EXPERIMENTAL METHODS IN ENVIRONMENTAL ENGINEERING

LAB MANUAL

Submitted by: Osama Saeed

Submitted to: Dr.Irfan Jalees
Date of Submission: 11 November 2022
Reg No: 2022-MSC-EVEN-206

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 EXPERIMENT NO 1:
DETERMINATION OF PH IN DIFFERENT WATER
SAMPLES

1.1: APPARATUS:
 Samples
 Ph Meter
 Beakers
 Buffer Solution(4,7,10)

1.2: RELATED THEORY:

1.2.1: WHAT IS PH?
 Ph is a unit of measure which describes the degree of acidity or alkalinity of a
solution.
 It is measured on a scale of 0 to 14.
 The term pH is derived from “p”, mathematical symbol of negetive logarithm, and
“H”, the chemical symbol for Hydrogen.

1.2.2: PH Scale:
The Ph scale as shown below, ranges from 0 to 14, with Ph
 7.0 being neutral
 Water with a low Ph is said to be acidic(0-6)
 Water with a high Ph is said to be basic(8-14)
Pure water would have a Ph of 7.0, but water sources and precipitation tend to be slightly
acidic, due to contaminants in water.

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 FIGURE-1: PH Scale

1.2.3: HOW DOES THE PH OF A WATER SOURCE CHANGE?

 Surface water typically has a PH value between 6-8.5 and groundwater tends to have
a ph of 6-8.
 The ph of a water source can vary naturally. Some types of rock and soil, such as
limestone, can neutralize acid more efficiently than other types of rock, such as
granite.
 When the carbon dioxide mixes with the water, a weak carbonic acid is formed; this
can cause the ph of a water body to decrease.
 When sulphur dioxide and nitrogen oxides are emitted, through industrial operations
and vehicles, acid rain can be produced. (TDS and pH — Safe Drinking Water Foundation,)

1.2.4: MEASUREMENT OF PH:

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We measure PH using indicator dyes,PH strips and PH meter.

FIGURE 2: PH Meter

1.3: PROCEDURE:
The procedure of the experiment consists of three parts:
 Calibration of PH Meter.
 Determination of PH of the sample.
1.3.1: CALIBRATION OF PH METER:
First of all, for the calibration of the instrument take different buffer solutions. The process of
calibration is as follows:
 Start by setting the temperature at room temperature, usually about 25C, by pressing
the C key and adjusting the temperature knob.
 Dip the electrode in the buffer solution of known PH(PH 4.0 buffer).
 Switch on the power supply and take the reading. Standardize the instrument using
calibration knob.
 After cleaning, again dip the electrodes in the buffer solution of PH 7.0. Note the
reading. If it is 7, then the instrument is calibrated. If not, correct the value and is
manupulated so that the reading becomes 7.0.
 The reading on the dial indicates the PH of the solution.
1.3.2: DETERMINATION OF THE PH OF THE SAMPLE:
 A water sample whose PH is to be found is taken in the beaker and the temperature
knob is adjusted such that the temperature of the solution is same as that of dial.

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  The electrode is washed with distilled water and reused with the sample and then it is
dipped in the sample. Measure the PH of the sample and note its results.

1.4: ENVIRONMENTAL SIGNIFICANCE:

 Most living things can survive wihin the a narrow PH range. If their PH of the body or
their environment fluctuates too much the organism can die.
 The growth of micro-organisims depend upon PH.
 For example, blood is normally slightly basic, with a P range of 7.35-7.45. If our
body’s PH deviates slightly from this range, we will start tpo feel sick. If our blood
falls below 6.8 or above 7.8, our body cells will stop functioning and death will occur.
If PH goes below 7.35, you have a condition called acidosis. Acidosis is caused by
overabundance of acid in the blood or built up of carbon dioxide in the blood. Carbon
dioxide can built up in the blood when lung function is poor or breathing is slow.
When the PH goes above 7.45, you have a condition called alkalosis.
 The PH of a stomach fluid, which contains hydrochoric acid, is between 1.0 and 3.5,
with a mean of approximately 2.0, and there is a range of commonly encountered
foods that are also of low PH.

1.5: RESULTS/CALCULATIONS:
SAMPLE NAME PH OF SAMPLE TEMPERATURE OC

Sample 1 2.33 20-25

Sample 2 8.75 20-25

Sample 3 11.99 20-25

Distilled Water Sample 4 8.93 20-25

Tap Water 7.74 20-25

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1.6: COMMENTS:
 In this experiment, we performed PH test on different water samples to ensure the
quality of water.
 Excess water is also called hard water.

 Excess of alkalinity in the body may cause nausea vomiting, hand tremors muscle
twisting, tinglingin the extremities of face confusion and potentiometric technique is
used in this experiment.

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 EXPERIMENT NO 2
DETERMINATION OF TURBIDITY IN DIFFERENT WATER
SAMPLES

2.1: PRINCIPLE OF TURBIDITY:

Turbidity is based on the intensity of light scattered by the sample under defined conditions.
The higher the intensity of scattered light, the more will be turbidity.

FIGURE 3: PRINCIPLE OF TURBIDITY

2.2: APPARATUS:
 Turbidity Meter
 Sample cells
 Tissue papers

2.3: RELATED THEORY:

2.3.1: TURBIDITY:
“Turbidity is the cloudiness or haziness of a fluid caused by a large number of individual
particles that are generally invisible to naked eye, similar to smoke in air”.
The measurement of turbidity is a key test of water quality.

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Turbidity can be caused by:
 Silt,sand and mud
 Bacteria and other gems
 Chemical precipitates
2.3.2: SOURCES
Multiple insoluble particles can produce turbidity.

2.3.3: SUSPENDED PARTICLES

Such particles which don’t settle at the bottom and their specific density is comparable with
that of water.

2.3.4: SETTLEABLE PARTICLES

These are particles which have specific gravity more than that of water e.g.. sand and clay.

2.3.5: COLLOIDAL PARTICLES

These are suspended particles having diameter from micrometer to nanometer(<10m).

2.3.6: WHO GUIDELINES FOR DRINKING WATER:

For drinking water supplies, the following guidelines should be taken into consideration:
 Drinking water should have a turbidity of 5 NTU or less. Turbidity of more than 5
NTU would be noticed by users and may cause rejection of the supply.
 Where water is chlorinated, turbidity should be less than 5 NTU and preferably less
than 1 NTU for chlorination to be effective.(Government of Pakistan
Environmental Protection Agency(Ministry of Environment) National Standards
for Drinking Water Quality(NSDWG),2008).

2.3.7: MEASURING TURBIDITY:

 Turbidity can be measured using an electronic turbidity meter.
 Turbidity is usually measured in nephlometric turbidity units(NTU).

2.4: PROCEDURE:
 Take water sample and shake it well.
 Then quickly transfer it to turbidity cell.

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  Volume of sample must be above the arrow mark.
 Then transfer turbidity cell into turbidity meter in 10-15 meter.
 Repeat the same procedure for every water sample.

2.5: RESULTS AND CALCULATIONS:

SAMPLE SOURCE TURBIDITY (NTU)

Sample 1 1.10
Sample 2 5.22
Tap Water 3.66

TABLE 2: CALCULATION OF TURBIDITY

2.6: COMMENTS:
 In this experiment, we performed the test on different samples in order to check the
turbidity value.
 Turbidity of water range(0-1) NTU is ideal for drinking purpose but according to
WHO guidelines, drinking water should have 5 NTU or less.
 Turbidity value increases when light rays scattered back because of dirt particles.
 Higher the turbidity of water the aesthetic look of water is poor.

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 EXPERIMENT NO 3
DETERMINATION OF THE AMOUNT OF CHLORIDES IN
DIFFERENT WATER SAMPLES

3.1 APPARATUS:
 Burette with burette stands and porcelain title
 Pipette with elongated tips
 Conical Flask
 Standard Flask
 Wash Bottle
 Beakers

FIGURE 4: APPARATUS

3.2 CHEMICALS REQUIRED:

 Powder of Chlorine
 Chlorine Reagent

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3.3 RELATED THEORY:
3.3.1 INTRODUCTION
 Chloride is a naturally occuring element that is common in most natural waters and is
most often found as a component of salt(sodium chloride) or in some cases in
combination with potassium or calcium.
 Upland and mountain water supplies are low in chloride concentration whereas river
and groundwater sources have a relatively high concentration.
 Ground water has a high salt content due to the reason that the solvent power of water
disssolves chlorides from top soils and deeper foundations.
 Chlorides are leached from various rocks into soil and water by weathering.
 Chloride ion is highly mobile and is transported to close basins or oceans, chloride in
surface and groundwater from both natural and anthropogenic sources such as Run-
off containing road de-icing salts, the use of inorganic fertilizers, land fill leachates,
septic tank effluents, animal feeds, industrial effluents, irrigation drainage and sea
water intrusion in coastal areas.
 Chlorides in water may be considerably increased by treatment processes in which
chlorine is used.(Chloride in Drinking Water¬ Government in Prince
Edward,2015)

3.3.2 WHO GUIDELINES VALUE:

 EPA considers it as a secondary contaminant with MCL=250 mg/l.
 If value exceeds the limit, then wate rwill have salty taste.

3.4 ENVIRONMENTAL SIGNIFICANCE:

 Chloride occur naturally in foodstuffs at levels normally less than 0.35 mg/l.
 In metal pipes, chlorides reacts with metal ions to form soluble salts, thus increasing
levels of metals in drinking water.
 Chloride increase the electrical conductivity of water and thus increase its corrosive
nature.
 Chloride concentration in acces of 250 mg/l can give rise to detectable taste in water.
 Healthy individuals can tolerate the intake the large quantities of chloride.

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  The most common toxicity is from chloride in the irrigation water. Chloride is not
absorbed and held back by soils, therefore it moves readily with the soil water, is
taken up by the crop, moves in the transpiration stream, and accumulates in the
leaves.
 Normally, plant injury occurs first at leaf tips(which is common for chlorides
toxicity), and progress from the tip back along the edges as severity increases.
 Excessive necrosis(dead tissue) occurs which is often accompanied by early leaf drop
or defoliation.

3.5 PROCEDURE:
1. Add 10 ml of the sample into a test tube with pipette.
2. Add 1 spoon of powder chlorine into water sample.
3. Add 2 drops of chlorine reagent.
4. Leave the test tube in stand for 1 min to complete reaction.
5. Fill the sample into the cell.
6. Measure in the photometer.

3.6 OBSERVATIONS AND CALCULATIONS:

3.6.1 FOR TOTAL CHLORIDE:
10 ml water + 2 drops of Cl^-2 +1 spoon powder chlorine

Readings of 3 samples(Group 1):

Sample 1= 2 ml
Sample 2= 3 ml
Sample 3= 3 ml
Average Reading= 2.67 ml
( 2.67∗N ( 0 . 141 )∗Eq . Wt ( 35.5 )∗1000 )
Chlorides(Cl-) = = 534.58 mg/l
( Volume of sample ∈mL )

Readings of three samples(Group 2):

Sample 1=1 ml
Sample 2=1 ml
Sample 3=0.8 ml

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Average Reading=0.933 ml
Cl-=0.933x0.141x35.5x1000/25= 186.8 mg/l

3.7 RESULTS:
In our water sample total chloride concentration is
 Photometric technique is used.
 Chloride concentration is not as much effects on human health.
 It is also secondary contaminate according to WHO.

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 EXPERIMENT NO 4
DETERMINATION OF HARDNESS IN WATER BY EDTA
TITRATION METHOD

4.1 APPARATUS:
 Burette
 Pipette
 Erlenmeyer Flask
 Measuring Cylinder

FIGURE 5: APPARATUS

4.2 REAGENTS:
 Standard EDTA titrant(0.01 M)
 Eriochrome black T indicator(EBT)
 Ammonia Buffer solution
 Erichrome Blue black R indicator(EBBR)
 Sodium Hydroxide

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4.3 RELATED THEORY:
WATER HARDNESS:
Hard water is water that has a high mineral content (in contrast with “soft water”). Hard
water is formed when water percolates through deposits of limestone, chalk or gypsum which
are largely made up of calcium and magnesium carbonates, bicarbonates and sulfates.

FIGURE 6: SOFT AND HARD WATER

4.3.1 UNITS OF HARDNESS:

Hardness is most commonly expressed as milligrams of calcium carbonate per liter. (mg/L as
CaCO3).
It is expressed in terms of calcium carbonate equivalent because its molecular weight 1s 100,
and also, its equivalent weight is 50, moreover it is the most insoluble salt that can be
precipitated in water treatment.

4.3.2 TYPES OF HARDNESS:

 Temporary Hardness
 Permanent Hardness

Temporary Hardness:

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The presence of magnesium and calcium carbonates in water makes it temporarily hard.
(Hardness of water-Types, Remove Temporary and permanent Hardness).

Removal of Temporary Hardness:

 Hardness in water can be removed by boiling the water.
 When we boil the soluble salts of Mg(HCO3)2 is converted into to Mg(OH)2 which is
insoluble and hence gets precipitated and is removed. After filtration, the water we get
is soft water.

4.3.3 Permanent Hardness:

When the soluble salts of magnesium and calcium are present in the form of chloride and
sulphides in water, we call it permanent hardness because this hardness can’t be removed by
boiling.

Removal of Permanent Hardness:

We can remove this hardness by treating water with washing soda. Insoluble carbonates are
formed when washing soda reacts with sulphide and chloride salts of magnesium and calcium
and thus, hard water is converted into soft water.

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 FIGURE 7: DIFFERENCE BETWEEN HARD WATER AND SOFT WATER

4.4 STANDARDS FOR HARDNESS:

 Total Hardness as CaCO3 = < 500 mg/L
 Recommendations have been made for the maximum and minimum levels of
calcium(40-80 ppm) and magnesium(20-30 ppm) in drinking water, and a total
hardness expressed as the sum of the calcium and magnesium concentrations of 2-4
mmol/l.

CONCENTRATION AS CACO3 INDICATION

0 to 60 mg/L Soft water
60 to 120 mg/L Moderately hard water
120 to 180 mg/L Hard water
>180 mg/L Very hard water
Table 3 : WATER HARDNESS SCALE

4.5 ENVIRONMENTAL SIGNIFICANCE:

4.5.1 Corrosive Nature:
A problem with very soft water is that because of its purity, the copper pipes used in the
house will start to dissolve in the water, the green mark on the porcelain under the dipping tap
is an accumulation of copper from the pipes.
4.5.2: Reduce Effectiveness of Soap:
Calcium and magnesium ions in the water join with the soap to form insoluble curd and
reduce the effectivenesss of soap using washing soda.
4.5.3: For Aquatic Animals:
Calcium and magnesium are essential in the biological processes of aquatic animals, for
example, bone, scale formation in fish and hardening of the newly formed shell. For most
pond fish, i.e, goldfish moderate to hard water is best. The optimum hardness range for most
pond fish would be between 100-300 mg/liter.
4.5.4: For Humans:
Calcium is essential for maintaining precise levels for normal heart, muscle fever and nerve
function. Many water softeners work by replacing hardness with sodium. Too much
sodium(salt) can be a problem for babies and infants as their kidneys are not as efficient at

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filtering it out of the blood. Too much sodium can also be a problem for those on a low
sodium diet.
4.5.5: Signs of Hardness in Home:
Hard water can be a detected in many ways. You may notice an accumulation of white/chalky
deposits on items such as plumbing, tubs, sinks, pots and pans. Other things you may notice:
 Increased difficulty in laundering and cleaning tasks,
 Decreased efficiency of water heaters,
 White spots on glassware,
 White spots on your car after washing,
 Soap scum such as bathtubs, shower tiles and basins
 Accumulation of hard, cream-colored deposits around fixtures and inside pipes.

4.6: PROCEDURE:
4.6.1: Calcium Hardness:
 Take 25 ml sample and add 25 ml of distilled water was added in an Erlenmeyer
Flask.
 Then add 2 ml of NH3 buffer solution in the flask.
 Now add a pinch of EBT indicator into the solution. The solution will turn pink in
colour.
 The solution was titrated against standard 0.02 N EDTA slowly till the colour changes
to deep violet.
 The volume of EDTA added was noted and labelled as “A” ml.
 The volume of EDTA used was noted and labelled as “B” ml.
A-B= C
( A−B ( mL )∗N ( 0 . 01 )∗Eq .Wt ( 100 )∗1000 )
 Total hardness (mg/L as CaCO3) =
( Volume of sample ∈mL )
4.6.2: Magnesium Hardness:
 Take 25 ml water sample and add 25 ml of distilled water in the Erlenmeyer flask.
 Then add 2 ml of NaOH solution in it.
 Add a pinch of MUREXIDE indicator in it. The color will change to magenta.
 Then it was titrated standard 0.02N EDTA slowly until the color changes to deep
violet.
 The volume of EDTA added was noted and labelled as “A” ml.

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  The volume of EDTA left was noted and labelled as “B” ml.

4.7: OBSERVATIONS AND CALCULATIONS:

Volume of the Sample 1 (Group 1):
Reading 1= 22.2 ml
Raeding 2= 24.1 ml
Reading 3= 26.6 ml
Average Reading= 24.3 ml
Total Hardness= 24.3x0.01x100x1000/25= 972 mg/l CaCO3

Volume of the sample 2(Group 2):

Reading 1= 8.5 ml
Reading 2= 10.2 ml
Reading 3= 10.7 ml
Average= 9.83 ml
Total Hardness= 393.2 mg/l CaCO3

4.8: COMMENTS:
In this experiment, we find the quantity
 Calcium Hardness
 Magnesium Hardness
 Total hardness.
 Volumetric technique is used in this experiment.

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 EXPERIMENT 5
DETERMINATION OF ALKALINITY IN DIFFERENT
WATER SAMPLES

5.1: APPARATUS:
 Burette
 Pipette
 Titration flask
 Burette Stand

FIGURE 8: APPARATUS

5.2: REAGENTS:
 Phenolphthlein
 Methyl Orange
 H2SO4
 Ethanol

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5.3: RELATED THEORY:
5.3.1: INTRODUCTION:
 Alkalinity is a measure of the water’s ability to neutralize acid.
 Buffering capacity of a water body.
 Presence of bicarbonates, carbonates and hydroxides.
 Alkalinity is not a chemical in water, but, rather it is a property of water that is
dependent on the presence of certain chemicals in the water.
 Maintaining a fairly stable Ph level.
 Alinity is the water’s capacity to resist changes in Ph that would make the water more
acidic.(Plymouth Technology,2005).

5.3.2: UNITS OF ALKALINITY:

 Alkalinity is expressed in units of milligrams per litre mg/l of CaCO3.
 Ppm of CaCO3.

Base VS Alkalinity:

Base Alkali

Bases do not dissolve in water Bases that dissolve in water are alkali

All bases are not alkali All alkali are bases

5.3.3: SOURCES:
 The main sources of natural alkalinity are rocks which contain carbonate, bicarbonate
and hydroxide compounds.
 One source of alkalinity is calcium carbonate(CaCO3), which is dissolved in water
flowing through geology that has limestone or marble.
 Limestone is rich in carbonates, so waters flowing through limestone regions or
bedrock containing carbonates generally have high alkalinity- hence good buffering
capacity. Conversely, areas rich in granites and some conglomerates and sandstones
may have low alkalinity and, therefore, poor buffering capacity.

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  The effluent from Wastewater Treatment Plants(WWPs) can add alkalinity to a
stream.

5.4: ENVIRONMENTAL SIGNIFICANCE:

5.4.1: Benefits:
 Ultra hydrating properties.
 Boosts immunity to neutralize acid.
 Ca. in alkaline water improves health.
 Alkalinity is especially important in areas where acid rain is a problem.
 Alkalinity is important to aquatic organisms because it protects them against rapid
changes in Ph.
5.4.2: Health impacts:
 Alkalosis
 Effect body’s Ph.
 Skin irritations
 Gastrointestinal issues

5.5: PROCEDURE:
1: Preparation of Buffers:
 Methyl Orange Buffer:
Take 100 ml distilled water.
Add 0.05g methyl orange and shake it.

 Phenolphthlein Buffer:
Take 50 ml distilled water.
Add 50 ml ethanol in it.
Then add 0,05g Phenolphthlein

2-3 drops of phenolphthalein indicator

Pink colour Appears (pH>8.3) Pink colour do not appears

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 OH- are present OH- are not present

Phenolphthalein alkalinity exists Phenolphthalein alkalinity do not exists

TABLE 4: DROPS OF PHENOLPHTHLEIN INDICATOR

Then titrate this solution against 0,02N sulphuric acid, till the solution becomes colorless,
Note the volume of H2SO4.

2. Methyl Orange Alkalinity(Total Alkalinity):

Then in the same flask add 2-3 ml of methyl orange indicator in it. Colour will become
yellow. Then titrate the solution against 0.02N H2SO4 until the solution becomes reddish
orange/pink.
Note the volume of H2SO4. Take atleast 3 readings.
Ions contributing for alkalinity:
OH- + H+ H20 P
CO3-2 + H+ HCO3- M
HCO3- + H+  CO2 + H2O

Carbonate Alkalinity P is not 0 but < T

Hydroxide Alkalinity P>½T

Bi Carbonate Alkalinity P<½T

3. Formula used in calculation:

Phenolphthlein Alkalinity= P= “A”x N x Eq.wt x 1000/Volume of the sample
Total Alkalinity= T= “B”x N x Eq.wt x 1000/Volume of the sample

5.6: OBSERVATIONS AND CALCULATIONS:

Sample 1(Group 1):
Reading 1: PA= 1.5-0= 1.5 ml Total= 10.9 ml
Reading 2: MOA= 10.9-1.5= 9.4 ml

Reading 3: PA= 1-0= 1 ml

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Reading 4: MOA= 8 ml Total= 9 ml

Reading 5: PA= 9.9-9= 0.9 ml Total= 8.1 ml

Reading 6: MOA= 18-9.9= 8.1 ml

PA= 1.5+1+0.9/3 = 1.13 ml

MOA= 9.4+8+8.1/3= 8.5 ml

PA=1.13 x 0.02 x 50 x 1000/25 = 45.2

MOA= 8.5 x 0.02 x50 x 1000/25 = 340
Total Alkalinity= 45.2+340= 385.2 mg/l

Sample 2: Tap water(Group 2):

Reading 1= 5.3 ml
Reading 2= 5.7 ml
Reading 3= 5.5 ml
Average= 5.5 ml
PA=0
MOA= 5.5 x 0.02 x 50 x1000/25= 220 mg/l
Phenolphthlein alkalinity is zero due to the faulty Titration apparatus.
Total Alkalinity= P+MO= 0+220= 220 mg/l

Sample 3(Group 3): PA=0

Initial Reading= 18.2 ml
Final Reading= 23.3 ml Difference= 23.3-18.2= 5.1 ml (B`)

B`
Initial Reading= 23.3 ml
Final Reading= 29.2 ml Difference= 29.2-23.3= 5.9 ml

B`
Initial Reading= 29.2 ml

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Final Reading= 34.5 ml Difference= 34.5-29.2= 5.3 ml

B` Avg= 5.1+5.9+5.3/3= 5.43

=B` x N x 50 x 1000/25= 5.43 x 0.02 x 50 x 1000/25= 217.2 mg/l

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