Department of Civil Engineering.

Indian Institute of Technology (ISM), Dhanbad

Laboratory Manual
Part-1

B. Tech (Civil Engg.) – 3rd Semester

Monsoon Semester (2020-2021)

CEC205: Environmental Engineering Laboratory
 LABORATORY GUIDELINES
1. The class will be divided into groups of 4-5 students working together in the lab and writing
the laboratory reports. Each group will submit only one lab report. Always bring a lab manual,
calculator, and lab notebook.
2. All lab data will be entered on a sheet of paper and checked with a Teaching Assistant before
attaching it with the lab report. The lab report will be submitted in the laboratory itself.
Lab Safety: Students without shoes will not be allowed in the lab. Bring lab coat and a
permanent marker to lab. Always wear full sleeves clothes. Wear safety glasses and gloves
when recommended. Leave bags and coats in designated areas. Bring only the essentials to the
lab bench. No eating, drinking, playing, or applying cosmetics (including hand lotion, etc.).
Never use broken or chipped glassware. Place broken glassware in specially marked containers.
Mouth pipetting is forbidden. Hands should be washed after contact with hazardous materials
and before leaving the lab.
Lab Etiquette: Return all chemicals and supplies to the proper location after use. It is necessary
to take chemicals from reagent bottles, pour out slightly more than the chemical needed into a
clean beaker. Never pour a chemical back into a reagent bottle. Clean up for the next person.
After each work period, all used glassware must be cleaned and set to drain. Remove label
tape, scrub inside of glassware with water and laboratory detergent, rinse with tap water, rinse
with distilled water, and place cleaned glassware on a rack to dry. No experiment is complete
until the laboratory is cleaned.

Lab Safety Do’s and Dont’s

Things to do:
1. Be on time. At the start of the lab period, there will be a short introduction to the experiment
you will perform that day.
2. Inform the TA/Instructor in case you find any difficulty while performing the experiment.
3. Be aware of all safety devices. Also, the instructor/TA will help you in case of any emergency.
4. Always be in proper well-cleaned lab coats as well as shoes.
5. Dispose of all chemicals, broken glass, and other lab materials into the proper containers as
directed by the instructor.

Things not to do:

1. Do not put pieces of lab equipment in your mouth.
2. Do not work with chemicals until you are sure of safe handling.
3. Do not use the phone or computer with gloves on your hands.
4. Never add water to acid.
5. Never smell, taste, or touch the chemicals.
6. Absolutely NO HORSEPLAY is allowed in the lab area!

Course Course Name of the course L T P Credit

Type Code

DP 2 CEC205 Environmental Engineering 0 0 2 2

Laboratory
Course Objective
The subject offers the readers a fundamental understanding of the water quality parameters and its role in
environmental engineering.
To describe methods of advanced effluent treatment for higher discharge standards and effluent re-use.
Learning Outcomes
After studying this course, students should be able to:
● Understand the water quality parameters and the significance.
● Understanding the operational condition during project work.
Expt Learning
Topics to be Covered Laboratory
No. Outcome
Calibration of pH meter, TDS and conductivity meter and Determination of
1 pH, TDS and conductivity of a given water sample. 1

2 Determination of Turbidity and Sulphate in given water sample 1

Understand
3 Determination of acidity and Alkalinity of given water sample. 1 the water
4 Determination of hardness, Chloride of given water sample. 1 quality
5 Determination of optimum coagulant dose using jar test. 1 parameters
6 Determination of optimum lime soda dose for hardness removal 1 and the
Determine DO, BOD and COD and biodegradability index of a given significance.
7 1 Understanding
wastewater Sample.
the operational
Determine the ammonical nitrogen and TKN concentration in the given
8 1 condition
wastewater samples. during project
9 Determine TS, TSS, VSS and FS in the given sludge samples. 1 work.
10 Determine the oil and grease content in given wastewater samples. 1 .
11 Determine the CNP ratio in the given wastewater sample. 1
Determine the MLVSS, MLSS, SVI and VSS/SS ratio of a given sludge
12 2
sample.
Text Books/References:

1. Relevant Indian and International Standard code of practice.

2. Manual for Environmental Engineering Laboratory.
 Experiment 1: Calibration of pH meter, TDS, and
conductivity meter and Determination of
pH, TDS, and conductivity of a given
water sample.

1a. Calibration of pH meter and Determination of pH of water sample

Aim: - To determine the pH of a given water sample with the stipulations.

METHOD USED

Apparatus

PH meter: Consisting of a potentiometer, a glass electrode, a reference

electrode, and a temperature compensating device. A balanced circuit is
completed through a potentiometer when the electrodes are immersed in
the test solution. Many pH meters are capable of reading pH or millivolt.

Standard solutions for calibration

Buffer solution of known pH i.e., 4.0, 7.0 & 9.2.

SIGNIFICANCE OF TEST/ PARAMETER

pH is one of the most important tests in almost every phase of environmental

engineering practice. Many chemical and biochemical reactions take place at a
specific pH value or within a narrow pH range. For example, control of pH is
particularly important in the chemical coagulation of water, disinfection, water
softening and corrosion control, etc. In wastewater treatment employing
biological processes, pH must be controlled within a range favorable to the
particular organism involved.
The pH is determined by measurement of the electromotive force (emf) of a cell
comprising of an indicator electrode (an electrode responsive to hydrogen ions
such as glass electrode) immersed in the test solution and a reference electrode
(usually a calomel electrode). Contact is achieved through a liquid junction,
which forms a part of the reference electrode. The emf of this cell is measured
with a pH meter. Since the pH is defined operationally on a potentiometric
scale, the measuring instrument is also calibrated potentiometrically with an
indicating (glass) electrode.

The pH of a solution denotes the intensity of the acidity or Alkalinity of a

solution and is defined by the relationship:

PH = - log10 [H+], where [H+] = the concentration of Hydrogen ions in moles.

The pH scale runs from 0.0 to 14, with 7.0 being neutral. Most of the
surface water pH ranges from 6.0 to 8.5. The pH can be measured either
by the indicator method or by the electrometric method using a pH
meter.

The electrometric method requires a pH meter, which is a sensitive

instrument to monitor the millivolts generated by Hydrogen ions and
enable the conversion of produced millivolts to corresponding equivalent
pH value in the digital format.

Calibration of pH meter

o Switch on the pH meter at least 15 minutes prior to the measurement.

o Wash the electrode with distilled water and wipe the same with tissue
paper.
o Keep the sample on a magnetic stirrer and stir continuously at
low rpm (there should be enough space between the probe and the
pellet).
o Dip the electrode in the buffer solution carefully and adjust the
temperature knob to the buffer's liquid temperature if the meter is
not equipped with automatic temperature adjustment.
o Turn the knob in pH mode and note the digital reading on the
meter. If the noted reading is approximately equal to the pH of the
standard buffer solution used for calibration, then the instrument
 is in order.
o If not, adjust the reading to the pH of the buffer solution by pH
adjustment knob.
o Select a minimum of two buffers for calibration within the range of
pH of the sample being measured.

PROCEDURE

1. Calibrate the pH meter by following the above procedure. Make

sure that buffers are being equilibrated to ambient temperature
and stirred when you perform the calibration. Also, ensure
through rinsing of pH probe with distilled water and blot dry prior
to change of buffers. Normally, two buffers are chosen for
calibration. Eg: When pH of sample is expected to be in acidic
range; select buffers 4 and 7, if in basic range; select buffers 7
and 9.2.

2. Once calibrated, the probe should be rinsed and dried with a soft
tissue paper before every sample analysis.

3. During sample analysis, the sample should be mixed continuously

(manually or mechanically). Extreme care should be taken while
mixing to avoid electrode breakage.

4. Observe the values and record.

5. Rinse the probe when you finish the measurement and leave the
probe immersed in pH 7 buffer solution for storage.

Caution: Never leave the probe in dry condition, always dip in buffer

solution.
OBSERVATION AND CALCULATION

Table1 Result of pH values of water/wastewater samples

S.NO SAMPLE TEMPTERATURE pH READING

 1b. Calibration of conductivity and TDS meter and Determination of
conductivity and TDS of water sample

Aim: To determine the Conductivity and TDS of the given sample

Theory: Conductivity is the capacity of water to carry an electrical current and
varies both with the number and types of ions the solution contains, which is
related to the concentration of ionized substances in the water. Most dissolved
inorganic substances in water are in the ionized form and hence contribute to
conductance. Conductivity measurement gives a rapid and practical estimate of
the variations in the dissolved contents of water.
The TDS is typically used to estimate the amount of total dissolved solids in the
sample. To determine the conversion factor for a specific solution of a known
TDS value, measure the solution's conductivity, and divide the mg/L TDS value
by the conductivity value reported. For example, a solution of a known TDS
value of 64 g/L and the measured conductivity value of 100 mS/cm has a
conversion factor of 64/100 or 0.64.
Environmental Significance:
Electrical conductivity measurements are often employed to monitor
desalination plants. It is useful for the detection of impurities in water. Used
for quantitative measurement of ionic constituents dissolved in water, which
are important for boiler feed water and cooling water, etc.; Used for checking
the correctness of water analysis as there is a distinct relationship between
conductivity and total dissolved solids (TDS). Conductivity data is useful in
determining the suitability of water and wastewater for disposal on land.
Irrigation waters up to 2 milli Siemens/cm conductance have been found to be
suitable for irrigation depending on soils and climatic characteristics.
Requirements: Conductivity/TDS Meter, Flask, Beaker, Wash Bottle
Reagents:
0.01 N, KCL solution: Dissolve 0.0746 grams of potassium chloride in 100 ml
of distilled water.
1. Switch on the electronic balance. Keep the weighing pan and set the
reading to zero.
2. Measure 100 ml of distilled water and transfer it to the beaker.
3. Weigh 0.07456 gram of Potassium Chloride (KCl).
4. Transfer 0.07456 gm of KCl to the beaker containing 100 ml of distilled
water and mix it by the glass rod thoroughly.
Procedure:
1. Rinse the electrode thoroughly with blot and dry.
2. Calibrate the instrument by measuring the conductivity/TDS of a
standard solution with known conductivity/TDS value.
3. Immerse the electrode in 0.01 N KCL solution, and the conductivity
should be 1413 micromhos at 25°C Temperature.
4. Now the instrument is calibrated.
5. Remove the cell from the KCl solution and wash it thoroughly with
distilled water.
6. Immerse the electrode/cell in the unknown sample whose
conductivity/TDS is to be determined.
7. Note down the instrument reading. If the cell constant is given on the
cell itself, then the measured value of conductivity = Cell Constant ‘C’ X
Screen reading
8. Change the mode of the instrument and measure the TDS of the sample.
Conductivity Cell Constant = Specific conductance / Measured
conductance.
Conversion factor for TDS = TDS of the standard sample / Specific
conductance
Specific conductivity of the given sample = Cell constant x Measured
conductance.
TDS of the given sample = Conversion factor x Specific conductivity of
the sample

RESULT

Table1: Result of conductivity/TDS of water/wastewater samples

S.NO SAMPLE CONDUCTIVITY TDS

Experiment 2: Determination of Turbidity and Sulphate
in given water sample

2a. Determination of Turbidity in given water sample

Aim: - To determine Turbidity of a given water sample

Introduction:
Turbidity is the technical term referring to the cloudiness of a solution, and it
is a qualitative characteristic that is imparted by solid particles obstructing the
transmittance of light through a water sample. Turbidity often indicates the
presence of dispersed and suspended solids like clay, organic matter, silt,
algae, and other microorganisms. So, in short, Turbidity is an expression of the
optical property that causes light to be scattered and absorbed rather than
transmitted in straight lines through the sample.
Environmental significance:
When the turbid water in a small, transparent container such as a 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 organisms that may not be
harmful. They may be harmful or cause undesirable tastes and odors.
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
colors to water and may interfere with light penetration and photosynthetic
reaction in streams and lakes. Turbidity increases the load on slow sand filters.
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 help to gauge the amount of
chemicals needed from the day-to-day operation of water treatment works.
Measurement of Turbidity in settled water prior to filtration is useful in
controlling chemical dosages so as to prevent excessive loading of rapid sand
filters. Turbidity measurements of the filtered water are needed to check on
faulty filter operation. Turbidity measurements are useful to determine the
optimum dosage of coagulants to treat domestic and industrial wastewaters.
Turbidity determination is used to evaluate the performance of water treatment
Plants. Turbidity in water may be caused by a wide variety of suspended
matter, such as clay, silt, and finely divided organic and inorganic matter,
soluble colored organic compounds, and other organisms. Under flood
conditions, great amounts of topsoil are washed to receiving streams. As the
rivers pass through urban areas, the domestic and industrial wastewaters may
be added.
Guideline:
According to WHO standard, 5 NTU is suggested as the turbidity limit for
drinking water, while 1 NTU is recommended to achieve the adequate
disinfecting safety. According to Bangladesh Environment Conservation Rules
(1997), drinking Water standard for Turbidity is 10 NTU (Nephelometric
turbidity unit).
Principle:
Turbidity is based on the comparison of the intensity of light scattered by the
sample under defined conditions with the intensity of the light scattered by a
standard reference suspension under the same conditions. The Turbidity of the
sample is thus measured from the amount of light scattered by the sample
taking a reference with standard turbidity suspension. The higher the intensity
of scattered light, the higher is the Turbidity. Formazin polymer is used as the
primary standard reference suspension.
Because of the wide variety of materials that cause Turbidity in natural waters,
it has been necessary to use an arbitrary standard. The original standard
chosen was; 1 mg SiO2/l =1 unit of Turbidity. The Silica used had to meet
certain specifications as to particle size. The Jackson candle turbidimeter has
been replaced by more reliable, sensitive, and easier to use instruments that
depend upon the principle of nephelometry. As a standard reference material,
Silica has been replaced by Formazin polymer. The Formazin suspensions were
first calibrated against the Jackson candle turbidimeter. The standard
nephelometry procedure is now reported in nephelometric turbidity units
(NTU). Because of the basic principles difference for Jackson candle
turbidimeter and nephelometric methods, results from the two methods can
vary widely. To avoid any confusion this may cause, turbidity measurements by
the standard nephelometry procedure are now reported in nephelometric
turbidity units (NTU), and the other one is reported in Jackson candle
turbidimeter units (JTU).
40 NTU is about equivalent to 40 JTU.
The applicable range of this method is 0-40 nephelometric turbidity units
(NTU). Higher values may be obtained with the dilution of the sample.
Sample handling and preservation:
Water samples should be collected in plastic cans or glass bottles. All bottles
must be cleaned thoroughly and should be rinsed with Turbidity free water.
The volume collected should be sufficient to ensure a representative sample,
allow for replicate analysis (if required), and minimize waste disposal. No
chemical preservation is needed. Do not allow samples to freeze. The analysis
should begin as soon as possible after the collection. If storage is required,
samples maintained at 4°C may be held for up to 48 hours.
Precautions:
The following precautions should be observed while performing the experiment:
 The presence of colored solutes causes a reduction in the measured
turbidity values. Precipitation of dissolved constituents (for example,
Fe) causes measured turbidity values to be high.
  Light absorbing materials such as activated carbon in significant
concentrations can cause low readings.
 The presence of floating debris and coarse sediments that settle out
rapidly will give low readings. Finely divided air bubbles can cause
high readings.

Apparatus:
1. Turbidity Meter
Chemicals
1. Formazin Polymer standards

Procedure:
1. The turbidity meter is required to be calibrated.
2. To the sample cells, add sample water up to the horizontal mark, wipe
gently with soft tissue and place it in the turbidity meter. Cover the
sample cell with the light shield.
3. Check for the reading in the turbidity meter. Wait until you get a stable
reading.
Result:

Sample No: Temperature (0C) Turbidity (NTU)

2b. Determination of Sulphate in given water sample.

Aim: To determine the amount of sulphate present in the given sample by the
gravimetric method.
Principle:
The sulphate in water is precipitated as Barium Sulphate by adding Barium
Chloride in hydrochloric acid medium. The precipitated matter is filtered,
washed free of Chloride, ignited, and weighed as barium sulphate. The reaction
taking place is provided below.
Na2SO4+BaC1---------------->BaSO4+2NaCl
The hydrochloric acid is added first to remove any carbonate ions that might be
present they would also produce a white precipitate, giving a false-positive
result. The reaction of Barium Sulphate with carbon in the water is as follows.
BaSO4+2C--------------------- >BaS+2C0 2
BaS+2O------------------------- >BaSO 4
Apparatus Required:
Crucible, Oven, weighing balance, pipette, beaker, water bath,
desiccators.
Reagents Required:
Dilute HCL
Solid Ammonium Chloride
1O%Barium Chloride solution
Reagents Preparation:
Barium Chloride Solution:
Dissolve l0g of Barium Chloride in 100 ml of distilled water.
Procedure:
1. Pipette out 5Oml of the sample into a clean 250m1 beaker.
2. Add 10 ml of dilute HCL & 1gm of solid ammonium chloride.
3. Heat to boiling & add l0ml of 10% Barium Chloride solution drop by drop
with constant stirring. Continue boiling for another 2 to 3 minutes.
 4. Allow the precipitate to settle and test for completion of precipitation by
adding a small amount of Barium Chloride solution through the sides of
the beaker.
5. If any turbidity is noticed, add a sufficient quantity of barium chloride to
precipitate all the sulphate.
6. Transfer-the contents to a sand bath & digest for half an hour to promote
granulation of the precipitate.
7. Filter through Waliman no 42 filter paper and wash with boiling water till
the filtrate runs free of chlorine.
8. Transfer the filter paper along with the precipitate to a weighed silica
crucible and dry it in an air oven.
9. Ignite over a low flame initially, taking care to ash the filter paper
completely, then ignite strongly over a rose head flame to constant
weight.
10. From the weight of Barium Sulphate obtained, calculate the
Sulphate content of the sample.

RESULT

𝑀𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑆𝑢𝑙𝑝ℎ𝑎𝑡𝑒 𝑖𝑜𝑛

411.6 = 𝑥100
𝑀𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑜𝑓 𝐵𝑎𝑟𝑖𝑢𝑚 𝑆𝑢𝑙𝑝ℎ𝑎𝑡𝑒

The sulphate concentration of the given water sample = ……….. Mg/L.

Experiment 3: Determination of Acidity and Alkalinity of given
water sample

3a. Determination of Acidity of given water sample

Aim: - To measure mineral and phenolphthalein acidity of water sample

SIGNIFICANCE OF TEST/PARAMETER

Acids contribute to corrosiveness and influence chemical reaction

rates, chemical speciation, and biological processes. The acidity of
water is its quantitative capacity to react with a strong base to a
designated ph. The measured value may vary significantly with the
endpoint pH used in the Determination. When the chemical
composition of the sample is known to study mineral acids, weak
acids such as carbonic and acetic and hydrolyzing salts such as iron
or aluminum sulfate may contribute to the measured acidity
according to the method of Determination.

Mineral acidity: It is measured by titration to a pH of about 3.5, the

methyl orange endpoint (also known as methyl orange acidity).

Total acidity: Titration of a sample to the phenolphthalein endpoint

of pH 8.3 measures mineral acidity plus acidity due to weak acids.
Thus this is called total acidity (or phenolphthalein acidity). This test
does not bear significant importance in water analysis because methyl
orange acidity invariably remains absent in the raw water, and even
phenolphthalein acidity (that too principally due to the excessive-
prevalence of dissolved carbon dioxide and carbonic acids) normally
does not exist to a significant extent in the raw water.

PROCEDURE

Reagents: Sodium hydroxide titrant (0.02 N); Phenolphthalein Indicator; Methyl

Orange.

Steps

1. Take a 50 ml sample in a conical flask and add 2-3 drops of

methyl orange indicator solution.
2. Fill the burette with 0.02 N NaOH solutions and titrate until the
solution's color changes to faint yellow color, indicating the
endpoint. Record the volume of titrant consumed as V1 in ml.
Calculate the methyl orange acidity using Eq (1a):

Methyl orange acidity (or Mineral Acidity) = (V1×1000)/ (Sample volume)

(1a)

When the 0.02 N NaOH solution, used in titration is not standardized to

0.02 N, mineral acidity is calculated using following Eq (1b):
Methyl orange acidity= (V1×N×50×1000)/ (Sample vol.) (1b)

VOLUME OF 0.02N NaOH

VOLUME OF
S.NO
SAMPLE METHYL ORANGE PHENOLPHTHALEIN
INITIAL
POINT (V1) POINT (V2)

Phenolphthalein Acidity Test

1. For the phenolphthalein acidity test, add 2-3 drops of

phenolphthalein indicator solution to the water sample from step 2 and
continue the titration till the faint pink color develops in the solution (i.e., the
endpoint of titration). Record the volume of titration consumed as V2 (mL) and
calculate total acidity or phenolphthalein acidity using Eq. (2):

Total acidity (or Phenolphthalein Acidity) = (V2×N×50×1000)/ (Sample vol.)

(2).
3b. Determination of Alkalinity of given water sample

Aim: - To determine the Alkalinity of a given water sample.

SIGNIFICANCE OF TEST/PARAMETER

Alkalinity of water is the measure of its acid-neutralizing capacity. It is the sum

of all the titratable bases. Alkalinity is significant in many uses and treatments
of natural waters and wastewaters. Because the Alkalinity of many surface
waters is primarily a function of carbonate, bicarbonate, and hydroxide
content, it is taken as an indication of the concentration of these constituents.
The measured values also may include contributions from borates, phosphates,
silicates, or other bases if these are present. Alkalinity in excess of alkaline
earth metal concentrations is significant in determining the suitability of water
for irrigation. Alkalinity measurements are used in the interpretation and
control of water and wastewater treatment processes. Raw domestic
wastewater has an alkalinity less than, or only slightly greater than, that of the
water supply. Properly operating anaerobic digesters typically have
supernatant alkalinities in the range of 2000 to 4000 mg calcium carbonate
(CaCO3)/L.

Alkalinity Relationships

1. Carbonate (CO3)-2alkalinity is present when phenolphthalein alkalinity is

not zero but is less than total Alkalinity.

2. Hydroxide (OH) ¯ alkalinity is present if phenolphthalein alkalinity is

more than half the Total Alkalinity.

3. Bicarbonate (HCO3) ¯ alkalinity is present if phenolphthalein alkalinity is

less than half the total Alkalinity.

These relationships may be calculated by the scheme shown in Table 2, where

P is phenolphthalein alkalinity, and T is total Alkalinity. Select the smaller
value of P or (T – P). Then, carbonate alkalinity equals twice the smaller value.
When the smaller value is P, balance (T – 2P) is bicarbonate. When the smaller
value is (T-P), the balance (2P-T) is hydroxide. All results are expressed as
CaCO3. The mathematical conversion of the results is shown in table 2.

Apparatus

PH Meter, burette, pipette, measuring cylinders, conical flasks.

Reagents

 Standard sulfuric acid, 0.02N

 Phenolphthalein Indicator

 Methyl Orange Indicator

PROCEDURE

1. Rinse and fill a burette with a standard acid solution.

2. Measure 100 ml or an appropriate portion of water sample

diluted to 100 mL into a clean, sample-rinsed graduated
cylinder; transfer it to a conical flask. (If the sample is highly
alkaline dilute the sample -titration goes over one burette full).

3. Add 1- 2 drops of phenolphthalein (P) indicator and if the

solution turns pink, titrate until the color disappears. Note the
burette reading (P).

4. Add 1- 2 drops of methyl orange indicator to this same water

sample and continue the titration until the color changes from
yellow to orange. Note the burette reading (T).
Note: If pink color does not appear after addition of Phenolphthalein indicator,
continue titration as explained earlier.
 VOLUME OF 0.02N H2SO4

VOLUME
S.NO
OF METHYL
PHENOLPHTHALEI
SAMPLE INITIAL ORANGE
N POINT (P)
POINT (M)

Phenolphthalein alkalinity as CaCO3 in mg/l = (V1*N of

H2SO4*50*1000)/Vol. of sample.

Total alkalinity (M. Alk) as CaCO3 in mg/l = (V2*N of H2SO4*

50*1000)/Vol. of sample

Table 2 Summary of type and Alkalinity in water

Hydroxide Carbonate Bicarbonate

Result of
Alkalinit Alkalinit Concentratio
Titration
y as y as n as CaCO3
CaCO3 CaCO3
P=0 0 0 T
P < ½T 0 2P T – 2P
P = ½T 0 2P 0
P > ½T 2P – T 2(T – P) 0
P=T T 0 0
RESULTS

P. Alkalinity as CaCO3 (mg/L)

"M.O." or Total Alkalinity as CaCO3 (mg/L) _________

(OH)- Alkalinity as CaCO3 (mg/L)

(CO3)2- Alkalinity as CaCO3 (mg/L)

(HCO3)- Alkalinity as CaCO3 (mg/L)

Experiment 4: Determination of hardness, Chloride of
a given water sample.

4a. Determination of hardness of water sample.

Aim: To determine the hardness of a given sample of water or wastewater.

Theory: Originally, water's hardness is a measure of soap consuming
capacity to produce foam or lather. Hardness produces scale in hot water
pipes, heaters, boilers, and other units precipitated chiefly by Calcium and
Magnesium ions commonly present in water. Also maybe precipitated by
ions of other polyvalent metals such as Aluminium, Iron, Strontium, and
Zinc and by Hydrogen ions. Calcium and Magnesium ions are usually
present in significant concentrations in natural water. The hardness of
water varies from place to place. Surface waters are softer than the
groundwater. Hardness is due to the dissolved salts of Carbonates,
Bicarbonates, Chlorides, Sulphate, Nitrates of Calcium, and Magnesium.
Temporary hardness is mainly due to Carbonate and Bicarbonate of
Calcium and Magnesium. Permanent hardness is mainly due to Sulphate
and Chlorides.
A small amount of dye Eriochrome Black –T is added to hard water
containing Calcium and Magnesium ion, the solution will become wine red.
EDTA is then added as a titrant. Complexes of Calcium and Magnesium are
formed after sufficient EDTA has been added. The solution turns from Wine
Red to Blue. This is the endpoint of the titration. A pH value of 10.2 is
usually maintained.
The degree of hardness of drinking water has been classified in terms of the
equivalent CaCO3 concentration as follows:
Soft: 0 - 60 mg/L.
Medium: 60 - 120 mg/L.
Hard: 120 -180 mg/L
Very hard: > 180 mg/L.
Environmental Significance:
  Scales are formed as the inner coating of the pipelines prevents
corrosion.
 Soft waters are corrosive and dissolve the metals.
 More cases of cardiovascular diseases are reported in soft water areas.
 Hard water is useful to the growth of children due to the presence of
calcium.
 Hard waters cause excessive consumption of soap used for cleaning
purposes. Sodium soaps react with multivalent metallic cations to
form a precipitate, thereby lose their surfactant properties. Lathering
doesn’t take place until all hardness ions precipitate out.
 This precipitate adheres to surfaces of tubes, sinks, dishwashers, and
may stain clothing.
 Scales formed mainly due to carbonate hardness act as insulations
and cause enormous fuel loss in the boiler.
 Scales deposited mainly due to an increase in pH to 9 at which
bicarbonates are converted as carbonates are formed in distribution
mains reducing their carrying capacity.

Apparatus: Titration Stand with Burette, Conical Flask, Beaker, Measuring

Cylinder, Pipette, Funnel, Wash Bottle, etc.
Reagents:
 Standard EDTA solution 0.01 M (0.02N): Dissolve 3.723 gm EDTA
disodium salt and dilute to 1000 ml distilled water.
 Eri0chrome black T indicator: Mix 0.5gm dye with 100 gm NaCI to
prepare dry powder or mix 0.5 gm of indicator in 100 ml of Ethyl
Alcohol.
 Ammonia Buffer solution: Dissolve 16.9g Ammonium Chloride
(NH4CI) in 143 ml of Ammonium Hydroxide (NH4OH). Add 1.25 gm
magnesium salt of EDTA and dilute to 250 ml with distilled water.
Procedure:
1. Take a well-mixed suitable volume of sample (25, 50, or 100 mL) in a
conical flask (V). Select a sample volume that requires less than 15
 mL EDTA titrant and complete titration within 5 minutes, measured
from the time of buffer addition.
2. Add 1-2 ml of Ammonia buffer solution. Usually, 1-2 mL buffer
solution is sufficient to give a pH of 10.0 to 10.1 and mix well.
3. Add a pinch of Eriochrome black T and titrate with standard EDTA
(0.01 M) till wine red color changes to blue color. Note down the
Volume of EDTA required.
4. Run a reagent blank with distilled water. Note the volume of EDTA
consumed
5. Calculate the volume of EDTA required by sample; C = (A-B)

Observation:
1. Titrant
2. Indicators: Eriochrome Black T Indicator
3. End Point: Wine Red to Blue
4b. Determination of Chloride of water sample.
Aim: To determine the chloride content of the given water sample by Mohr's
method
Theory: Chloride in the form of Chlorine ion is one of the major inorganic
anions. The salty taste produced by Chloride concentration is variable and
dependent on the chemical composition of water. The Chloride is higher in
wastewater than in raw water. Along the sea coastal, Chloride may be
present in high concentrations because of saltwater intrusion into the water
and sewage system. In this method, a slightly alkaline solution is used.
Potassium chromate can indicate the endpoint of Silver nitrate titration of
Chloride as quantitatively precipitated before red Silver chromate is formed.
As the silver nitrate solution is slowly added, a precipitate of silver chloride
forms as per the following reaction:
Ag+(aq) + Cl–(aq) → AgCl(s)
The endpoint of the titration occurs when all the chloride ions are
precipitated. Then additional silver ions react with the indicator's chromate
ions, potassium chromate, to form a red-brown precipitate of silver
chromate as per the following reaction.
2 Ag+(aq) + CrO 4 2– (aq) → Ag2 CrO4(s)

Environmental Significance:
 Chlorides associated with sodium (Sodium Chloride) exert salty taste
when its concentration is more than 250 mg/L. These impact a salty
taste to water. Chlorides are generally limited to 250 mg/L in water
supplies intended for public water supply.
 In many arrears of the world where water supplies are scarce, sources
containing as much as 2000 mg/L are used for domestic purposes
without adverse effects once the human system becomes adapted to
the water.
 It can also corrode concrete. Magnesium chloride in water generates
hydrochloric acid after heating, which is highly corrosive and creates
boilers problem.
  Chloride determinations in natural waters are useful in the selection
of water supplies for human use.
 Chloride determination is used to determine the type of desalting
apparatus to be used.
 Chloride determination is used to control pumping of ground water
from locations where seawater intrusion is a problem.

Apparatus: Titration Stand with Burette, Conical Flask, Beaker, Measuring

Cylinder, Pipette, Funnel, Wash Bottle, etc. Reagents:
 Standard Silver nitrate titrant (0.0141 N): Dissolve 2.395 gm of silver
nitrate in distilled water and dilute to 1000 ml. Standardize against
0.0141 N sodium chloride solution.
 Standard sodium chloride solution (0.0141 N): Dissolve 824 mg of
sodium chloride (Dried) in distilled water and dilute to 1 litre. 1 ml = 500
μg of chloride.
 Potassium chromate indicator solution: Dissolve 50 gm of potassium
chromate in a little distilled water. Add a few drops of silver nitrate
solution until a definite red precipitate is formed. Let it stand for 12-
hour, filter and dilute to 1 litre with distilled water.

Procedure:
1. Take a well-mixed suitable volume of sample (25, 50, or 100 mL) in a
conical flask (V).
2. Add 1ml of potassium Chromate indicator. The color of the solution turns
to yellow color.
3. Titrate against Standard silver Nitrate solution till color change from
yellow to brick red.
4. Note the Burette volume of silver Nitrate added (A)
5. For better accuracy, titrate distilled water (blank) in the same manner.
Note the burette volume of silver Nitrate added for distilled water (B).
6. Calculate the volume of EDTA required by sample; C = (A-B)
 Observation:
1. Titrant
2. Indicators: Potassium Chromate Solution
3. End Point: Yellow to Brick Red

(Where N is the normality of the solution

35.45 is the equivalent weight of Chloride Ion
V is the volume of the sample)
Experiment 5: Determination of optimum coagulant dose
using jar test.
Aim: To determine the amount of optimum coagulant dose
using the jar test.

Introduction:
Chemical coagulation is a treatment method widely used for the removal of
small-sized and colloidal impurities from water. Surface water generally
contains a wide variety of colloidal impurities that may cause the water to
appear turbid and may impart color to the water. Colloidal particles that
cause color and Turbidity are difficult to separate from water because they
will not settle by gravity and are so small that they pass through the most
common filtration media pores. To be removed, the individual colloids must
aggregate and grow in size to settle by gravity. Chemical agents are used to
promoting colloid aggregation by destroying the forces that stabilize colloidal
particles.
The process of destroying the stabilizing forces and causing aggregation of
colloids is referred to as chemical coagulation. Coagulation involves reducing
electrical forces of repulsion and promoting "chemical type" interaction
between colloids, which eventually results in settling of the colloids and
accomplishes removal of Turbidity and color. At higher coagulant doses,
"charge reversal" is possible, resulting in resuspension of the colloids. Hence
optimum coagulant doses are determined through laboratory model tests
where the water to be treated subjected to a range of coagulant doses, and
the removal efficiencies are observed. Many authors used the term
"coagulation" to describe the process by which the charge on particles is
destroyed, and the term "flocculation" to describe the aggregation of
particles into larger units. The chemical used for this purpose is called
coagulants. The most common coagulants used in water and wastewater
treatment are aluminium and ferric salts such as Alum, Ferric Chloride, and
Ferric Sulfate. The common metal salt Alum (Aluminium Sulphate) is a good
coagulant for water containing appreciable organic matter.
Theoretically, each mg/L of alum consumes approximately 0.50 mg/L (as
CaCO3) of Alkalinity for water with low Alkalinity. This may result in a
significant reduction in pH that may interfere with aluminum hydroxide
flocs' formation. If the Alkalinity is insufficient, coagulant aids such as lime
[Ca (OH)2], soda ash (Na2 CO3 ), activated Silica, and polyelectrolytes are
used to provide the necessary Alkalinity. Iron coagulants can be operated
over a wider pH range and generally effective in removing Turbidity and
watercolor. However, they are usually more costly.
𝐴𝑙 (𝑆𝑂 ) . 18𝐻 𝑂 + 3𝐶𝑎(𝐻𝐶𝑂) → 3CaS𝑂 + 2Al (OH) + 6C𝑂

Environmental Significance:
Besides efficient removal of Turbidity and color, coagulation with alum and
ferric Chloride or ferric sulfate is also widely used for the removal of heavy
metal ions (e.g., lead, arsenic) from water. In this process, heavy metal ions
are primarily removed by adsorption (and Subsequent precipitation) onto
coagulated flocs of metal (either aluminum or iron) hydroxides. Coagulation
with alum and ferric chloride/sulfate is successfully used for the removal of
arsenic from water

Theory on the Experiment:

Treatment of water by coagulation involves -
(1) Determination of optimum dose of coagulant by jar test.
(2) Determination of power input for the flocculator.
The test to determine optimum coagulant dose will be carried out in the
glass jar. It is important to determine the optimum dose to avoid charge
reversal and resuspension colloids. Optimum coagulant dose is considered
as the amount of coagulant, which produces water with the lowest Turbidity.
Materials required:
Reagent:
Standard Alum solution.
Apparatus:
- Coagulation (stirring) device
- pH meter
- Turbidity meter
- Glass beakers (1000 mL)
 -
Procedure:
1. Determine the pH and Turbidity of the water to be treated.
2. Fill six 1000 mL beakers each with 500 mL water to be treated,
3. Add required (as instructed by teacher) coagulant (standard alum
solution) to each beaker.
4. Mix the samples in the beaker with the help of the stirring device.
Subject the samples to one minute of rapid mixing followed by 15
minutes of slow mixing (about 40 rpm).
5. Allow the flocs to settle down for about 15 minutes. Observe the
characteristics of the flocs and the settling rates.
6. Collect the supernatant from each beaker and measure the pH and
Turbidity of each.
7. Plot pH versus alum dose in a graph paper and observe the effect of
alum dose on pH.
8. Plot turbidity (NTU) versus the coagulant (alum) dose (mg/L) in a
graph paper. Determine the optimum dose of alum from this plot.

OBSERVATION PH(initial) Initial Alum PH(final) Final

NO Turbidity Dose(mg/l) Turbidity
Experiment 6: Determination of optimum lime soda dose for
hardness removal
Aim: The amount of lime and soda required to soften a hard
water sample.
THEORY
The hardness of water is defined as the soap settling property of that water.
The soap is sedimented by the presence of Ca+2 and Mg+2 ions in the water.
Ions such as Fe+ 2, Zn+2, and Al+3 also help to settle. However, high amounts
of Ca+ 2 and Mg+ 2 ions in water usually lead to water hardness. This is the
most common type of hardness in natural waters. The hardness caused by
these materials is known as total hardness. The part of the total the
hardness, corresponding to carbonate and bicarbonate ions in the water, is
defined as carbonate hardness. These ions also determine water alkalinity.
Waters are classified according to hardness grades as follows.
(mg/L) CaCO3 Degree of
Hardness
0-75 Soft
75-150 Middle
150-300 Hard
300 and over Very hard

The Aim of Softening:

Hard water can cause various problems. The problems created by hard
waters are as follows;
 They cause excessive soap consumption.
 They cause skin irritation.
 They cause lime accumulation in boilers, hot water pipes,
and heaters.
 They cause discoloration in porcelain. Especially in homes,
the white color of the sinks and bathtubs are discolored.
 They reduce the life of fabrics and cause them to wear out.
 They cause problems in the canned food industry.
Hardness removal (chemical softening) is a process that removes all or part of
the hardness by adding various chemical substances into the water. The
processes used for water softening are chemical sedimentation and ion
exchange methods. Chemical sedimentation can be carried out in 3 ways.
1-Lime-soda process.
2-Caustic-soda process
3-Sodium phosphate process
Lime soda process: In the lime-soda process, hard water is treated with
lime (CaO or Ca (OH)2) firstly, after that with soda. In this process, the
hardness is removed by sedimentation as calcium carbonate or magnesium
hydroxide. Lime is added either as calcium hydroxide or calcium oxide, and
soda is added as sodium carbonate. The substances form hardness in water,
and the reactions of lime and soda can be written as follows.

Ca(OH)2 + CO2 CaCO3 + H20

Ca(OH)2 + Ca(HCO3)2 2CaCO3 + 2 H20

Mg(HCO3)2 + Ca(OH)2 MgCO3 + CaCO3 + 2 H20

MgCO3 + Ca(OH)2 Mg(OH)2 + CaCO3

MgCl2 + Ca(OH)2 CaCl2 + Mg(OH)2

MgSO4 + Ca(OH)2 Mg(OH)2 + CaSO4

2NaHCO3 + Ca(OH)2 CaCO3 + Na2CO3 +2H20

CaCl2+ Na2CO3 CaCO3 + NaCl

CaSO4 + Na2CO3 CaCO3 + Na2CO3

The usual method for lime soda processing involves treatment with excessive
lime. The pH should be greater than 9 for sedimentation of the magnesium
hydroxide. Usually, pH is between 10-10.5. A small amount of alum or sodium
aluminate is added to ensure good sedimentation. If the water contains
excessive Alkalinity after the softening process is completed, there is a
possibility of calcium carbonate precipitation in the pipes. The softened water
is treated with H2SO4 or CO2 to remove the Calcium Carbonate from the
softened water. This reaction is called Recarbonization.
If it is requested to retain permanent hardness in water, soda should not be
used after lime dosing. This application is defined as a partial softening
operation.
MATERIALS USED
- Ca(OH)2 and Na2CO3
- NH4Cl
- Eriochrome Black T and EDTA
- Phenolphthalein and Methyl Orange
- H2SO4
- Beaker
- Jar test setup
PROCEDURE
1. Determine the pH of the raw water sample.
2. Place 1 liter of raw water in each of the three beakers of the laboratory
stirrer. Immerse blades and stir the raw water samples at about 100
rpm.
3. Add lime-soda solutions into each of the beaker to obtain the desired
concentrations in the raw water samples.
4. Let the samples mix at approx. 100 rpm for 1minute, then decrease the
speed to approx. 30 rpm. Allow the sample to mix for 10 minutes.
Observe any changes in the suspended matter in the sample.
5. At the end of the mixing period, turn off the stirrer, let the flocs settle (at
least 20 minutes). Determine the pH of each treated water sample.
6. Measure the hardness of the samples and find the minimum lime dose to
remove hardness.
RESULTS, CALCULATIONS, and DISCUSSION
-
 The amount of lime and soda required to soften hard water is calculated.
 Graphically associate the lime scale with total hardness and Alkalinity.

Dose of Lime-Soda Visual observation of

Beaker No: Solution Precipitates (Bad,
Fair, Good, Excellent
etc.)

Alternately hardness of the water beakers can be determined by the EDTA

titration method and Optimum coagulant dose for maximum hardness removal
can be determined.

Optimum Dose of Lime-Soda solution = _______________ mg/l