D
For the bracketing approach:
Mg Na/l = [({(B-A)(s-a)}/(b-a))+A]D
Where:
B= mg Na/l in upper bracketing standard
A= mg Na/l in upper bracketing standard
b= emission intensity of upper bracketing standard
a= emission intensity of upper bracketing standard
s= emission intensity of sample
D= dilution ration=(ml sample + ml distilled water) / ml of sample
Results:
The sodium content in the given sample:
Sample 1: …………………………
Sample 2: …………………………
Discussion:
Activity:
Write down how high or low concentrations of sodium can effect health of humans and effect the
environment.
Marks Obtained:
Signature of Course Co-ordinator:
Reagents:
1. Deionised distilled water
2. Stock potassium solution
3. Intermediate potassium solution.
Procedure:
1. Prepare a blank and potassium calibration standards in stepped amounts in any of the
following applicable ranges 0 to 1.0, 0 to 10 or 0 to 100 mg/ltr.
2. Starting with the highest calibration standard and working towards the most dilute, measure
emission at 766.5 nm.
3. Repeat the operation with both calibration standards and samples enough limes to secure a
reliable average reading for each solution.
4. Construct a calibration curve from the potassium standards.
5. Determine potassium concentration of sample from calibration curve.
Procedure:
For Bracketing Approach:
1. From the calibration curve, select and prepare potassium standards that immediately bracket
the emission intensity of the sample.
Calculations:
For direct reference to the calibration curve:
Mg K/l = (mg K/l in portion) * D
Results:
DETERMINATION OF NITRATES
Aim: To determine the nitrates by Spectrophotometer method.
Introduction:
Nitrate reacts with phenol disulphonic acid produces a nitro derivative, which is alkaline
medium develops a yellow color. The color produced follows the Beer’s law and is directly
proportional to the concentration of nitrate present in the sample.
Apparatus:
1. Spectrophotometer; 2. Nessler’s tubes
Figure: Spectrophotometer
Reagents:
1. Standard silver sulphate,
2. Phenol-di-sulphonic acid
3. Ammonium hydroxide,
4. Stock nitrate solution,
5. Standard nitrate solution.
Procedure:
1. Take 50 ml of filtered sample in an Erlenmeyer flask.
2. Add an equivalent amount of silver sulphate to remove chlorides (1 mg/ltr = 1 ml Ag2SO4
solution)
3. Heat slightly and filter the precipitate of AgCl.
4. Evaporate the filtrate in a porcelain dish to dryness.
9. Prepare the standard curve using suitable aliquots of standard nitrate solution in the range of 5 to
500 mg.
Results:
Environmental Significance:
1. Nitrate determinations are important whether the water supplies meet the BIS for the
control of the methemoglobinemia in infants.
2. It is used to access the self-purification properties of water bodies and nutrient balance in
surface waters and soil.
3. It is useful to find out state of decomposition of organic matter in waste water.
Questions:
Marks Obtained:
Signature of Course Co-ordinator:
DETERMINATION OF IRON
Aim: To determine the Iron content in the given sample by phenanthroline method.
Introduction:
Iron is brought into solution reduced to the ferrous state by boiling with acid and
hydroxylamine and treated with 1-10 phenanthroline at pH 3.2-3.3 to form a complex orange red
colour. The intensity of colour is proportional to the concentration of iron and obeys Beer’s law.
Apparatus:
2. Nesslers tubes; 2. Conical flasks; 3. Pipettes; 4. Hot Plate
Procedure:
1. Take 50ml of given sample in a conical flask.
2. Add 1 ml of Hydroxyl amine hydrochloride solution and 2ml of Conce. HCl. Add few glass
beads and heat this sample until the volume of the solution reduces to 15 – 20 ml.
3. Cool the solution to room temperature and transfer this to a Nessler’s tube.
4. Add 2ml of phenanthroline solution and 10 ml of Ammonium acetate buffer.
5. Make up the contents of Nessler’s tube exactly to 100ml by adding distilled water and allow
at least 10-15 minutes for colour development.
6. Compare this solution with Iron standards and note down the reading with which standard it
matches.
7. The matching colour standard will give the concentration of iron in the sample.
Results:
Discussion:
Environmental significance
1. Iron content of the water is important in determining the suitability of water for domestic and
industrial purposes.
2. Determination of iron is useful to select the treatment unit and design of treatment units
3. 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.
4. It is also used to aid in the solution of problems in distribution systems where iron fixing
bacteria are troublesome.
5. The iron determination is helpful in assessing the extent of corrosion and aiding in control of
corrosion.
Questions:
1. Other than the above method, which method of analysis can be employed to determine the quantity
of Iron.
Marks Obtained:
Signature of Course Co-ordinator:
DETERMINATION OF MANGANESE
Aim: To determine the manganese content in the given sample.
Introduction:
Manganese is associated with iron minerals and occurs in nodules in ocean, fresh water and soils.
The common ores are pyrolusite and psilomelane. Manganese is used in steel alloys, batteries and
food additives. The FAO-recommended maximum level for manganese in standard is 50μg/L. BIS
desirable limit is 0.1 mg/L.
Principle:
Persulphate oxidation of soluble manganous compounds to form permanganate is carried out in the
presence of silver nitrate. The resulting colour is stable for at least 24h if excess Persulphate is
present and organic matter is absent.
Apparatus: 1. Colorimetric equipment 2. Conical flasks; 3. Pipettes; 4. Hot Plate
Reagents: Ammonium persulphate; Standard manganese solution
Procedure:
1. Pipette a portion containing 0.05 to 2mg Mn into a 250mL conical flask. Add distilled water, if
necessary, to 90mL and proceed.
2. To a suitable sample portion add 5mL special reagent and 1 drop H2O2. Concentrate to 90mL by
boiling or dilute to 90mL.
3. Add 1g (NH4)2S2O8, bring to a boil and boil for 1min.
4. Do not heat on a water bath. Remove from heat source, let stand 1 min and then cool under the tap
(boiling too long results in decomposition of excess Persulphate and subsequent loss of
permanganate colour; cooling too slowly has the same effect).
5. Dilute to 100mL with distilled water free from reducing substances and mix. Prepare standards
containing 0, 5, to 1500μg Mn by treating various amounts of standard Mn solution in the same way.
Photometric determination:
1. Use a series of standards from 0 to 1500μg Mn/100 ml. final volume.
2. Make photometric measurements against a distilled water blank.
The following table shows light path length appropriate for various amounts of manganese in 100ml.
final volume:
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.
Questions:
1. What is the environmental significance of iron and manganese in water supplies?
2. Discuss briefly how iron and manganese get into underground water supplies?
3. What analytical methods area generally used for measuring the concentration of manganese in
water supplies?
4. What is the principle of colorimetric determinations?
Marks Obtained:
Signature of Course Co-ordinator:
Reagents:
1. Standard Potassium Dichromate (0.25N)
2. Sulphuric Acid with Silver Sulphate
3. Standard Ferrous Ammonium Sulphate(0.1N)
4. Ferroin Indicator.
5. Mercuric Sulphate (HgSO4)
Observations:
Calculations:
Where ;
Quantity of FAS added for blank solution = A (ml)
Quantity of FAS added for water sample = B (ml)
= ………………………….. mg/lt.
Discussion:
Environmental significance:
1. The COD test is used extensively in the analysis of industrial wastes.
2. It is widely used in place of BOD in assessing the operation of treatment facility because
of the speed with which the result can be obtained.
3. It is useful to access strength of wastes which contain toxins and biologically resistant
organic substances.
Questions:
Marks Obtained:
Signature of Course Co-ordinator:
Introduction
1. Objective
To measure the ambient concentrations of gases and particulate matter by using High Volume
Sampler (HVS).
2. Instruments
a. High volume sampler (HVS) b. Whatman filter paper c. Impingers
3. Principle
PM10 and TSPM are measured by passing air at flow rate of about 1 lpm through high efficiency
cyclone which retains the dust particles greater than 10 micron size and allow only fines (less than 10
micron particles) to reach the glass microfibre filter where these particles are retained. The
instrument provides instantaneous flow rate and the period of operation (on-time) for calculation of
Department of Civil Engineering – 15CVL76 Page 99
GLOBAL ACADEMY OF TECHNOLOGY
air volume passed through the filter. Amount of particulates collected is determined by measuring the
change in weight of the cyclone cup and filter paper.
4. Reagents for gaseous pollutants a. 0.1 N Sodium tetra-chloratemercurate (SO2) b. Sodium
hydroxide and sodium arsanite (NO2)
5. Procedure
i. For particulates
a. Perform leak check of the instrument before starting the sample.
b. Filter paper need to be inspected for pin holes.
c. Filter conditioning need to be done at 20-25ºC temperature and less than 50% Relative Humidity.
d. Never fold filter completely.
e. Do not touch filters by dirty hands always use disposable hand gloves.
f. Under take regular cleaning of key components of the machine.
g. Ensure stable power supply to the machine. Do not leave loose contact of supply wire to the
machine.
h. Always fill up distilled water in manometer assembly.
i. Do not switch on and off machine using Timer Switch.
j. Clean impinge and rotameter regularly and also clean manifold once in two months.
k. Do not take flow reading immediately after switching on the machine. Give 5 minute for flow
stabilization and for heat up the blower components.
l. Always attach a new weighed cyclone cup with every filter change.
m. Do not switch on machine without filter paper
n. If machine is not expected to be operated within 48 hrs drain out the manometer water and store
machine with water in the manometer tank.
o. Do not run machine during rain in open atmosphere.
ii. For gaseous
The increasing general awareness of atmospheric pollution and its hazards to the health and well-
being of industrial workers, educational buildings, offices etc., is bound to result in greater stress on
accurate, reliable and frequent assessment of work place pollution and worker-exposure. Use
additionally impinge tray with HVS sampler simultaneously sample gaseous pollutants.
6. Calculation for particulates
a. Initial Manometer Reading =
b. Final Manometer Reading =
c. Initial Filter Paper Weight =
Department of Civil Engineering – 15CVL76 Page 100
GLOBAL ACADEMY OF TECHNOLOGY
d. Final Filter Paper Weight =
e. Initial Cyclone Cup Weight =
f. Final Cyclone Cup Weight =
g. Total Suspended Particulate Matter Concentration =
Distance 1m 2m 4m
Sound Pressure
Level, dB(A) in
classroom
Sound Pressure
Level, dB(A) in
alternate space
Comments:
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