Environmental Engineering-I Lab Manual

Table of contents:

Experiment #01 Introduction to Environment Engineering-I Laboratory………………………..2

Experiment #02 Determination of pH of water...........................................................................4

Experiment #03 Determine the turbidity of the given solution....................................................8

Experiment # 04 To determine the Total Hardness, of different water samples 1

Experiment # 05 Determination of chloride concentration in different water samples............... 24

Experiment #06 Determination of the amount of sulfates in water ........................................... 26

Experiment # 07 Determination of Total Suspended Solids, Total Fixed Solids and Total

Volatile Solids .......................................................................................................................... 29

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Experiment #01

Introduction to Environment Engineering-I Laboratory

Introduction

Environmental Engineering

Is the application of science and engineering principles to improve the natural environment (air,
water, and/or land resources), to provide healthy water, air, and land for human habitation (house
or home) and for other organisms, and to remediate polluted sites.
Environmental Engineering-I

It particularly involves the principles of environmental engineering and inculcates abilities for
design and implementation of water supply schemes.

Environment Engineering-I Laboratory

Environmental Engineering-I Laboratory involves different tests and analysis to evaluate

suitability of tap water for drinking purpose. Water Quality test on mineral water (Gourmet,
Aquafina, etc.) are also performed to find out different parameters are within their prescribed
range or not.

The following are the different equipment’s and instruments used in the Environmental
Engineering-I Laboratory:

1. pH meter
2. Nephelometric Turbidity Unit
3. Automatic/ Conventional burette
4. Titration glassware
5. Spectrophotometer
6. Magnetic stirrer.
7. Dessicator
8. Drying oven
9. Analytical balance

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10. Filtration apparatus

11. Fiber filter disks
12. Muffle furnace
13. Petri dishes.
14. Conductivity Meter

Assignment # 01:
Enlist the different Instruments and Equipment’s used in the Environmental Engineering-I Lab
and explains their purposes and importance in the analysis and testing of drinking water.

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Experiment # 02

Determination of pH of water

Related Theory

Scope

1. This test method is the procedure for determining the pH of drinking water, waste water and
natural water by use of pH water.
2. Practically, every phase of water supply and waste water treatment e.g. acid base
neutralization, water softening, precipitation, coagulation, disinfection and corrosion control
is pH dependent.
3. It is used in alkalinity and carbon dioxide measurement and much other acid base
equilibrium.

pH

pH is a term use to express the intensity of an acid or alkaline condition of a solution. It is a way
of expressing the hydrogen ion concentration, or more precisely, the Hydrogen ion activity. It is
important in almost every phase of environmental Engineering practice.

The pH meter:

Every pH meter must be calibrated before use; a good instrument should have at least 2 controls
on its panel.

a. Zero Calibration:

The first one is to zero the instrument i.e. to off-set the asymmetry potential. It is usually named
“Calibration” for the calibration procedure, a buffer solution of pH7 and pH4 is to be used.

b. Temperature Compensation:

It adjusts the temperature dependence of the slope according to the sample temperature.

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Environmental Significance

 Water Supply

In the field of water supply pH is a factor that must be considered in coagulation, disinfection,
water softening and corrosion control.
When water has a low pH, it is often referred to as "soft water." Soft water is more acidic,
therefore, it can be corrosive and harmful to any metals it comes into contact with. When the
water corrodes the metal, this corrosion can then seep into the water. Another problem with soft
water; it can cause stains in any clothing that is washed in it.
When water has high levels of pH, it is considered to be "hard water." Hard water isn't
necessarily harmful to us. However, it is known to make water have a bad taste and it causes
lime scale to build up on plumbing fixtures and pipes. Hard water can also create a scum like
appearance on clothing and dishware. If you wash your hair in hard water, it can make your hair
look dull. Having hard water can become quite costly, because of potential repair bills. While pH
levels may not adversely affect your health, it can certainly cause some problems.
To balance the pH, in drinking water, a neutralizer can be used. A neutralizer puts a chemical
solution into the water. The solution helps to prevent the water from reacting w ith any metals it
comes into contact with. This will prevent the metal from being corroded and contaminating the
water.
 Waste water Treatment

In sewage and industrial WWs treatment employing biological processes, pH must be controlled
within a range favorable to the particulate organisms involved.

 Chemical Processes

Chemical processes used to coagulate sewage or industrial wastes, dewater sludge or oxidized
certain substances such as cyanide ion, requires that the pH be controlled within rather narrow
limits.

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Measurement

a. Principle

The basic principle of electrometric pH measurement is the determination of the activity of

hydrogen ions by potentiometric measurement using a standard hydrogen electrode and a
reference electrode.

b. Apparatus
i. Self-contained pH-meter consisting of potentiometer, a glass electrode reference
electrode (combined), and a temperature compensating device.
ii. Beakers
c. Reagents
i. Standard buffer of different pH such as 7, 10 and 4.
ii. Water Sample
d. Procedure
1. Calibrate the instrument.
2. After using of apparatus for various liquid standard solutions pH changes so in order to
perform next experiment we have to make standard solution pH within neutral range.
3. So for this purpose Buffer Solutions are used to neutralize the standard solution used for
testing because buffer solutions resist against change in pH of the solution.
4. Switch on the instrument.
5. Take that sample whose pH is to be determined.
6. Insert glass electrode probe of the pH meter in the solution which was initially present in
standard buffer solution and wait for 5-10 minutes when blinking quotation of stabilizing
on the screen of pH meter stops note that reading.
7. Take the glass electrode probe out from the solution and placed again in standard Buffer
solution.
8. For next experiment repeat the previous procedure.
e. Precautions
1. The pH meter should be calibrated against standard buffer solutions of known pH prior to
measurement of a sample.
2. Fresh samples should be used to determine pH.

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3. The temperature at which measurements are made should always be reported, since pH
measurement is influenced by temperature.
4. Errors may be caused by presence of sodium at pH values greater than 10.

f. Observation & Calculation

Sample Name pH of Sample Temperature oC

Results and Discussion

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Experiment # 03
Determine the turbidity of the given solution

Related Theory
Turbidity
It is a measure of the degree to which the water loses its transparency due to the presence of
suspended particles.
Turbidity is a measure of the light scattering ability of water and is indicative of the
concentration of suspended matter in water. The turbidity of water is also related to clarity, a
measure of the transparency of water and settle-able material, which refers to suspended matter
which settle after a defined time period as opposed to that which remains in suspension.
Source of turbidity
There are three major types of particles that contribute to turbidity. The first is algae, which
grows in all kinds of lakes and streams. Second, dead organic matter (from algae, plants, bacteria
and fungi etc.) also gets washed into lakes, streams, oceans and adds more particles to the water.
Turbidity of water is due to suspended solids such as:
 Clay
 Plankton
 Slit
 Finely divided organic matter
 Microscopic organisms and similar materials
Unit of Turbidity
Because of a wide variety of materials that cause turbidity in natural waste, it has been necessary
to use arbitrary standards:
1 mg SiO2/L = 1 Unit of Turbidity. The silica used must meet certain specification as to the
particle size.
When using Nephelometer, the units are referred to as NTU = Nephelometric Turbidity Unit
Some instrument use standard as farmzaine, hence FTU units are used. Two methods are used
for the estimation of turbidity.

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Principle of turbidity meter

When particles are suspended in water and a light is shined through the sample, not all of the
light will pass straight through the sample. Instead, the light will reflect off of the suspended
particles and some of the light will exit at a right angle to the direction of entry into the sample.
Our meter uses a laser pointer as a light source, and two photodiodes as detectors for the
intensity of the transmitted and refracted light.
By measuring the voltages off of both of the photo diodes, we can derive a function which
calculates turbidity from the ratio of the voltage across the 90 degree sensor to the voltage across
the 180 degree sensor.
Environmental Significance
Turbidity is an important consideration in public water supplies for three major reasons:
 Aesthetics
Consumer of public water supplies expert and have a right to demand turbidity free water. Most
of people are aware to demand waste water is highly turbid. Any turbidity in the drinking water
is automatically associated with possible waste water pollution and the health hazards associated
by it.
 Filterability
Filtration of water is rendered more difficult costly when turbidity increases. The use of slow
sand filter has become impractical in most areas because high turbidity shortens filter runs and
increases cleaning costs. Satisfactory operation of rapid sand filter generally depends upon
effective removal of turbidity by chemical coagulation before the water is admitted to the filters.
Filters to do so can result in short filter runs and production of inferior quality water, unless
filters with special construction and operations are used.
 Disinfection
Disinfection of public water supplies is usually accomplished by means of chlorine, ozone,
chlorine dioxide or ultraviolet radiation. To be effective, there must be contact between the agent
and the organisms that the disinfection is to kill.
In turbid waters, most of the harmful organisms are exposed to the action of the disinfectant.
However, in case in which turbidity is caused by municipal waste water suspended solids or run-
off from animal feed lots, many of the pathogenic organisms may be encased in the particles and
protected from the disinfectant.

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Measurement
a. Apparatus
i. Self-Contained Turbidity Meter
b. Reagents
i. Formazin suspension
ii. Turbid free water
iii. Stock Turbidity Suspension Solution
c. Procedure
1. Select a suitable scale.
2. Add the standard solution in turbidity-meter cell and placed it in turbidly-meter.
3. Calibrate the Instrument.
4. Through shake sample. Wait until air bubbles disappear before pouring sample into
turbidity cell. When necessary, immerse turbidity tube in an ultrasonic bath for 1 to 2
seconds to dislodge bubbles. Letting the sample stand for a period of time to allow air
bubbles to dissipate will also allow solids to settle thus changing the characteristics of
the sample being evaluated.
5. Wipe outside of the tube to remove finger prints, dust dirt and water droplets. Place cell
in turbidity meter.
6. Read turbidity directly from instruments display.
d. Observation & Calculation

No of sample Source Turbidity (NTU)

1.
2.
3.
4.

e. Results & Discussion

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Experiment # 04
To determine the Total Hardness, of different water samples.

Related Theory
Scope
This method is applicable for drinking water.
Hard water
Hard Water was originally described as the soap-destroying power of water, caused by the
presence of calcium and magnesium salts and measured by titration against a standard soap
solution.
Sources of Hardness Minerals in Drinking Water
Water is a good solvent and picks up impurities easily. Pure water -- tasteless, colorless, and
odorless -- is often called the universal solvent. When water is combined with carbon d ioxide to
form very weak carbonic acid, an even better solvent results. As water moves through soil and
rock, it dissolves very small amounts of minerals and holds them in solution. Calcium and
magnesium dissolved in water are the two most common minerals that make water "hard." The
degree of hardness becomes greater as the calcium and magnesium content increases and is
related to the concentration of multivalent cations dissolved in the water. Calcium is dissolved in
water as it passes over and through limestone deposits. Magnesium is dissolved as water passes
over and through dolomite and other magnesium bearing formations. Because groundwater is in
contact with these geologic formations for a longer period of time than surface water,
groundwater is usually harder than surface water.
Although strontium, aluminum, barium, iron, manganese, and zinc also cause hardness in water,
they are not usually present in large enough concentrations to contribute significantly to total
hardness.
Types of Hardness
There are two types of hardness.

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i. Temporary Hardness
It is due to the presence of bicarbonate of calcium and magnesium and can be removed by
boiling. It is also called the carbonate hardness. It is sensitive to heat and precipitate readily at
high temperature.
ii. Permanent Hardness
It is attributed to other salts such as sulfate and chloride salts, which cannot be removed by
boiling. It is also called the non-carbonate hardness and is not sensitive to temperature.
Classification of Hardness
The degree of hardness consumers consider objectionable will vary, depending both on the water
and the degree of hardness to which consumers have become accustomed. The following table
shows a classification of water hardness:
Description of Hardness mg/L as CaCO3
Soft 0-50
Moderately Soft 50-100
Slightly Soft 100-150
Moderately Hard 150-200
Hard 200-300
Very Hard >300

Environmental Significance
 Water hardness is important to fish culture and is a commonly reported aspect of water
quality. Calcium has an important role in the biological processes of fish. It is necessary for
bone formation, blood clotting and other metabolic reactions. Fish can absorb calcium for
these needs directly from the water or food. The presence of free (ionic) calcium at relatively
high concentrations in culture water helps reduce the loss of other salts (e.g. sodium and
potassium) from fish body fluids (i.e. blood). Sodium and potassium are the most important
salts in fish blood and are critical for normal heart, nerve and muscle function. In low
calcium water, fish can lose (leak) substantial quantities of these salts into the water. Fish
must then use energy supplied by their feed to re-absorb lost salts. That can reduce the
energy available for growth and may extend the time necessary to grow fish to market

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size. For some species (e.g. red drum and striped bass), environmental calcium is required
for good survival.
 Hardness was originally defined as the capacity of water to precipitate soap. Calcium and
magnesium precipitate soap, forming a curd which causes “bathtub ring” and dingy laundry
(yellowing, graying, loss of brightness, and reduced life of washable fabrics), and feels
unpleasant on the skin (red, itchy, or dry skin). To counteract these problems, synthetic
detergents have been developed. These detergents have additives known as sequestering
agents that “tie-up” the hardness ions so they cannot form the troublesome precipitates.
Although synthetic detergents overcome these problems, both soap and detergent are wasted
by hardness.
 Hard water interferes with almost every cleaning task from laundering and dishwashing to
bathing and personal grooming. Clothes laundered in hard water may look dingy and feel
harsh and scratchy. Dishes and glasses may be spotted when dry. Hard water may cause a
film on glass shower doors, shower walls, bathtubs, sinks, faucets, etc. Hair washed in hard
water may feel sticky and look dull. Water flow may be reduced by deposits in pipes.
 Hard water is not a health hazard. In fact, the National Research Council (National Academy
of Sciences) states that hard drinking water generally contributes a small amount toward total
calcium and magnesium human dietary needs. They further state that in some instances,
where dissolved calcium and magnesium are very high, water could be a major contributor of
calcium and magnesium to the diet.
Measurement
a. Apparatus
i. Automatic burette (or conventional one)
ii. Titration glassware
b. Reagents
i. Ammonia buffer solution; for Total Hardness
ii. Eriochrome Black T, for Total Hardness
iii. Standard EDTA titrant, 0.01M

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c. Procedure
Hardness can be determined by Complex-o-metric titration.
For Total Hardness
1. Take 25 ml of water sample in titration flask.
2. Add 25 ml Distilled water in it to dilute the water solution (to avoid formation of CaCO 3).
Distilled water does not participate in ion exchange in reaction.
3. Add 1-2 ml of Buffer solution (Ammonia Buffer NH4Cl + NH4OH) to maintain pH in
solution 7-9.
4. Add small amount of EBT (Ecrichrome Black T) as indicator. As a result of addition of
EBT, solution of color changes to wine red.
5. Titrate it against 0.01N EDTA solution. Add EDTA from burette until color changes to
blue.
6. Test three samples and determine mean volume of titrant used.
7. Total Hardness (mg/L) as CaCO3 is calculated from the following formula:

Where;
Normality of EDTA = 0.01N
Volume of sample used=25ml
MW of CaCO3 = 100

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d. Observation & Calculation

Total Hardness
Sample # Initial Final Volume of Volume of Total
Reading Reading Titrant sample Hardness
used (ml) (ml) as CaCO3
(mg/L)

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Experiment # 05

Determination of chloride concentration in different water samples

Related Theory

Scope

This method is applicable to groundwater and drinking water. Detection limit is about 2 mg/L.

Introduction

Chloride is the anion of the element chlorine. Chlorine does not occur in nature, but is found
only as chloride. The chloride of sodium, potassium, calcium and magnesium are all highly
soluble in water.

Occurrence

Chloride is a common constituent in water, is highly soluble, and once in solution tends to
accumulate. Typically, concentration of chloride in fresh water range from a few to several
hundred mg/L. In sea water the concentration is approximately 19800mg/L. Chloride inputs to
surface waters can arise from irrigation return flows, sewage effluents discharges and various
industrial processes. Chloride can only be removed from water by energy-intensive processes or
ion exchange.

Environmental Significance

 Chlorides in reasonable amounts are not harmful to human.

 At concentration above 250 mg/L they give a salty taste to water.
 In many areas of the world where water supplies are scares, source containing as much as
2000mg/L are used for domestic purposes without the development of adverse effects, once
the human system become adopted to the water.
 Chlorides are used to some extent as tracer in environmental engineering practice.
 A normal 70kg human body contains approximately 81.7g of chloride & 451 of water.

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 Normal daily loss of fluid is 1.5-2.0 of water and 4g of chloride. 90-95% of the Cl- losses
occur in urine 4-8% in faeces and 2% in sweat.

Measurement

a. Apparatus
i. Photometer
ii. Volumetric flask
b. Reagents
i. Standard silver nitrate solution
ii. Standard sodium chloride solution
iii. Potassium chromate indicator solution
iv. Sodium Hydroxide solution
c. Procedure
1. Add 10ml of water sample in to a test tube with pipette.
2. Add 1 blue microscope (in the cup of chlorine reagent) of reagent Cl - and shake
vigorously until the reagent is completely dissolved.
3. Leave the test tube in stand for 1 min to complete reaction.
4. Fill the sample in to the cell.
5. Measure in the photometer.
d. Precautions
i. For photometric measurement the cells must be clean.
ii. pH of solution must be within the range 4.5-5.5.
e. Observation & Calculation

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Experiment # 06

To determine the amount of sulfates in water

Related theory

Scope

This method is applicable to ground water. The minimum detection level is about 1 mg/L.

Introduction

The sulfate ion is one of the major anions occurring in natural water. Sulfates are important in
public and industrial water supplies because of the tendency of water containing appreciable
amount to form hard scale in boilers and heat exchangers.

Sulfates form salts with various cations such as potassium, sodium calcium, magnesium, barium,
lead and ammonium. Potassium, sodium, magnesium and ammonium sulfates are highly soluble,
where calcium sulfate is partially soluble and barium and lead sulfates are insoluble. Sulfate is
one of the major dissolved components of rain.

Sulfate is a common constituent of water and arises from the dissolution of mineral sulfates in
soil and rock, particularly calcium sulfate (Gypsum) and other partially soluble sulfate minerals.

Typically, the concentration of sulfate in:

o Surface water is 5 mg/L, although concentration of several 100mg/L may occur where
dissolution of sulfate rich effluent from acid mine drainage take place; and
o Sea water is just over 900mg/L

Sources

i. Sulfate ores
ii. The presence of shale’s
iii. Industrial wastes

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Environmental Significance

 The sulfate content is an important consideration in determining their suitability for public
and industrial water supplies.
 It is important in public water supplies because of its cathartic effects on humans, when it is
present in the excessive amounts. For this reasons the recommends upper limit is 250 mg/L
in the waters intended for human consumption.
 People not used to drinking water with high levels of sulfates can experience dehydration and
diarrhea. Kids are often more sensitive to sulfate than adults. As a safety measure, water with
sulfate level exceeding 400mg/L should not be used in the preparation of baby food. Elder
children and adults become used to high sulfate levels after a few days.

Measurement

a. Principle

Sulfate ion is precipitated in HCl medium with BaCl2 so as to form BaSO4 crystals of uniform
size. Light absorbance of BaSO4 suspension by nephelometer (Turbiditi-meter) and the sulfate
concentration is determined with the help of a prepared standard curve.

b. Apparatus
o Magnetic stirrer
o Nephelometer
o Stopwatch
o Measuring spoon, Capacity (0.2-0.3)
c. Procedure
i. Formation of barium sulfate turbidity

Measure 100ml sample or a suitable portion made up to 100ml into a 250ml

Erlenmeyer flask. Add 20ml buffer solution and mix in stirring apparatus. While
stirring add a spoonful of BaCl2 crystals and begin timing immediately. Stir for 60+2
sec at constant speed.

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ii. Measurement of Barium sulfate turbidity

After stirring period has ended, pour solution into turbidi-meter and measure the
turbidity.

iii. Preparation of Calibration curve

Estimate SO42- standard by comparing turbidity reading with a calibration curve

prepared by carrying sulfate standards through the entire procedure. Space standard at
5 mg/L increments in a 0 to 40 mg/L sulfate range. Above 40mg/L the accuracy of
the method decreases.

d. Observation and calculation

Sr # Concentration of sulfates (mg/L) Turbidity (NTU)

Blank

1. 0

2. 5

3. 10

4. 15

5. 20

6. 25

7. 30

8. 35

9. 40

Tap Water

Concentration of sulfates from calibration curve (mg/L) =

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Experiment# 07
Determination of Total Suspended Solids, Total Fixed Solids and Total
Volatile Solids

Related Theory
Scope
The procedure is applicable to wasters of wide range of quality including surface water,
industrial and domestic effluents and treated wastewater.
Introduction
Environmental engineering is concerned with the solid material in a wide range of natural waters
and wastewaters. The usual definition of solids (referred to as "total solids") is the matter that
o
remains as residue upon evaporation at 103~105 C. The organic fraction of solid material is
o
estimated (by weight loss) by burning the sample at 500 ± 50 C to volatilize the organics. The
various components of "total solids" can be simplified as follows:

Figure1: Solids Classification.

Environmental Significance:

The total solids (TS) contents of sludges are used in the design and process control of wastewater
treatment facilities. Total dissolved solids (TDS) are used to evaluate the suitability of water for
both domestic supplies and industrial purposes. The total suspended solids (TSS), including the

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volatile fraction (VSS), are commonly monitored to evaluate the degree of pollution in natural
waters and serves as a key process control parameter for wastewater treatment operation.

DETERMINATION OF TOTAL SUSPENDED SOLIDS (TSS)

Definition
It refers to the solid material in water and wastewater sample which is retained by a filter of 2.0
µm (or smaller) nominal size under specified conditions.
Purpose
TSS is an important parameter in wastewater treatment. The data obtained from this test is used
in the design of wastewater treatment plants.
Interferences
i. Exclude large floating particles or submerged agglomerates of non homogeneous
materials from the sample if it is determined that their inclusion is not representative.
ii. For samples with high TDS thoroughly wash the filter to ensure removal of dissolved
materials.
Apparatus
i. Dessicator
ii. Drying oven
iii. Analytical balance
iv. Filtration apparatus
v. Fiber filter disks
vi. Muffle furnace
vii. Petri dishes.
Procedure
1. Weigh out the fibre filter papers on the analytical balance.
2. Attach the assembly of the vacuum filtration unit.
3. Take 50 mL sample volume and filter through using the vacuum pump as an aid. Continue
suction for three minutes to ensure all dissolved solids have been removed.
4.After the vacuum filtration process, take the filter paper and dry it.
5.Transfer the filter paper in a petri (pyrex) dish and cover it with a lid. Place this dish into an
oven at 102 to 105 °C temperature for 30 to 60 minutes till the solids are dried.
6.After this place the filter paper in a dessicator for cooling.

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7. Weigh the dried solids.

Calculation
TSS (mg/L) = * 1000*1000

C= Weight of dried residue and filter in g

X= initial weight of the filter in g.

DETERMINATION OF TOTAL FIXED AND VOLATILE SUSPENDED SOLIDS:

Definition
Fixed solids is the term applied to the residue of total suspended solids after ignition for a
specified time at a 550 º C. Volatile solids is the term used for the weight lost on ignition of the
same sample.
Purpose
In wastewater treatment volatile suspended solids are considered to depict the biomass of
wastewater (presence of microbes and bacteria). Therefore their determination is helpful in the
design of a secondary wastewater treatment system. Fixed solids are considered to be the
inorganic constituents of wastewater and give an estimate of the inorganic component.
Procedure
1. After performing the filtration of the sample, perform the test of TSS.
2. Using the dried filter, ignite the sample in a muffle furnace at 550 º C for 15 to 20 minutes.
3. Ensure that the filter sample is completely covered in the petri dish.
4. After the dish has been ignited, place the dish to be cooled in the dessicator.
5. Weigh the fibre filter paper on the analytical balance.
Calculation
( )
VSS (mg/L) =
( )
FSS (mg/L) =

A= weight of dried residue and dish or filter before ignition (g)

B= weight of residue and dish/filter after ignition (g)
E= weight of dish or filter (g)

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