Environmental Sciences Lab

(CYFC0131)

(B. Tech. First year)

Laboratory Manuals
(NEP w.e.f. August, 2023)

Department of Chemistry DR B R Ambedkar

National Institute of Technology, Jalandhar
Jalandhar– 144 011(Punjab)-INDIA

Prepared by: Dr N C Kothiyal & Dr B S Kaith

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Prepared by: Dr N C Kothiyal & Dr B S Kaith

 Environmental Sciences Lab
List of Practicals

Experiment No Objective
Experiment No.1 Determination of odour number of the given water sample

Experiment No.2 Determination of TS (total solids), TDS (total dissolved solids) and TSS
(total suspended solids) of the given water sample

Experiment No.3 Determination of Turbidity of the given water sample

Experiment No.4 Determination of pH of the given water sample

Experiment No.5 Determination of Conductivity of the given water sample

Experiment No.6 Determination of Heavy metals concentration in the given water sample

Experiment No.7 Determination of Chloride content in the given water sample

Experiment No.8 Estimation of Hardness in the given water sample

Experiment No.9 Removal of toxic dyes from textile effluent using adsorbents

Experiment No.10 Removal of heavy metals from industrial effluent using adsorbents

Prepared by: Dr N C Kothiyal & Dr B S Kaith

 EXPERIMENT-1
TO DETERMINE ODOUR AND TASTE IN A WATER SAMPLE

Aim: TO DETERMINE ODOUR AND TASTE IN A WATER SAMPLE

Principle: Taste and odour can originate from natural inorganic and organic chemical contaminants and
biological sources or processes (e.g. aquatic microorganisms), from contamination by synthetic chemicals,
from corrosion or as a result of problems with water treatment (e.g. chlorination). Taste and odour may
also develop during storage and distribution as a result of microbial activity.

Taste and odour in drinking-water may be indicative of some form of pollution or of a malfunction during
water treatment or distribution. It may therefore be an indication of the presence of potentially harmful
substances. The cause should be investigated and the appropriate health authorities should be consulted,
particularly if there is a sudden or substantial change.

There are a number of diverse organisms that often have no public health significance but which are
undesirable because they produce taste and odour. As well as affecting the acceptability of the water, they
indicate that water treatment and/or the state of maintenance and repair of the distribution system are
insufficient.

Actinomycetes and fungi can be abundant in surface water sources, including reservoirs, and they can also
grow on unsuitable materials in the water supply distribution systems, such as rubber. They can produce
geosmin, 2-methyl isoborneol and other substances, resulting in objectionable tastes and odours in the
drinking-water.

Blooms of cyano bacteria and other algae in reservoirs and in river waters may cause odour and taste.

High concentrations of chloride give a salty taste to water. Concentrations in excess of 250 mg/l are
increasingly likely to be detected by taste, but some consumers may become accustomed to low levels of
chloride-induced taste.

Most individuals are able to taste or smell chlorine in drinking-water at concentrations well below 5 mg/l,
and some at levels as low as 0.3 mg/l. Hence in the chlorination process, the residual chlorine at the
consumer end is not to exceed 0.2 mg/l.

CLASSIFICATION OF ODOURS

(a) No odour (b)Ammoniacal bad eggs (sulphide) (c) chlorine (bleach) (d) earthy (e) fruity (f) fuel (g)
milky (h) oily (i) soapy (j) Fishy and some other (this should be specified)
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TASTE

No Taste (b) Sweet (c) Salty (d) Sour (e) Bitter

Apparatus Required:-
1. 500 mL clear flasks
2. Watch glasses or stopper
3. Heating device with temperature readout
Procedure :- For Cold Odour:-
Fill the 500 ML flask with around 200 ML of sample. Close the stopper. Shake the flask well at
room temperature. Open the flask and smell at the mouth of the flask. Report the odour in terms of
the classifications mentioned above

Procedure for Hot Odour: -

The intensity of the cold odour may be very low and cannot be detected. For this purpose, heat the
flask to around 58-60 degrees C. Remove the stopper and smell at the mouth of the flask.
The odours can be detected by a group of observers as single observation may not be correct. See
how many agree to a common odour.

Odour Intensity: -
The intensity of the odour can be determined on its strength. Numbers are assigned as follows: -
0--No odour 1--Very Faint 2-- Faint
3--Distinct 4--Decided
5--Very Strong
Add your results in a tabular form as indicated below.
Sample Date Source Odour Cold Odour Hot Odour Remarks
Number Name Classification intensity intensity

As far as taste is concerned, it should be noted only when the full potability of water is ascertained,
i.e., it should be free from all impurities (Physical, Chemical and Biological)

Prepared by: Dr N C Kothiyal & Dr B S Kaith

Sample Number Date Source Name Classification of Taste Remarks

NOTE: - Potable water should be colorless, tasteless and odourless. Refer :- IS:-10050:-
Specifications for Drinking Water
Viva questions
1. What is the objective of the experiment?
2. Why is it important to determine the odor and taste in a water sample?
3. What are the potential sources of odor and taste in water?
4. What equipment and chemicals are required for this experiment?
5. Describe the step-by-step procedure of the experiment.
6. How would you collect a water sample for analysis?
7. How would you ensure that the water sample is representative of the source?
8. Explain the techniques used to determine the odor of the water sample.
9. Describe the techniques used to determine the taste of the water sample.
10. What are the different types of tastes that can be identified in water?

Reference
1. Standard methods for the examination of water and wastewater, 21st Edition, Washington:
APHA., 2012. 2.
2. Sawyer, C. N., McCarty, P. L., and Perkin, G.F., Chemistry for Environmental Engineering
and Science, 5th edition McGraw Hill Inc., 2002.
3. B. Kotaiah and Dr. N. Kumara Swamy, Environmental Engineering Laboratory Manual,
Charotar Publishing House Pvt. Ltd., 1st Ed., 2007.

Prepared by: Dr N C Kothiyal & Dr B S Kaith

 EXPERIMENT-2
AIM-DETERMINATION OF TS (TOTAL SOLIDS), TDS (TOTAL DISSOLVED SOLIDS) AND
TSS (TOTAL SUSPENDED SOLIDS) OF THE GIVEN WATER SAMPLE

1. TOTAL SOLIDS (TS) (Gravimetric method)

AIM Determine the total solid in given water sample.

REQUIREMENTS Porcelain dishes, measuring cylinder, balance and oven etc.

PRINCIPLE
Residue after the evaporation and subsequent drying in oven at specific temperature 103 – 1050 C of a known
volume of sample are total solids. Whereas loss in weight on ignition of the same sample at 550 0C in which
organic matter is converted in to CO2 & H2O while temperature is controlled to prevent decomposition and
volatilization of inorganic matter as much as consistent with complete oxidation of organic matter, are
volatile solids.

PROCEDURE Weight the previously dried empty porcelain dishes (W1) already kept at 1050C for 2 hours
and in desiccator for 30 minutes. Take 100 ml well mixed sample in each porcelain dishes and place the
porcelain dishes in the oven at 1050C carefully for 24 hours. After 24 hours take the dishes out and keep in
the desiccator for 30 minutes for cooling. Now weight the porcelain dishes and note the final weight (W2).
Repeat the process of weighing and drying till constant weight is achieved.

CALCULATION

𝑊𝑊2 −𝑊𝑊1 ×1000

Total solids (mg/L) =
𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉 𝑜𝑜𝑜𝑜 𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠 (𝑚𝑚𝑚𝑚)

Similarly calculate for other two dishes & take average to repeat the results as below-

OBSERVATION TABLE

S. No. Sample Initial weight Final weight TS (mg/l) Average

Description TS
(mg/l)
1.
2.
3.
RESULT Total solids in the given water sample was found----- mg/l at 1050C.

Prepared by: Dr N C Kothiyal & Dr B S Kaith

PRECAUTIONS

1. Glassware should be clean.

2. Cool the dish properly.

3. Note the weight carefully.

2. TOTAL SUSPENDED SOLID (TSS) (Gravimetric method)

AIM Determines the TSS of given water sample.

REQUIREMENT Filter paper (whatman no-41), beaker, hot plate, physical balance, funnel,

measuring cylinder, desiccator, oven etc.

PRINCIPLE
Non filterable residue left on the filter paper and further dried at 1030C – 1050C are suspended solids and
the loss in weight of the filter paper ignited at 5500C are volatile suspended solids.
PROCEDURE

Dry the filter paper in oven (1050C) and cool in desiccator then weight it. Then filter 300 ml sample through
filter paper, keep the filter paper in oven for overnight to dry, cool the filter paper in a desiccator and again
weight it.

CALCULATE THE TSS USING FOLLOWING FORMULA

W1 = Initial weight of filter paper

W2 = final weight of filter paper

V = Volume of sample

𝑊𝑊2 −𝑊𝑊1 ×1000

Total suspended solids =
𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉 𝑜𝑜𝑜𝑜 𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠 (𝑚𝑚𝑚𝑚)

OBSERVATION TABLE

S. No. Sample Initial weight Final weight of TSS (mg/l)

Description of filter paper
filter paper (gm)
(gm)
1.
2.
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Prepared by: Dr N C Kothiyal & Dr B S Kaith

 3.

RESULT The total suspended solids in given water sample was observed------- mg/l.

PRECAUTIONS

1. Glassware should be clean.

2. Weigh the filter paper carefully.

3. Note the weight carefully.

3. TOTAL DISSOLVED SOLID (TDS) (Gravimetric method)

AIM Determines the TDS of given water sample.

REQUIREMENT Filter paper atman no-41), beaker, hot plate, physical balance, funnel,

measuring cylinder, desiccator, oven etc.

PRINCIPLE

Water is a good solvent and picks up impurities easily. Pure water -- tasteless, colorless, and odorless is often
called the universal solvent. Dissolved solids" refer to any minerals, salts, metals, cations or anions dissolved
in water. Total dissolved solids (TDS) comprise inorganic salts (principally calcium, magnesium, potassium,
sodium, bicarbonates, chlorides, and sulfates) and some small amounts of organic matter that are dissolved
in water.
In general, the total dissolved solids concentration is the sum of the cations (positively charged) and anions
(negatively charged) ions in the water. Therefore, the total dissolved solids test provides a qualitative
measure of the amount of dissolved ions but does not tell us the nature or ion relationships
An elevated total dissolved solids (TDS) concentration is not a health hazard. The TDS concentration is a
secondary drinking water standard and, therefore, is regulated because it is more of an aesthetic rather than
a health hazard. An elevated TDS indicates the following:
1) The concentration of the dissolved ions may cause the water to be corrosive, salty or brackish taste, result
in scale formation, and interfere and decrease efficiency of hot water heaters; and
2) Many contain elevated levels of ions that are above the Primary or Secondary Drinking Water Standards,
such as an elevated level of nitrate, arsenic, aluminum, copper, lead, etc.
PROCEDURE

Prepared by: Dr N C Kothiyal & Dr B S Kaith

Dry the beaker in oven (1050C) and cool in desiccator then weight it. Then Take 300 ml filtered sample in
this beaker and evaporate up to dryness on a hot plate, cool in a desiccator and again weight it.

CALCULATE THE TDS USING FOLLOWING FORMULA

Subtract the initial weight (in grams) of the empty container from the weight of the container with the dried
residue to obtain the increase in weight. Then do the following:

W1- Weight of clean dried container (gm)

W2- Weight of container and residue(gm)

V- Volume of Sample (ml)

𝑊𝑊2 −𝑊𝑊1 ×1000

Total dissolved solid =
𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉𝑉 𝑜𝑜𝑜𝑜 𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠 (𝑚𝑚𝑚𝑚)

OBSERVATION TABLE

S. No. Sample Initial weight of Final weight of TDS (mg/l)

Description beaker (gm) beaker (gm)
1.
2.
3.

RESULT The total dissolved solids in given water sample was observed ------- mg/l.

PRECAUTIONS

1. Glassware should be clean.

2. Weigh the beaker carefully.

3. Note the weight carefully

VIVA QUESTIONS
1. What is total dissolved solid and total suspended solid?
2. What is the significance of total dissolved solids?
3. The pore size of the filter paper used for filtration is
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Prepared by: Dr N C Kothiyal & Dr B S Kaith

 4. The chemical substance used in the desiccators is _____.
5. What is TDS level of drinking water?
6. What is the unit of TDS in water?
7. What is the significance of solids determination of wastewater?

EXPERIMENT-3
AIM: DETERMINATION OF TURBIDITY OF A GIVEN WATER SAMPLE

APPARATUS Nephelo-Turbidity meter with sample cell

REAGENTS FOR CALIBRATION OF THE INSTRUMENT

Solution 1: Dissolve 1 gm Hydrazine Sulphate (NH2)2H2SO4 (carcinogen) in distilled water and dilute to
100 ml in a volumetric flask

Solution 2: Dissolve 10 gm Hexamine LR grade (CH2)2N4 in distilled water and dilute to 100 ml in a
volumetric flask

Take 12.5 ml of solution 1 and 12.5 ml of solution 2 in a 100 ml volumetric flask and dilute to 100 ml, allow
to stand for 24 hours at 25 0C. the turbidity of this suspension is 1000 Nephelometric Turbidity Unit (NTU).

THEORY

Turbidity is an expression of optical property that uses light scattering properties of suspension in the sample.
Turbidity in water is caused by suspended matter such as clay, silt, finely divided organic and inorganic
matter soluble, colored organic compounds, plankton and other microscopic organisms. Turbidity is
measured by shining light through a sample and measuring the degree of scattering as measured by a light
detector placed at right angles to the original light path. Above measuring technique is known as
Nephelometry. Turbidity can also be measured by shining light through a sample and measuring the degree
of light penetration as measured by a light detector placed in line to the original light path. This measuring
technique is known as Turbidimetry.

PRINCIPLE

Nephelo-Turbidity meter operates on the principle that light passing through a substance is scattered by
matter suspended in the substance. In this instrument, a strong light beam is passed upward through a tube
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Prepared by: Dr N C Kothiyal & Dr B S Kaith

containing the sample. As the beam passes through the sample, the light is scattered in proportion to
suspended particles. At 900 to the light path, this scattered light is sensed by the phototube to give the
turbidity reading. The unit of measurement is NTU.

CALIBRATION OF THE INSTRUMENT

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

2. 2. Select appropriate range depending upon the expected turbidity of the sample.
3. Set zero of the instrument with turbidity free water using blank solution and adjust 000 with the ‘set
zero’ knob. The CAL control should be moved by 5 turns clockwise
from 0 position.
4. Now in another test tube, take standard suspension that already prepared. For 0-200 NTU range use
100 NTU solution and for higher range use 400 NTU solution as standard.
PROCEDURE

1. Take the test tube containing distilled water in the test tube holder and close the test tube holder lid.

2. Select the required range for measurement.

3. Adjust the display to 000 by adjusting ‘set zero’ knob.

4. Remove the test tube containing distilled water & insert another test tube containing standard solution
(say 400 NTU). Place it in the test tube holder.

5. Take the measurement of the solution suspension & adjust the ‘calibrate’ knob so that the display
reads the selected standard solution value.

6. Again check the display zero with the test tube containing distilled water.

7. Now the instrument is ready to take measurement of any unknown suspension.

CALCULATION

Turbidity (NTU)= NTU measured/proportion of sample in dilution

OBSERVATION TABLE

S. No. Sample Description Turbidity (NTU) Average turbidity

(NTU)
1.
2.

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 3.

RESULT The turbidity of given water sample was observed ____NTU (Nephelo Turbidity Unit).
PRECAUTIONS

1. Sample test tube must be thoroughly cleaned both inside and outside. In case the test tube gets
scratched, discard it.
2. Do not touch the test tube where the light strikes i.e.at the sides of the test tube. So, hold the test
tube only at the top end.
3. Fill the test tube with samples or standards which have been thoroughly agitated.
4. Allow sufficient time for the air bubbles to escape otherwise the reading will slowly come down.
When the readings are taken in the agitated state with air bubbles, the readings will be higher.
VIVA QUESTIONS

1. What is the significance of determination of turbidity?

2. What is the method of determining turbidity?
3. What affects turbidity?
4. What is the principle of turbidity?
5. What is the highest turbidity value of drinking water?
6. What do you mean by 1 NTU?
7. What is the light source for the Nephelo turbidity meter?
8. What is the light source for the Nephelo turbidity meter?
9. The material used in the standard solution for nephelometer is ___.
REFERENCES

• Standard methods for the examination of water and wastewater, 21st Edition, Washington:
APHA., 2012. 2.
• Sawyer, C. N., McCarty, P. L., and Perkin, G.F., Chemistry for Environmental Engineering
and Science, 5th edition McGraw Hill Inc., 2002.
• B. Kotaiah and Dr. N. Kumara Swamy, Environmental Engineering Laboratory Manual,
Charotar Publishing House Pvt. Ltd., 1st Ed., 2007.

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Prepared by: Dr N C Kothiyal & Dr B S Kaith

 Experiment No-4
Aim: To determine the pH of given samples using

(1) universal indicator

(2) pH paper, and

(3) Digital pH meter.

Principle:

pH value of water indicates the hydrogen ion concentration in water and concept of pH was put forward by
Sorenson (1909). pH is expressed as the logarithm of the reciprocal of the hydrogen ion concentration in
moles/ litre at a given temperature. The pH scale extends from 0 (very acidic) to 14 (very alkaline) with 7
corresponding to exact neutrality at 25°C. pH is used in the calculation of carbonate, bicarbonate and CO2,
corrosion and stability index etc. While the alkalinity or acidity measures the total resistance to the pH change
or buffering capacity, the pH gives the hydrogen ion activity. pH can be measured colorimetrically or
electrometrically.

Colorimetric method is used only for rough estimation. It can be done either by using universal indicator or
by using pH paper. The hydrogen electrode is the absolute standard for the measurement of pH. They range
from portable battery operated units to highly precise instruments. But glass electrode is less subjected to
interferences and is used in combination with a calomel reference electrode. This system is based on the fact
that a change of 1 pH unit produces an electric charge of 59.1 mV at 25°C.

Apparatus:

1. pH meter with electrode

2. Beaker
3. Thermometer
4. Colour comparator with discs
5. Cuvettes
Reagents:

1. Buffer solutions
2. pH paper
3. Universal indicator
Procedure:

a) Using Universal Indicator

(If comparators are not available, compare the colour with colours given in the chart.)
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 1. Using pH Papers 10 mL of sample is taken in a cuvette.

2. Another 10 mL sample is taken in another cuvette and 0.2 mL of universal indicator is added
and placed in the hole provided for.

3. A colour disc corresponding to this indicator is inserted into the comparator and the disc
rotated such that the 2 circles indicate identical colours.

4. The reading is noted.

5. The procedure can be repeated using an indicator whose range is near the value obtained.

6. The exact pH is obtained.

b) Using pH Meter

1. Follow the manufacturer ‘s operating instructions.

2. Dip the electrode in the buffer solution of known pH.

3. Switch on the power supply and take the reading. Standardize the instrument using the
calibrating knob.

4. After cleaning, again dip the electrodes in the buffer solution of pH 7. Note the reading. If it
is 7, the instrument is calibrated. If not, correct the value and is manipulated so that the
reading in the dial comes to 7.0.

5. A solution whose pH is to be found is taken in a beaker and the temperature knob is adjusted
such that the temperature of solution is same as that in dial.

6. The electrode is washed with distilled water and reused with the solution and then it is dipped
in the solution.

7. The reading on the dial indicates the pH of the solution.

8. Results

Sample No. pH

pH paper pH meter Universal indicator

1.

2.

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Prepared by: Dr N C Kothiyal & Dr B S Kaith

 3.

PRECAUTIONS:

1. The instrument should be kept in the stand by position only, unless during the actual measurement.

2. "Set 7" control should be operated only in the stand by position.

3. While cleaning the electrodes, do not touch the tip of the electrodes.

Viva questions

1. What is the purpose of determining the pH of water?

2. What are the various methods available to measure the pH of water?

3. Which method did you use in this experiment to determine the pH of water? Why did you choose
this method?

4. What is the principle behind the method you used to determine the pH of water?

5. What are the materials and equipment required for this experiment?

6. Describe the procedure you followed to determine the pH of water.

7. How did you calibrate the pH meter before taking measurements?

8. What are the factors that can affect the accuracy of pH measurements?

9. How did you handle these factors to ensure accurate pH measurements in your experiment?

10. What precautions did you take while handling the pH meter and the samples?
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Prepared by: Dr N C Kothiyal & Dr B S Kaith

 Experiment No-5
Aim: Determination of Conductivity of the given water sample

Principle:

Conductivity is a numerical expression of the ability of an aqueous solution to carry the electric current. This
ability depends on the presence of ions, their mobility, valence, relative concentrations and on the
temperature of measurement. The inorganic acids, bases, and salt solutions are relatively good conductors.
On the contrary, molecules of organic compounds that do not dissociate in aqueous solution have a poor
conductivity.

The conductivity is measured in the laboratory in term of resistance measured in ohms. The electric
resistance of a conductor is inversely proportional to its cross-sectional area and directly proportional to its
length. The magnitude of the resistance measured in an aqueous solution therefore depends on the
characteristics of the conductivity cell used. Specific resistance is the resistance of a cube of 1cm. In aqueous
solutions such a measurement is seldom made because of the difficulties in fabrication of electrode.

Actually, the electrodes measure a given fraction of the specific resistance known as the

cell constant =C

𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀 𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟,𝑅𝑅𝑚𝑚
C=
𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟,𝑅𝑅𝑠𝑠

The reciprocal of resistance is conductance. It measures the ability to conduct a current and is expressed in
reciprocal of ohms i.e mhos. In water analysis generally micromhos is used. Knowing the cell constant, the
measured conductance is converted to the specific conductance or conductivity, Ks, as the reciprocal of the
specific resistance.

Ks = 1/Rs = C/R m

The term conductivity is preferred and usually reported in micromhos per centimeter (µ mhos/cm). Freshly
made distilled water has a conductivity of 0.5 to 2 .0 µ mhos/cm that increases after some days due to the
absorption of CO2 from atmosphere. The conductivity of potable waters varies generally from 50 to 1500 µ
mhos/cm. The conductivity of municipal waste waters may be near to that of the potable water. However,
10000 µ mhos/cm.

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Measurement of conductivity with lesser accuracy than laboratory analysis is done continuously by the field
recorders. These automatic recorders give idea about any sudden drastic change in the quality of raw water
or the waste water, so that required precautions may be taken.

Actually, the total dissolved solids in water can be estimated by measuring its conductivity and multiplying
it by an empirical factor. This factor varies from 0.55 to 0.9 depending upon the soluble components of water
and the temperature. This factor can be obtained for a system by observing the conductivity and the dissolved
solids and then it can be used for continuous monitoring.

Apparatus

1. Conductivity meter: This is an instrument consisting of a source of alternating current, a

Wheatstone bridge, a null indicator and a conductivity cell. Generally, an instrument capable of
measuring conductivity with an accuracy of 1 % or 1 µ mhos/cm is used. A thermometer capable
of reading up to 0.1 ˚C within a Range of 15 to 30˚C is used.

2. Conductivity Cell: Platinum-electrode type conductivity cells containing platinized electrodes

are used depending upon the expected range of conductivity. Non platinum- electrode type
conductivity cells containing electrodes constructed from durable metals like stainless steel are
used for continuous monitoring systems.

Reagents

(a) Conductivity of water: Pass distilled water through a mixed bed deionizer and discard first liter.
Conductivity should be less than 1 µ mhos/cm mg.

(b) Standard Potassium Chloride Solution (KCl, 0.01M), Dissolve 745.6 of anhydrous KCl in
conductivity water and dilute to 1000 ml at 25 ˚C. This the standard reference solution having a
conductivity of 1413 µmhos/cm at 25 ˚C, useful for the cell constants between 1 and 2.

(c) Procedure

1. Determination of Cell Constant

Wash the conductivity cell with 0.01 M KCl solution. Adjust the temperature of the standard KCl at 25±
0.1oC. Measure resistance of the KCl and note the temperature.

The Cell Constant, C = (0.001413) (RKCL) [1+0.0191(t-25)]

2. Conductivity Measurement

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Rinse cell with the sample. Adjust temperature of the sample to 25± 0.1oC. Measure sample resistance or
conductivity and the temperature. If the temperature deviates from 25oC the corrected conductivity shall be
as follows

𝐾𝐾𝑚𝑚 × 𝐶𝐶
K=
(1+0.019(𝑡𝑡−25))

Km is the measured conductivity at t oC.

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OBSERVATIONS AND CALCULATION:

Total dissolved solids

Electrical in mg/l= EC x ‘K’ (selected
Temperature conductivity
µmhos / cm
Water or measured ‘K’)
sample no.

Result:

The electrical conductivity of the given water sample is …. µ mhos/ cm

Viva questions

1. What is the purpose of determining the conductivity of the given water sample?

2. What are the factors that affect the conductivity of water?

3. Describe the experimental setup used for determining the conductivity of the water
sample.

4. How is conductivity measured in the experiment?

5. What is the significance of using a conductivity meter in this experiment?

6. How is the conductivity of the water sample affected by temperature?

7. How do you ensure the accuracy and precision of conductivity measurements?

8. Can you explain the principle behind the measurement of conductivity in water?

9. What are the units of conductivity commonly used in this experiment?

10. What precautions should be taken while handling the conductivity meter and water
samples during the experiment?

11. How can you minimize external interferences during conductivity measurements? 20

Prepared by: Dr N C Kothiyal & Dr B S Kaith

 Experiment No-6
Determination of Iron

Aim: To determine the quantity of iron present in the given sample of water.

Principle

Iron is usually present in natural water and is not objectionable, if concentration is less than 0.3
ppm. It may be in true solution in colloidal state that may be peptized by organic matter, in the
inorganic and organic iron complexes, or in relatively coarse suspended particles. It may be
either ferrous or ferric, suspended or filterable. Iron exists in soils and minerals mainly as
insoluble ferric oxide and iron sulphide (pyrite). It occurs in some areas, also as ferrous
carbonate (siderite), which is very slightly soluble.

The phenanthroline method is the preferred standard procedure for the measurement of iron in
water except when phosphate or heavy metal interferences are present. The method depends
upon the fact that 1, 10-phenanthroline combine with Fe++ to form an orange-red complex. Its
colour conforms to Beer‘s law and is readily measured by visual or photometric comparison.
Small concentration of iron can be most satisfactorily determined by colorimetric analysis. It
is also based on Beer‘s law. By measuring the intensities of transmitted and incident light
through a coloured solution and knowing its optical density or transmission, we can prepare a
calibration curve and subsequent concentration can be read.

Phenanthroline Method

Apparatus:

1. Colorimetric equipment; one of the following is required:

(a) Spectrophotometer, for use at 510 nm, providing a light path of 1 cm or longer.
(b) Nessler tubes, matched, 100 mL, tall form.
2. Glassware like conical flasks, pipettes and glass beads.

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conical flasks pipette

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Reagents

1. Hydrochloric acid

2. Hydroxylamine solution

3. Ammonium acetate buffer solution

4. Sodium acetate solution

5. Phenanthroline solution

6. Stock iron solution

7. Standard iron solution (1 mL = 10 µg Fe)

Procedure

1. Pipette 10, 20, 30 and 50 mL Standard iron solution into 100 mL conical flasks.
2. Add 1 mL hydroxylamine solution and 1 mL sodium acetate solution to each
flask.
3. Dilute each to about 75 mL with distilled water.
4. Add 10 mL phenanthroline solution to each flask.
5. Make up the contents of each flask exactly to 100mL by adding distilled water
and left stand for 10 minutes.
6. Take 50 mL distilled water in another conical flask.
7. Repeat steps 2 to 5 described above.
8. Measure the absorbance of each solution in a spectrophotometer at 508 nm
against the reference blank prepared by treating distilled water as described in
steps 6 and 7. Prepare a calibration graph taking meter reading on y-axis and
concentration of iron on x-axis.
9. For visual comparison, pour the solution in 100 mL tall form Nessler tubes and
keep them in a stand.
10. Mix the sample thoroughly and measure 50 mL into a conical flask.
11. Add 2 mL conc. hydrochloric acid (HCl) and 1mL hydroxylamine solution. Add
a few glass beads and heat to boiling. To ensure dissolution of all the iron,
continue boiling until the volume is reduced to 15 to 20 mL.

12. Cool the flask to room temperature and transfer the solution to a 100 mL Nessler
tube.

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 13. Add 10 mL ammonium acetate buffer solution and 2 mL phenanthroline
solution and dilute to the 100 mL mark with distilled water.

14. Mix thoroughly and allow at least 10 to 15 minutes for maximum colour
development.

15. Measure the absorbance of the solution in a 1cm cell in a spectrophotometer

at 508 nm.

16. Read off the conc. of iron (mg Fe) from the calibration graph for the
corresponding meter reading.

17. For visual comparison, match the colour of the sample with that of the standard
prepared in steps 1 to 7 above.

18. The matching colour standard will give the concentration of iron in the sample
(µg Fe).

Observation:

Sample no. Iron content in mg/L

1.

2.

3.

Standard iron solution in Iron content in micro Absorbance

ml gram.

Sample No. Absorbance Iron content graph in micro Iron as Fe in mg/L

gram

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Result: Iron (Fe) in mg/L = μg Fe/mL of sample = ......... mg/L

Viva Questions

1. What is the purpose of determining the quantity of iron in the given sample of water?

2. How can the presence of iron in water impact its quality and usability?

3. What methods can be used to determine the quantity of iron in a water sample?

4. Describe the process of sample preparation for iron analysis in water.

5. What is the principle behind the method used to determine the iron content in water?

6. What are the reagents and instruments required for the analysis of iron in water?

7. Explain the procedure for the colorimetric determination of iron in water.

8. How does the calibration curve help in quantifying the iron concentration in the sample?

9. What are the potential sources of error in iron analysis of water samples, and how can
they be minimized?

10. How can the results of the iron analysis in water be reported?

EXPERIMENT-7
DETERMINATION OF CHLORIDE CONTENT IN THE GIVEN WATER SAMPLE

AIM To estimate the amount of chlorides present in the given sample of water.

PRINCIPLE Chlorides ion is determined by titration with standard AgNO3 in which AgCrO4
precipitatesout. The end of titration is indicated by formation of red silver chromate from
excess AgNO3 and potassium chromate used as an indicator in neutral to slightly alkaline
solution.
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APPARATUS
1. Pipette
2. Burette
3. Conical flask etc.

REAGENTS
1. Potassium chromate (K2CrO4) indicator
2. Silver nitrate (AgNO3) of 0.0141N
PROCEDURE
1. Adjust the pH of sample between 7.0-8.0.
2. Standardize AgNO3 against standard NaCl solution.
3. Take 20ml well mixed sample and add 1.0ml of K2CrO4.
4. Titrate with standard AgNO3 solution till AgCrO4 starts precipitating.
5. For better accuracy titrate 20ml of distilled water in the same way to establish reagent
blank.
OBSERVATIONS

Volume of Burette reading Volume of Remarks

sample (ml) AgNO3
Initial (ml) Final (ml)
run down (ml)

CALCULATION

Chlorides (Cl-) in mg/l = (A-B) x N x 35.45/ml of

sample

Where

A = ml of AgNO3 run down for the sample

B = ml of AgNO3 run down for the blank
N = Normality of AgNO3 used 26

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 RESULTS
Chlorides present in the given sample = mg/l

VIVA QUESTIONS

1. What is the purpose of measuring the chloride content in water?

2. How is the chloride content in water determined in this experiment?

3. Can you explain the principle behind the method used to detect chloride in water?

4. What are the potential sources of chloride contamination in water?

5. How does the presence of chloride in water impact human health or the environment?

6. What safety precautions should be taken when handling chemicals and samples during
the experiment?

7. Are there any interferences or limitations associated with the chosen method for
chloride analysis?

8. How do you ensure the accuracy and precision of the results obtained in this
experiment?

9. Can you discuss any potential methods for chloride removal from contaminated water?

10. Are there any recommended guidelines or regulatory limits for chloride levels in
drinking water?
REFERENCES

• Standard methods for the examination of water and wastewater, 21st Edition,
Washington: APHA., 2012. 2.
• Sawyer, C. N., McCarty, P. L., and Perkin, G.F., Chemistry for Environmental
Engineering and Science, 5th edition McGraw Hill Inc., 2002.
• B. Kotaiah and Dr. N. Kumara Swamy, Environmental Engineering Laboratory
Manual, Charotar Publishing House Pvt. Ltd., 1st Ed., 2007.

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 EXPERIMENT: 8
Aim: Determine the total hardness in the given water sample.

Requirements:
Water sample
Burette
Glass funnel
Pipette
Titration Flask

Dropper

Measuring cylinder

Reagents: EDTA, Eriochrome Black-T, NH2CL, Ammonia Buffer, MagnesiumCarbonate,

90% ethyl alcohol, Distilled water
Introduction:

Hardness in water is due to the presence of dissolved salts of calcium and magnesium. It is
unfit for drinking, bathing, washing and it also forms scales in boilers. Hence it is necessary
to estimate the amount of hardness producing substances present in the water sample. Once
it is estimated, the amount of chemicalsrequired for the treatment of water can be calculated.
The estimation of hardness is based on complexometric titration. Hardness of water is
determined by titrating witha standard solution of ethylene diamine tetra acetic acid (EDTA)
which is a complexing agent. Since EDTA is insoluble in water, the disodium salt of EDTA
istaken for this experiment. EDTA can form four or six coordination bonds with a metal
ion. Two type of hardness is present in water first is temporary hardness and second is
permanent hardness. Temporary hardness is due to the presence ofbicarbonates of calcium
and magnesium ions. It can be easily removed by boiling. Permanent hardness is due to the
presence of chlorides and sulphates of calcium andmagnesium ions. This type of hardness
cannot be removed by boiling.

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.

Reagent preparation:
1. EDTA solution: 4gm EDTA and 0.1gm magnesium bicarbonate dissolve in 800 ml
distilled water.

2. Eriochrome Black-T: 0.4gm Ericrome Black T, 4.5 gm hydroxylmine hydrochloride add

in100 ml 95% ethyl alcohol.

3. Ammonia Buffer: Stock A: 16.9gm of NH4CL in 143ml of conc. NH4OH, Stock B:

1.25gm magnesium salt of EDTA dissolve in 50 ml distilled water. Mix both stock solutions
and dilute to 250ml with DDW. Dilute 10ml of the solution to 100ml with DDW.

Procedure:
1. The burette is filled with standard EDTA solution to the zero level.

2. Take 50ml sample water in flask. If sample having high Calcium content then take
smaller volume and dilute to 50ml.
3. Add 1ml Ammonia buffer.

4. Add 5 to 6 drop of Ericrome black – T indicator. The solution turns into winered
colour.
5. Note the initial reading.

6. Titrate the content against EDTA solution. At the end point colour changefrom
wine red to blue colour.
7. Note the final reading and record it. Repeat the process till we get concordant
value.
8. Take 50ml sample in another flask and boil it to remove temparory hardness.
(Add distilled water to getfinal volume of water.)

9. Repeat step 3-7.

Calculations:

S.No. Water sample (50ml) Initial Value Final Value Ml of EDTA

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 3

Total hardness of water mg/L (CaCO3 Scale) = ml of EDTA used (unboiled) *103/ml of
sample

Permanent hardness of water mg/L (CaCO3 Scale) = ml of EDTA used (boiled)*103 /ml of
sample

Temporary hardness of water mg/L (CaCO3 Scale) = Total hardness of water -Permanent
hardness of water

Observation:
The colour of soluble distilled water and R.O water instantly changed into blue while tap water
and pond water turned wine red when Ericrome black T was added and therefore after turned
blue when titrated against EDTA solution.

Result:
The collected water sample contains Total hardness = ppm Permanent
hardness = ppm
Temporary hardness = ppm
Viva Questions:
Q1. What is hardness of water?
Q2. How do you differentiate hard water from soft water?
Q3. What are the types of hardness? How are they caused?
Q4. How hardness of water is expressed?
Q5. What are buffers?
Q6. Give an example for acidic buffer and basic buffer.
Q7. What is standard solution?
Q8. Name the deposition formed when hard water is boiled? Write its reaction.
Q9. Why and how pH is maintained in the experiment?
Q10. Name the deposition formed when hard water is boiled? Write its reaction.
Q11. Why disodium salt of EDTA is used instead of EDTA in determining the total hardness
of water?

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 EXPERIMENT: 9
Aim: Removal of toxic dyes from textile effluent using adsorbents

Requirements:
Dye
Absorbent
Distilled water
UV-Spectrophotometer
Stirrer
Thermostat
Beaker
Volumetric flask

Introduction:
Dyes are colored compounds which are widely used in textiles, printing, rubber, cosmetics,
plastics, leather industries to color their products results in generating a large amount of colored
wastewater. The presence of chromophores in dyes account for the development of color,
which auxochromes are attached to. The multifaceted applications of dyes in daily life involve
their release together with other toxic organic/inorganic chemicals from industrial effluents,
resulting in detrimental effects on the environment. Adsorption is a surface phenomenon which
deals primarily with the utilization of surface forces. Adsorption is used as top-quality
treatment procedures for the removal of dissolved organic pollutants like dyes from industrial
wastewater. Adsorption is defined as concentration of materials on the surface of solid bodies.
Dyes from textile wastewater can be separated by using adsorbent as fly ash. Also, activated
carbon-based adsorbents are widely used in the field of adsorption of dyes due to their unique
characteristics such as internal pore morphology, surface characteristics, porosity, pore
volume, chemical structure,

Principle:
Ultraviolet-visible (UV-vis) spectroscopy is used to obtain the absorbance spectra of a
compound in solution. Ultraviolet-visible (UV-vis) spectroscopy work on The Beer-Lambert
law.

1. A light source, 31

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2. Some optics for focusing the light,
3. A coloured filter, which passes light of the colour which is absorbed by the treated sample,
4. A sample compartment to hold a transparent tube or cell containing the sample and
5. A light-sensitive detector

Beer-Lambert Law:
The Beer-Lambert Law relates the absorption of light at a particular wavelength to the
concentration of the substance that is absorbing the light as follows:
A= 𝜀𝜀𝜀𝜀𝜀𝜀
Where, A is the absorption at a particular wavelength. ε is the molar absorption coefficient for
the compound at the wavelength at which the absorption is measured and is characteristic for
the compound. This constant is a measure of how strongly a compound absorbs at a particular
wavelength. c is the concentration of the compound and is independent of wavelength. l is the
path length of the test tube used to hold the sample

Procedure:
1. An accurately weighed quantity of the dye is dissolved in double-distilled water to prepare
a stock solution (100ppm)
2. Experimental solutions of the desired concentrations(10ppm) are obtained by successive
dilutions
3. A weighed quantity of the adsorbent is kept in contact with an appropriate concentration of
the dye solution and measured volumes are withdrawn at different intervals of time. For this
purpose, 1 g silica gel is used for 100 ml dye solution of 10ppm concentration.
4. The adsorbent-adsorbate system is kept in a thermostat at 30 + 0.1°C and is shaken
continuously
5. At suitable time intervals, shaking is done so that the necessary withdrawals of the sample
solution (5 ml) can be made; these are later used for the determination of the concentration
remaining in solution. The progress of adsorption at various time intervals is measured by a
spectrophotometer
6. The amount present on the surface of the absorbent is determined by the difference of the
initial and remaining concentrations of dye solution
7. The experiments are carried out by varying the amount of the adsorbent, the temperature,
and the concentration of the dye solution
8. Amount of dye taken up at various intervals of time is plotted.
Observations:
Sr.no. Time (min.) Absorbance (a.u.)
1. 0
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 2. 10
3. 20
4. 30
5. 40

Initial absorbance of dye = x

Final absorbance of dye = y
𝑥𝑥−𝑦𝑦
Percentage of dye removed (z)= %
𝑥𝑥

Results:
Percentage of dye removed from the textile = z
Precautions:
1. All the measurements were made at a wavelength corresponding to the maximum absorbance
2. All measurement must be carried out at same time interval
3. Temperature must be kept constant
4. all solutions

Viva questions:
Q1. What are dyes? How are these released in environment?
Q2. What are the different types of dyes?
Q3. Why dye removal is important?
Q4. What are adsorbents? What are their properties?
Q5. What are the other methods that can be used for dye removal?
Q6. What is the principle of UV spectrophotometer?
Q7. What is the wavelength range of visible region?
Q8. What are different sources of dyes in environment?

1. Soumi Dutta;Bramha Gupta;suneel Kumar srivastava;Ashok Kumar Gupta; (2021). Recent

advances on the removal of dyes from wastewater using various adsorbents: A critical review
. Materials Advances, (), –. doi:10.1039/d1ma00354b
2. M.N. Ahmed; R.N. Ram (1992). Removal of basic dye from waste-water using silica as
adsorbent. , 77(1), 79–86. doi:10.1016/0269-7491(92)90161-3

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 EXPERIMENT: 10

Aim: Removal of heavy metals from industrial effluent using adsorbents

Requirements:
Heavy metal solutions
Absorbent
Distilled water
Spertrophotomter
Sonicator
Stirrer
Beaker

Introduction:
The most popular heavy metals are lead (Pb), zinc (Zn), mercury (Hg), nickel (Ni), cadmium
(Cd), copper (Cu), chromium (Cr), and arsenic (As) which are highly toxic. The adsorption
mechanism is defined by the physicochemical properties of adsorbent and heavy metals and
operating conditions. Generally, heavy metal ions can be adsorbed onto the adsorbent’s surface.
Carbon-based nanoporous adsorbents, especially activated carbons (ACs), carbon nanotubes
(CNTs), and graphene (GN), are extensively used in the applications of heavy metal removal
owing to their tremendous surface area.

Procedure:
1. Stock solution of heavy metal ions is prepared(1.0 × 10 -3 M)
2. Experimental solutions of the desired concentrations are obtained by successive dilutions
20 mg of Absorbent is added to 20 ml of different concentrations of heavy metal standard
solutions (30, 50, 100 & 200 ppm)
3. The solution is sonicated for 20 min. at 100 rpm and then allowed to cool and followed by
equilibration at room temperature for 24 hrs
4. Solids is allowed to settle down and were removed using syringe filtration
5. The residual heavy metals is determined by atomic absorption spectrophotometer (AAS)
analysis
6. The adsorption isotherms is obtained by increasing the concentration of heavy metal
solutions from 50 up to 200 ppm
7. The removal percentage of the adsorbed heavy metal concentration is estimated

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Precuations:

1. All the measurements were made at a wavelength corresponding to the maximum absorbance

2. All measurement must be carried out at same time interval

3. Temperature must be kept constant

Viva questions:
Q1. How heavy metal ions are released in environment?
Q2. Name some heavy metal ions which are toxic to the environment.
Q3. Different methods that can be utilized to remove heavy metals from the wastewater?
Q4. Why is it important to remove heavy metal ions from the environment?
Q5. What are adsorbents? What are their properties?
Q6. How toxic heavy metal ions are released in environment? State their sources and toxicity.

1. Arora, Rajeev (2019). Adsorption of Heavy Metals–A Review. Materials Today:

Proceedings, 18(), 4745–4750. doi:10.1016/j.matpr.2019.07.462

2. Karnib, Mona; Kabbani, Ahmad; Holail, Hanafy; Olama, Zakia (2014). Heavy Metals
Removal Using Activated Carbon, Silica and Silica Activated Carbon Composite. Energy
Procedia, 50(), 113–120. doi:10.1016/j.egypro.2014.06.014

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