Environmental Science

INDEX
Sl.No. EXPERIMENTS PAGE

3-5
Determination of pH of water sample by pH meter
1.

6-9
Determination of Turbidity of water by Turbidity meter
2.

10-12

Determination of colour of water sample by Standard Color

3. Solutions Method and Dilution Multiple Method

13-17
Determination of Available Chlorine in Bleaching Powder
4.

18-20
Determination of Total Solids, Dissolved Solids and
Suspended Solids in Water using oven drying and muffle
5.
furnace

21-26
Determination of dissolve oxygen of water by DO meter
6.
and Winkler method

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INTRODUCTION TO ENVIRONMENTAL SCIENCE

LABORATORY

This is an introduction to environmental science and sustainability lab course.

Students will have hands on experience and perform laboratory work in
identifying and analyzing different environmental problems related with air,
water pollution, and environmental degradation. Furthermore, students will
learn about the interdependence of ecosystems such as the impacts of
excessive fertilizer and nutrient usage in agricultural systems, which can result
in both surface and ground water pollution. Students will also learn how
individual consumption patterns can make a difference in energy use and
protect the environment.

Course Context:
This is an introduction course and serves as one of the required sciences course for
students of all major. The number of registration for this course increases every year
and offered every semester. Students with non-science major account for 65 % and
science major account for 35 %. Outstanding high school, freshman, sophomore,
junior and senior students register for this course.

Course Content:
This course is a multi-disciplinary science course within chemistry, ecology,
hydrology, energy and environment. The course includes lecture class, six indoor
labs, one field lab and group project. Students perform an experiment on acid and
base reaction, water quality, air pollution, toxic analysis, and nutrient analysis.
Students learn how to write a lab report, analyze and interpret chemical analysis.
students learn how to identify environmental problem and propose an action
remedial plan.

Course Goals:
The objective of this course is to make students familiar with the environmental
issues. Students will able to understand about acid rain deposition, invasive and
exotic species, large scale deforestation, anthropogenic influence on atmospheric
conditions, and different kind of pollution. students will learn about the
interdependence of ecosystems such as the impacts of excessive fertilizer and
nutrient usage in agricultural systems, which can result in both surface and ground
water pollution. This course would enable students to be aware of and to learn about
the burning topics related to the environment from across the globe.

Course Features:
Students perform experiment and will have hands on experience in identifying and
analyzing different environmental problems related with air, water pollution, and
environmental degradation. Students identify environmental problems on campus
and propose an action remedial plan and present the findings with presentation and
a complete a term paper.

Course Philosophy:
This course was designed from the multi-disciplinary view of Earth and Environment
department. The course is designed to give awareness and exposure to students to
identify environmental problem and propose a solution to the problem. We can make
a difference if we come together and act in a way so that we can not only enjoy a
healthy environment, but also preserve it for the future generations.

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EXPERIMENT NO: 1

DETERMINATION OF pH OF WATER
AIM: To determine pH of water sample by pH meter.

APPARATUS AND CHEMICALS:

1) buffer solution of pH 4 and pH 7

2) pH meter along with electrodes
3) KCl solution
4) Distilled water
5)Thermameter
6. pH paper

PRINCIPLE:

If two solutions are separated by pH glass (the bulb of a conventional glass pH electrode), an
electrical potential will be developed across the membrane.If the solution inside the bulbcontains
hydrogen ion concentration, the membrane potential will change as the hydrogen ion concentration of
the other solution varies. If electrical connections are made to these solutions (a) inside the glass by
the pH electrode’s internal element and (b) outside the glass by a ‘reference electrode’, the membrane
potential can be measured by a high impedence voltmeter.

ENVIRONMENTAL SIGNIFICANCE:

Determination of pH is one of the important objectives in biological treatment of the wastewater. In

anaerobic treatment, if the pH goes below 5 due to excess accumulation of acids, the process is
severely affected. Shifting of pH beyond 5 to 10 upsets the aerobic treatment of the wastewater. In
these circumstances, the pH is generally adjusted by addition of suitable acid or alkali to optimize the
treatment of the wastewater. pH value or range is of immense importance for any chemical reaction.
A chemical shall be highly effective at a particular pH.. Chemical coagulation, disinfection, water
softening and corrosion control are governed by pH adjustment.

Lower value of pH below 4 will produce sour taste and higher value above 8.5 a bitter taste. Higher
values of pH hasten the scale formation in water heating apparatus and also reduce the germicidal

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potential of chlorine. High pH induces the formation of tri-halomethanes, which are causing cancer in
human beings

STEPWISE PROCEDURE OF pH DETERMINATION :

A. CONNECTING THE ELECRODE:

1. Setup the electrode stand and fit the pH electrode into it.
2. Carefully remove the procreative rubber cap from the filling hole of electrode. The level of
KCl solution should be a few mm below the hole. Top up if necessary with saturated KCl
solution. Now put the rubber cap back

B. PREPERATION OF BUFFER SOLUTIONS:

3.Dissolve one buffer tablet of 7 pH in 100 ml of distilled water . The pH of this solution is 7 pH .
Similarly, the buffer solution if any other value can be prepared. Put this buffer solution in a bottle
and store in a cool place.

C. CALIBRATION OF pH METER:

4. Connect the combination pH electrode to the input socket , wash it with water and switch on the
instrument.
5.Dip the electrode in 7 pH buffer solution.
6.Set the ‘TEMPERATURE oC to control the buffer solution temperature
7.Set the Function selector switch to pH position and adjust the ‘CALIBRATE’ control till the digital
display shows the precise pH value of the buffer solution.
8.Now move the Function Selector Switch to ‘STAND BY’
9.Remove the electrode from the buffer solution and wash it with distilled water or re-iodised water.
10.Dip the combination electrode into another buffer solution (say 4 pH)
11.Set the ‘TEMPERATURE oC control to the temperature of the selected buffer solution.
12. Set the Function selector switch to pH position .Adjust the ‘slope’ correction control , at the front
panel until the display shows the pH value of the selected buffer solution.

D. WORKING PROCEDURE:

13. Once the electrode and pH meter is calibrated dip the charged electrode at selected temperature
in a sample of water whose pH has to be determined.
14. Repeat the process at different temperature for the sam sample of water
15. A graph of pH vs TEMPERATURE is plotted.

E. MEASUREMENT of mV :

1. Connect the combination pH electrode to the input socket.

2. Set the Function Selector Switch to mV position.
3. Dip the combine electrode in solution under test.
4. The display will display mV value of the solution under test.

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OBSERVATION:

Sl. No. TEMPERATURE pH of sample water

1.
2.
3.
4.
5.
6.
8.
9.
10.

PERMISSIBLE LIMIT:

 pH of drinking water should lie in the range of 6.5 to 8.5 .

INFERENCE:

PRECAUTION :

1. A pH electrode is fragile and one should not be tempted to use it as a stirring glass rod when
adjusting pH.
2. A pH meter needs to be calibrated daily with the help of standard buffer solutions.
3. pH readings are temperature sensitive due to changes of glass electrode resistance .A 10- fold
increase in resistance results for every 30 oC rise in temperature.Avoid temperature
fluctuations and never keep the pH meter exposed to direct sunlight.
4. The glass electrode should not be left out of the storage solution for prolonged intervals as the
glass membrane gets dehydrated resulting in slower response and can eventually lead to
complete response failure. The slectrode should not be immersed in dehydrating solutions
such as sulphuric acid and ethanol.
5. Glass is rapidly attacted by HF acid so never keep the electrode in HF solution as it can lead
to irreparable damage of the electrode.
6. Store sensors at ambient temperatures of 10 C to 30 C.Protective caps as well as solution
storage caps provided by the supplier should be installed onto the end of the sensor when not
in use. Ideally the sensor should be stored in 3 to 3.5 M KCl solution. Keep a check to ensure
that the storage solution has not evaporated.

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EXPERIMENT NO. 2

DETERMINATION OF TURBIDITY
AIM: To determine Turbidity of a sample of water by Turbidity meter

APPARATUS and CHEMICALS:

1. Turbidity Meter
2. Sample Cells
3. Standard flasks
4. Funnel
5. Wash Bottle
6. Tissue Papers
7. Hexamethylenetetramine
8. Hydrazine sulphate
9. Distilled water

PRINCIPLE:

The principle of nephelometry is based on the scattering of light by solid or colloidal particles
suspended in solution. When light is passed through the suspension, part of incident radiant
energy is dissipated by absorption, reflection, and reaction while remainder is transmitted. In
fact the measurement of the intensity of transmitted light is a function of the concentration of
dispersed phase and this becomes the basis of turbid metric analysis. In nephelometry light is
passed through the sample solution (suspended particles) directly and the amount of scattered
radiation is measured generally at 90°C . The measurement of intensity of scattered light as a
function of concentration of dispersed phase is the basis of analysis of nephelometry.

ENVIRONMENTAL SIGNIFICANCE:

When the turbid water in a small, transparent container such as drinking glass is held up to the light,
an aesthetically displeasing opaqueness or milky coloration is apparent. The colloidal material which
exerts turbidity provides adsorption sites for chemicals and for biological organism that may not be
harmful. They may be harmful or cause undesirable tastes and odours. Disinfection of turbid water is
difficult because of the adsorptive characteristics of some colloids and because the solids may
partially shield organisms from disinfectant. In natural water bodies, turbidity may impart a brown or
other color to water and may interfere with light penetration and photosynthetic reaction in streams
and lakes. Turbidity increases the load on slow sand filters.

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The filter may go out of operation, if excess turbidity exists. Knowledge of the turbidity variation in
raw water supplies is useful to determine whether a supply requires special treatment by chemical
coagulation and filtration before it may be used for a public water supply. Turbidity measurements are
used to determine the effectiveness of treatment produced with different chemicals and the dosages
needed.. Turbidity measurements of the filtered water are needed to check on faulty filter operation.
and the optimum dosage of coagulants to treat domestic and industrial wastewaters. Turbidity
determination is used to evaluate the performance of water treatment plants.

STEP WISE PROCEDURE:

A. STOCK TURBIDITY SUSPENSION:

1. Solution -I: Dissolve 1.0 gm Hydrazine Sulphate in distilled water and dilute to 10 ml in a
volumetric flask.
2. Solution- II: Dissolve 10.00 gm hexamethylenetetramine in distilled water and dilute to 100
ml. in a volumetric flask.
3. In 100 ml volumetric flask mixes 5 ml Sol. I and 5 ml sol II .Let them stand for 24 hrs at 25 +
3o C dilute to mark and mix. The turbidity of this suspension is 400 NTU.

4. Prepare the solution and suspension weekly.

5. Dilutions of other values can be prepared from this 400 NTU solution by the following
successive dilution method:

SOLUTION SUSPENSION DIST. WATER

1.) 200 NTU 50 ml 50 ml
2.) 100 NTU 25 ml 75 ml

1. Switch ON the instrument and keep it ON for some time.

2. Select appropriate range depending upon the expected turbidity of the sample
3. Set zero of the instrument with turbidity free water using a blank solution and adjust 000 with
the ‘SET ZERO ‘knob.
4. Now in another test tube, take standard suspension. For 0-200 NTU range use 100 NTU
solution and for higher range use 400 NTU solutions as standard.

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5. Take its measurement and set the display to the value of the standard suspension with the
Calibrate Knob.
6. Now the instrument is ready to take measurement of any solution of unknown concentration.

B. OPERATION:

1. Allow sufficient warm up period after switching ON the instrument.

2. Take the test tube containing distilled water or blank solution in the test tube holder and
close the test holder cover. Make sure that the mark on test tube coincides with the mark
on the panel.
3. Select the required range for measurement.
4. Adjust the display to 000 by adjusting ‘SETZERO’ knob.
5. Remove the test tube containing distilled water and fill another test tube containing
standard solution say 400 NTU as per expected range of unknown solution. Place it in the
test tube holder.
6. Take the measurement of the solution suspension and adjust the Calibrate Knob so that
the display reads the selected solution value.
7. Again check the display zero with the test tube containing distilled water
8. Now the instrument is ready to take measurement of any unknown suspension.

OBSERVATION:

Sample No Temperature of Sample (°C) Turbidity

(NTU)

2.

3.

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PERMISSIBLE LIMIT:

 Fresh drinking water turbity should be nil. However 0-5 mg/L or 10 -25 NTU as per Indian
Standard.

INFERENCE:

PRECAUTION:

1. The presence of coloured solutes causes measured turbidity values to be low. Precipitation of
dissolved constituents (for example, Fe) causes measured turbidity values to be high.

2. Light absorbing materials such as activated carbon in significant concentrations can cause low
readings.

3. The presence of floating debris and coarse sediments which settle out rapidly will give low
readings. Finely divided air bubbles can cause high readings

4. Sample test tube should be thoroughly cleaned both inside and outside. In case the test tube gets
scratched or etached , discard it.

5. Do not touch the test tube where the light strike i.e at the sides of the test tube. So hold test tube
only at the top end

6. Fill the test tube with samples or standards which have been thoroughly agitated. Allow
sufficient time for the air bubbles to escape the reading will come down slowly.

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EXPERIMENT NO. 3

DETERMINATION OF COLOUR OF WATER

AIM: To determine colour of sample water by Standard Color Solutions Method, Dilution Multiple
Method and Spectrophotometric method

APPARATUS AND CHEMICALS:

1) potassium chloroplatinate
2) cobalt chloride
3) Spectrophotometer (HACH, DR 4000U)
4) Filtration system including filter paper, funnel, holder, beaker etc
5) Color -comparison tubes

ENVIRONMENTAL SIGNIFICANCE:

Though presence of color in water is not always harmful to human but in most cases it is. Even if the
water is not harmful, aesthetically people do not prefer to use water with color. Moreover, disinfection
by chlorination of water containing natural organics (which produces color) results in the formation of
tri-halomethanes including chloroform and a range of other chlorinated organics leading to problems
which is a major concern in water treatment. So it is important to limit the color of water for domestic
supplies..

THEORY ON EXPERIMENTAL METHOD:

Available methods for determining color of water:

1. Standard Color Solutions Method

2. Dilution Multiple Method
3. Spectrophotometric method

1. Standard color solution method

Waters containing natural color are yellow-brownish in appearance.

Standard Color Solution: Solutions of potassium chloroplatinate (K2PtCl6) tinted with small
amounts of cobalt chloride yield colors that are very much like the natural colors. In this method, the
color produced by 1 mg/l of platinum (as K2PtCl6) and 0.5mg/l of cobalt (as CoCl2•6H2O) is taken as
the standard one unit of color. Usually, a stock solution stock solution of K 2PtCl6 that contains
500mg/l of platinum is prepared, which has a color of 500 units. Then, a series of working standards
may be prepared from it by dilution.
Color -comparison tubes are usually used to contain the standards. A series ranging from 0 to 70 color
units is employed and samples with color less than 70 units are tested by direct comparison with the
prepared standards. For samples with a color greater than 70 units, a dilution is made with distilled
water distilled water to bring the resulting color within the range of the standards. In this case, the
final result should be corrected using a dilution factor.

2. Dilution multiple method

Color of most domestic and industrial waste waters are not yellow-brownish hue. Other systems of
measurement have to be used to measure and describe colors that do not fall into this classification.

For dilution multiple methods, color is measured by successive dilutions of the sample with color -
free water until the color is no longer detectable comparing with distilled water. The total dilution
multiple is calculated and used to express the color degree.

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3. Spectrophotometric method

The platinum-cobalt method is useful for measuring color of potable water and of water in which
color is due to naturally occurring materials. It is not applicable to most highly colored industrial
wastewaters. In the laboratory color of water is usually measured using spectrophotometer which uses
light intensity of a specific wavelength (455 nm). The color test measures (inversely) an optical
property of water sample which result from the absorption of light of specific wavelength by the
soluble color substances present in water, Before measuring the color of water it is necessary to plot
standard calibration curve for color using different standard platinum-cobalt solutions of known
concentrations within the range of interest.

Procedure for Spectrophotometric Analysis:

1. Prepare standard samples having color within a specific range by mixing different
concentration of standard potassium chloroplatinate solution with distilled water. Using these
samples to prepare a color calibration curve (absorbance vs. color concentration) for the
spectrophotometer.

2. Take 50-mL of filtered test sample in a beaker. Take 50-mL distilled water in another beaker.
Use this sample as blank.

3. Set the spectrophotometer to determine color concentration of the sample.

4. Put the blank sample inside the spectrophotometer cell and set the reading "zero''.

5. Bring out the blank sample and place the test sample inside the spectrophotometer
6. After a While the display will show the color concentration of the sample.

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OBSERVATION:

Sample No Temperature of Sample (°C) Color

1.

2.

3.

PERMISSIBLE LIMIT: Colour of water should be in the range of 10-20 as per BIS.

INFERENCE:

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EXPERIMENT NO. 4

DETERMINATION OF TOTAL RESIDUAL CHLORINE

AIM: To determine Total Residual Chlorine in a given sample of chlorinated water by starch Iodide
method

APPARATUS AND CHEMICALS:

1. Mortar And Pestle

2. Volumetric Flask
3. Burette
4. Pipette
5. Erlenmeyer Flask.
6. Concentrated glacial acetic acid
7. Standard sodium thiosulphate solution (0.025N)
8. Potassium iodide
9. Starch indicator
10.Iodine solution (0.025 N).
11. Bleaching powder

Introduction:

The presence of chlorine residual in drinking water indicates that: 1) a sufficient amount
of chlorine was added initially to the water to inactivate the bacteria and some viruses
that cause diarrheal disease; and, 2) the water is protected from recontamination during
storage. The presence of free residual chlorine in drinking water is correlated with the
absence of disease-causing organisms, and thus is a measure of the portability of water

When chlorine is added to drinking water, it proceeds through a series of reactions

described below and depicted graphically on the next page.
When chlorine is added to water, some of the chlorine reacts first with organic materials
and metals in the water and is not available for disinfection (this is called the chlorine
demand of the water). The remaining chlorine concentration after the chlorine demand is
accounted for is called total chlorine. Total chlorine is further divided into: 1) the
amount of chlorine that has reacted with nitrates and is unavailable for disinfection which
is called combined chlorine and, 2) the free chlorine, which is the chlorine available to
inactivate disease-causing organisms, and thus a measure to determine the portability of
water.
For example, if using completing clean water the chlorine demand will be zero, and there
will be no nitrates present, so no combined chlorine will be present. Thus, the free
chlorine concentration will be equal to the concentration of chlorine initially added. In
natural waters, especially surface water supplies such as rivers, organic material will

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exert a chlorine demand, and nitrates will form combined chlorine. Thus, the free
chlorine concentration will be less than the concentration of chlorine initially added

Chlorine Usage Chart:

Chlorine Addition Flow Chart

Chlorine Added
Initial chlorine
concentration
added to water

Chlorine Demand
Reactions with organic
material, metals, other
compounds present in
water prior to
disinfection

Total Chlorine
Remaining chlorine
concentration after
chlorine demand of
water

Free Chlorine Combined Chlorine

Concentration Concentration of chlorine
of chlorine combined with nitrogen in
available for the water and unavailable
disinfection for disinfection.

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Principle

Bleaching powder is commonly used as a disinfectant. 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.

Procedure:

1. Dissolve 1g bleaching powder in 1 liter of distilled water in a volumetric flask, and stopper the container.
(This can be done by first making a paste of the bleaching powder with mortar and pestle.)

2. Place 5 mL 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.

3. Titrate with 0.025 N sodium thiosulphate solutions until a pale yellow colour is obtained. (Deep yellow
changes to pale yellow.)
4. Add 1mL of starch solution and titrate until the blue colour disappears.

5. Note down the volume of sodium thiosulphate solution added (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 solutions 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 = A2 - A3

Note: Blank titration is necessary to take care of the oxidizing or reducing reagents' impurities.

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Observation:

Bleaching powder solution x Standard sodium thiosulphate solution (0.025 N)

Distilled water × Standard sodium thiosulphate solution (0.025 N)

Distilled water x Standard iodine solution (0.025N)

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Calculation
(V – A1) or (V + A4) x N x 35.46
mg of Cl2/mL (B) =
mL of bleaching powder solution taken

1000 mL of bleaching powder solution contains 1000 x B mg of Cl2 i.e., 1000 mg

bleaching powder contains 1000 B mg of Cl2

1000 x B
therefore, 100 mg of bleaching powder contains =
10

% of chlorine available = .........

Results
Available chlorine in the given bleaching powder is. ...%

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EXPERIMENT NO. 5

DETERMINATION OF TDS, SUSPENDED SOLIDS IN WATER

AIM: To determine the total suspended solids, total dissolved solids and total solids of a given sample.

PRINCIPLE:

Determination of total solids is made by evaporating and drying of a measured

Sample in an oven at 1050C for a period of 1 hour. Since water for potable use
contains small amount of suspended mater, it is usual to filter a sample of water
and determine solids in filtrate by the fore going method. The difference between
Total solids in unfiltered and filtered samples are taken as measure of the
Suspended solids is also classified as volatile or organic solids and fixed or
Inorganic solid.

ENVIRONMENTAL SIGNIFICANCE:

Dissolve minerals, gases and organic constituents may produce aesthetically displeasing colour, taste and
odour. Some dissolve organic chemicals may deplete the dissolved oxygen in the receiving water and
some may be inert to biological oxidation, yet others have been identified carcinogens. Water with higher
solids content often has a laxative and sometimes the reverse effect upon people whose bodies are not
adjusted to them. Higher concentration of TDS about 3000mg/L may also produce distress in livestock. In
industries, the use of water with high amount of dissolved solids may lead to scaling in boilers, corrosion
and degraded quality of the product.
Estimation of total dissolve solids is useful to determine whether the water is suitable for drinking
purpose, agriculture and industrial purpose. Suspended organic solids aesthetically may release obnoxious
odour. Biologically active suspended solids may include disease causing organisms as well as toxic
producing strains of algae.

APPARATUS:

1. Standard beaker
2. Conical Flask
3. Filter paper
4. Digital balance
5. Oven
6. Water quality analyzer

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PROCEDURE:

(I)SUSPENDED SOLIDS:

1. Take 25 ml of sample in beaker

2. Note the weight of properly dried filter paper (W1)
3. Properly fold and place the filter paper on the Erlenmeyer flask
4. Pour the sample trough the filter paper and filter it completely
5. Transfer the filter paper to an oven at1050C for one hour
6. Note the weight of dried filter paper (W2)
7. The difference between the above two weight gives the suspended solids (W3)

(II)DISSOLVED SOLIDS:

1. Take suitable quantity of sample in a beaker

2. Switch on the water quality analyzer and dip the concerned electrode in the
sample
3. After few minutes note the digital reading, which gives the amount of dissolved
solids in mg/l (W4)

(III)TOTAL SOLIDS

1.Add suspended solids (w3) and dissolved solids(w4) which gives total
Solids

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OBSERVATIONS:

1. Total suspended solids in the sample =

2. Total dissolved solids in the sample =

3. Total solids in the sample =

PERMISSIBLE LIMIT:

As per Indian Standard permissible limit for TDS in drinking water should not exceed 500 mg/L.

INFERENCE:

PRECAUTIONS:

1. Water or wastewater samples which contain high concentrations of Calcium, Chloride,

magnesium or sulphate can rapidly absorb moisture from the air.
2. Such samples may need to be dried for a longer period of time, cooled under proper desiccation
and weighed rapidly in order to achieve a reasonable constant weight.
3. Volume of sample should be adjusted to have residue left after drying as 100 to 200 mg. It is
mainly to prevent large amount of residue in entrapping water during evaporation.
4. Sample with high concentrations or bicarbonate require additional drying at 180 C to ensure that
all of the bicarbonate is converted to carbonate.

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EXPERIMENT NO. 6

DETERMINATION OF DISSOLVE OXYGEN IN WATER:

AIM: To determine D.O. in a sample water by Winkler Test and D.O meter.

APPARATUS and CHEMICALS:

1. BOD bottles capacity 300 ml .

2. Sampling device for collection of samples.
3. Manganese sulphate
4. Sodium Hydroxide
5. Potassium Iodide
6. Sodium Azide
7. Conc. Sulphuric Acid
8. Starch
9. Sodium Thiosulphate
10. D.O. Meter with electrode
11. Sodium Sulphite
12. Titrating Flask
13. Burette with Burette Holder

PRINCIPLE:

The basic principle of electrochemical determination of dissolve oxygen concentration is the use of
membrane covered electrochemical sensors. The main components of the sensors are the oxygen
permeable membrane, the working electrode, electrolyte solution and a reference electrode. A voltage is
supplied between the gold or platinum or silver cathode and the anode that consists of either lead or silver
and causes the oxygen to react electrochemically. The higher the oxygen concentration the higher the
resulting electric current. The current in the sensor is measured and after calibration, converted into the
concentration of dissolved oxygen.

ENVIRONMENTAL SIGNIFICANCE:

Oxygen dissolved in water, often referred to as D.O. is a very important parameter of water quality and is
an index of physical and biological process going on in water. There are two main sources of dissolved
oxygen in water. (i) Diffusion from air (ii) Photo- synthetic activity within water. Diffusion of oxygen
from air to water is a physical phenomenon and depends upon solubility of oxygen which, in turn, is
influenced by factors like temperature, water movements and salinity etc. Photo- synthetic activity is a
biological phenomenon carried out by autotrophy population, light conditions and available gases etc.
Non polluted surface water is normally saturated with dissolved oxygen and demanding pollutants (like
organic waste) causes rapid depletion of DO from water. The solubility of atmospheric oxygen in fresh
water ranges from 14.6 mg/L at 0°C to about 7.0 mg/L at 35°C under one atmospheric pressure. Since it

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is poorly soluble gas its solubility directly varies with the atmospheric pressure at any given temperature.
Oxidizable ammonia, nitrates, ferrous ion etc. also cause decrease in dissolved oxygen content.
Organisms have specific oxygen requirements, e.g. 2-5 gm/l for most of the fishes. Low dissolved oxygen
may prove lethal for many organisms.
It is necessary to know DO levels to assess quality of raw water and to keep a check on stream pollution.
DO test is the basis of BOD test which is an important parameter to evaluate pollution potential of wastes.
Oxygen is an important factor in corrosion. DO test is used to control amount of oxygen in boiler feed
waters either by chemical or physical methods. DO is necessary for all aerobic biological wastewater
treatment processes. In liquid waste dissolved oxygen is the factor that determines whether the biological
changes are brought out by aerobic or anaerobic organisms.

STEPWISE PROCEDURE:

A. DETERMINATION OF D.O BY WINKLER METHOD

(I)PREPARATION OF REAGENT
1. Manganese sulphate : Dissolve 480 g MnSO4 . 4H2O, 400 g MnSO4 .2H2O or 364 g MnSO4 .H2O
and dilute to 1000 ml. filter if necessary. This solution should not give colour with starch when added to
an acidified solution of KI.
2. Alkali iodide-azide reagent: Dissolve 500 g NaOH ( or 700 g KOH) and 150 g KI or 135 g. NI dilute
to 1000 ml.Add 10 g NaH3 dissolved in 40 ml distilled water. This solution should not give colour with
starch solution when diluted and acidified.
3. Sulphuric acid : H2SO4, conc. 1 ml is equivalent to about 3 ml alkali-iodide-azide reagent.
4. Starch indicator: Prepare paste or solution of 2.0 g L.R. grade soluble starch powder and 0.2 Salicylic
acid as preservative in distilled water. Pour this solution in 100 ml boiling water. Allow to boil for few
minutes, cool and then use.
5. Stock sodium thiosulphate 0.1 N: Dissolve 24.82 g Na2S2O3 .5H2O in boiled distilled water,
preserve by adding 0.4 g solid NaOH or 1.5 ml 6N NaOH or dilute to 1000 ml.
6. Standard sodium thiosulphate 0.025 N : Dilute 250 ml stock Na2S2O3 solution to 1000 ml with
freshly boiled and cooled distilled water. Add preservative before making up the volume. (This solution
will have to be standardized against standard of dichromate solution for each set of titrations).

(II) PROCEDURE:
1. Collect sample in a BOD bottle using DO sampler.
2. Add 2 ml MnSO4 followed by 2 ml of alkali-iodide-azide reagent. The tip of the pipette should be
below the liquid level adding these reagents. Stopper immediately.
3. Mix well by inverting the bottle 2-3 times and allow the precipitate to settle leaving 150 ml clear
supernatant.
4. At this stage, add 2 ml conc. H2SO4. Mix well till precipitate goes into solution.

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5. Take 203 ml in a conical flask and titrate against Na2S2O3 using starch as an indicator. When 2 ml
MnSO4 followed by 2 ml alkali-iodide-azide reagent is added to the samples as in (2) above 4.0 ml

of original sample is lost. This 203 ml taken for titration will correspond to 200 ml of original
sample.

B. PROCEDUR FOR DETERMINING D.O. BY D.O. METER

(I) DO Probe Assembly

1. DO probes consist of silver and gold electrode cells, an electrolyte tube with ring. The
following procedure may be followed for assembly of DO probe. Be careful to handle its
membrane. Fit the membrane on the lower part of the electrolyte tube.

2 .Fill potassium chloride solution (7.5%) in the electrolyte tube to its top. Insert the electrode
in the electrolyte tube and tightly screw it up. Now the probe is ready to use.

(II) DO OPERATION:

1. Set the temperature knob to the solution temperature and CAL Knob to extreme right
position.
2. Place the DO probe in 2% sodium sulphite solution. Allow the display to attain
equilibrium. If the display does not read 000 set the zero knob to bring the display to read
000 by keeping temperature knob to actual temp. of the solution. Calibrate knob should
be at extreme right position.
3. Now calibrate the instrument with known value of DO solution as obtained by Winkler
method as well as sample with zero DO (Add excess of Na2SO3 and a trace of CaCl2 to
bring DO to zero).
4. Take 250 ml flask and fill 2/3 of it with distilled water
5. Stopper the flask and shake it for 20 sec. Remove the stopper back and swirl the water
back and repeat the process 4 times.
6. Measure the temp. of water and set the temp. knob at a temp. of water in the flask.
7. Hold DO probe in the flask and agitate the water. Note the reading for different temp.
setup. If necessary adjust he meter reading with CAL knob.
8. Note the instrument id ready to take measurement of DO value of any unknown solution.

(III) CALCULATION FOR WINKLER TEST:

Reactions:

2NaOH + MnSO4 = Mn(OH)2 + K2SO4

2Mn(OH)2 + O2 = 2MnO(OH)2
MnO(OH)2 + H2SO4 = MnSO4 + 2H2O + [O]
2KI + H2SO4 + [O] = K2SO4 + H2O + I2
I2 + I- = I3-
2S2O 3 + I3- = 3I - + S4O 6 –

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OXYGEN CONC. in g/L =

V= Volume of Sodium Thiosulphate

N= Normality of Sodium Thiosulphate

D.O METER

BOD BOTTLE ELECTRODE PROBE

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OBSERATIONS:

(I) By Winkler method

Volume of Sample
Initial Final
S.No corresponding to Difference DO mg/L
burete burete
original used in (A) mL =(AxNx8000)/V
reading reading
Titration (V) Ml
1.

2.

3.

(II)By DO Meter

Sl.No.
TEMPERATURE DISSOLVE OXYGEN
1.
2.
3.
4.
5.

PERMISSIBLE LIMIT as per Indian Standard

 For ground water : 2-3 mg/L

 For supply water : 4 mg/L
 For river water: 9 mg/L

INFERENCE:

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PRECAUTIONS:

(I) Regarding WINKLER TEST:

 Do not allow air to trap while sampling water during BOD analysis.
 Dip the tip of the pipette just at the bottom of the BOD bottle and
gently release the reagents.
 Take care that the chemicals do not flow out from the bottle while Shaking/swirling.
 Observe the colour changes during the BOD reaction, if any.

(II) Regarding INSTRUMENT:

 Do not touch the silve electrode

 Since the instrument is based on on the diffusion process, the agitation of the solution is must.
Hand shaking of the solution may not give accurate readings. Magnetic stirrer is recommended
for this purpose.
 BOD bottle is recommended as a container for measurement of sample solution in the laboratory.
Because DO probe tight fits in BOD bottle and no atmospheric oxygen may dissolve during
measurement.
 Any accumulation of organic matter on the membrane will affect the CAL.It is advisable to clean
the membrane with a soft tissue paper after use.

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