Sanitary Manual

"Yarmouk University"
"Hijjawi Faculty for Engineering Technology"

"Department of Civil Engineering"
"Sanitary Engineering laboratory CE 453"
Sanitary Engineering
Laboratory Manual
 Table of contents
Experiment Page
Basic orientation on safety measures in the sanitary engineering LAB 1
Introduction for preparing solutions 9
Solids determination and gravimetric analysis 14
Beer’s law and spectrophotometric analysis 21
Titration skills and acid / base chemical analyses 26
Determination of water alkalinity 36
Determination of Hardness 41
pH, Turbidity and Electrical Conductivity (EC) 45
Jar Test and Modeling of the coagulation-flocculation process 50
Determination of 5-day BOD of wastewater samples 54
Data sheet 60
Basic orientation on safety
measures and regulations in
the laboratory
Prepared by Eng. Elham G.Al-Hamaideh 1

Syllabus
❖ Description:
This Lab course is intended to practice basic water quality analyses. Gravimetric,
volumetric and spectrophotometeric analytical methods are used to determine quality
parameters of raw water, finished water and wastewater. Parameters tested include
alkalinity, hardness, salinity and solids, BOD.
❖ Textbooks and Readings:
Water quality LAB Manual, assembled by Shahalam
❖ Reference:
1. Handout Materials
2 .Water Supply and Pollution Control, 5th edition, Viessman, Jr. and Hammer,
HarperCollins College Publishers, 1993.
3 .Wastewater Engineering: Treatment, Disposal and Reuse, Metcalf & Eddy, Inc., 3rd
ed., 1991.
❖ Goals
This course is designed to provide the students with hands on experience in practicing
laboratory procedures on selected parameters of water quality-as applied to schemes of
water and wastewater treatment.
❖ Learning Outcomes
1. Basic orientation on safety measures in the sanitary engineering LAB.
2. Solids determination and gravimetric analysis.
3. Beer’s law and spectrophotometric analysis as.
4. Titration skills and acid / base chemical analyses.
5. Determination of water alkalinity.
6. Determination of water hardness.

7. Determination of pH, Turbidity, and electrical conductivity (EC) for different
water samples.
8. Jar Test and Modeling of the coagulation-flocculation process
9. Determination of 5-day BOD in influent and effluent of wastewater treatment plants
❖ Marks
Reports 25 %
Midterm Exam 30 %
Quizzes 5%
Final Exam 40 %

Course Outline
Basic orientation on safety measures in the sanitary

1 Lab Session
engineering LAB
Solids determination and gravimetric analysis 1 Lab Session
Beer’s law and spectrophotometric analysis 1 Lab Session
Titration skills and acid / base chemical analyses 1 Lab Session
Determination of water alkalinity 1 Lab Session
Determination of water hardness 1 Lab Session
Determination of pH, Turbidity, EC and for different

1 Lab Session
waters samples
Jar Test and Modeling of the coagulation-flocculation

1 Lab Session
process
Determination of 5-day BOD in influent and effluent of

1 Lab Session
wastewater treatment plants

Regulation and Safety Rules
✓ Introduction
Safety is a collective responsibility that requires the full cooperation of everyone in the
laboratory. However, the ultimate responsibility for safety rests with the person actually
carrying out a given procedure. In the case of an academic laboratory, that person is
usually the student. Accidents often result from an indifferent attitude, failure to use
common sense, or failure to follow instructions. Each student should be aware of what
the other students are doing because all can be victims of one individual's mistake. Do
not hesitate to point out to other students that they are engaging in unsafe practices or
operations. If necessary, report it to the instructor. In the final assessment, students have
the greatest responsibility to ensure their own personal safety. This guide provides a list
of do's and don'ts to minimize safety and health problems associated with experimental
laboratory work. It also provides, where possible, the ideas and concepts that underlie
the practical suggestions. However, the reader is expected to become involved and to
contribute to the overall solutions. The following are general guidelines for all
laboratory workers:
1) Follow all safety instructions carefully.
2) Become thoroughly acquainted with the location and use of safety facilities such as
safety showers, exits and eyewash fountains.
3) Become familiar with the hazards of the chemicals being used, and know the safety
precautions and emergency procedures before undertaking any work.
4) become familiar with the chemical operations and the hazards involved before
beginning an operation.
✓ Personal Protection
• Eye Protection
All people in the laboratory including visitors must wear eye protection at all times,
even when not performing a chemical operation. Wearing of contact lenses in the
laboratory is normally forbidden because contact lenses can hold foreign materials
against the cornea. Furthermore, they may be difficult to remove in the case of a splash.
Soft contact lenses present a particular hazard because they can absorb and retain
chemical vapors. If the use of contact lenses is required for therapeutic reasons fitted
goggles must also be worn. In addition, approved standing shields and face shields that
protect the neck and ears as well as the face should be used when appropriate for work

at reduced pressure or where there is a potential for explosions, implosions or splashing.
Normal prescription eyeglasses, though meeting the Food and Drug Administration's
standards for shatter resistance, do not provide appropriate laboratory eye protection.
• Clothing
Clothing worn in the laboratory should offer protection from splashes and spills, should
be easily removable in case of accident, and should be at least fire resistant.
Nonflammable, nonporous aprons offer the most satisfactory and the least expensive
protection. Lab jackets or coats should have snap fasteners rather than buttons so that
they can be readily removed. High-heeled or open-toed shoes, sandals, or shoes made
of woven material should not be worn in the laboratory. Shorts, cutoffs and miniskirts
are also inappropriate. Long hair and loose clothing should be constrained. Jewelry such
as rings, bracelets, and watches should not be worn in order to prevent chemical seepage
under the jewelry, contact with electrical sources, catching on equipment, and damage
to the jewelry.
• Gloves
Gloves can serve as an important part of personal protection when they are used
correctly. Check to ensure the absence of cracks or small holes in the gloves before
each use. In order to prevent the unintentional spread of chemicals, gloves should be
removed before leaving the work area and before handling such things as telephones,
doorknobs, writing instruments, computers, and laboratory notebooks. Gloves may be
reused, cleaned, or discarded, consistent with their use and contamination.
A wide variety of gloves is available to protect against chemical exposure. Because the
permeability of gloves of the same or similar material varies from manufacturer to
manufacturer, no specific recommendations are given here. Be aware that if a chemical
diffuses through a glove, that chemical is held against the worker's hand and the
individual may then be more exposed to the chemical than if the glove had not been
worn.
• Personal Hygiene
Everyone working in a chemistry laboratory should be aware of the dangers of ingesting
chemicals. These common sense precautions will minimize the possibility of such
exposure:
1) Do not prepare, store (even temporarily), or consume food or beverages in any
chemical laboratory.

2) Do not smoke in any chemical laboratory. Additionally, be aware that tobacco
products in opened packages can absorb chemical vapors.
3) Do not apply cosmetics in a laboratory.
4) Wash hands and arms thoroughly before leaving the laboratory, even if gloves have
been worn.
5) Wash separately from personal laundry, lab coats or jackets on which chemicals have
been spilled.
6) Never wear or bring lab coats or jackets into areas where food is consumed.
7) Never pipette by mouth. Always use a pipette aid or suction bulb.
✓ Laboratory Protocol
The chemistry laboratory is a place for serious learning and working. Horseplay cannot
be tolerated. Variations in procedures including changes in quantities or reagents may
be dangerous. Such alterations may only be made with the knowledge and approval of
the instructor.
• Housekeeping
In the laboratory and elsewhere, keeping things clean and neat generally leads to a safer
environment. Avoid unnecessary hazards by keeping drawers and cabinets closed while
working. Never store materials, especially chemicals, on the floor, even temporarily.
Work spaces and storage areas should be kept clear of broken glassware, leftover
chemicals and scraps of paper. Keep aisles free of obstructions such as chairs, boxes
and waste receptacles. Avoid slipping hazards by keeping the floor clear of ice,
stoppers, glass beads or rods, other small items, and spilled liquids. Use the required
procedure for the proper disposal of chemical wastes and solvents.
• Cleaning Glassware
Clean glassware at the laboratory sink or in laboratory dishwashers. Use hot water, if
available, and soap or other detergent. If necessary, use a mild scouring powder.
Wear appropriate gloves that have been checked to ensure that no holes are present.
Use brushes of suitable stiffness and size. Avoid accumulating too many articles in the
cleanup area. Usually work space around a sink is limited and piling up dirty or cleaned
glassware leads to breakage. Remember that the turbid water in a sink may hide a jagged
edge on a piece of broken glassware that was intact when put into the water. A pair of
heavy gloves may be useful for removing broken glass, but care must
be exercised to prevent glove contamination. To minimize breakage of glassware, sink
bottoms should have rubber or plastic mats that do not block the drains.

Avoid the use of strong cleaning agents such as nitric acid, chromic acid, sulfuric acid,
strong oxidizers, or any chemical with a "per" in its name (such as perchloric acid,
ammonium persulfate, etc.) unless specifically instructed to use them, and then only
when wearing proper protective equipment. A number of explosions involving strong
oxidizing cleaning solutions, such as chromic sulfuric acid mixtures, have been
reported. The use of flammable solvents should be minimized and, when they are used,
appropriate precautions must be observed.
✓ Working Alone
Avoid working alone in a building or in a laboratory.
✓ Reports:
Reports on experiments will be due ONE WEEK after the experiment is completed, at
the beginning of each class. Reports submitted after 14:00 on will be counted as one
day late. Late reports are accepted for only 2 days and will be penalized 35 % per day.
No report after that day will be accepted at all.

Introduction for Preparing
Chemical Solutions

Experiment #1: Introduction for Preparing Chemical Solutions
Lab experiments and types of research often require preparation of chemical solutions in their
procedure. To carry out this, it is very important to understand basic terms which are:
• Solute - The substance which dissolves in a solution

• Solvent - The substance which dissolves another to form a solution. For example, in a
sugar and water solution, water is the solvent; sugar is the solute.
• Solution - A mixture of two or more pure substances. In a solution one pure substance
is dissolved in another pure substance homogenously. For example, in a sugar and
water solution, the solution has the same concentration throughout, ie. it is homogenous
There are a number of different ways of expressing solute concentration that are
commonly used. Some of these are listed below.
1. Molarity "M"
The molarity of a solution is calculated by taking the moles of solute and dividing by the liters
of solution.
𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 (𝑚𝑜𝑙𝑒𝑠)

𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 =
𝑙𝑖𝑡𝑒𝑟𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 (𝐿)
o Examples
- Ex#1:
What is the molarity when 0.75 mol is dissolved in 2.50 L of solution?
0.75 (𝑚𝑜𝑙𝑒𝑠)
𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 = = 0.3 𝑀
2.5 (𝐿)
- Ex#2:
Calculate the molarity of 25.0 grams of KBr dissolved in 750.0 mL.
𝑚𝑎𝑠𝑠 (𝑔) 25 (𝑔)

𝑚𝑜𝑙𝑒𝑠 = = = .210 𝑚𝑜𝑙
𝑀. 𝑚 (𝑔/𝑚𝑜𝑙) 119 (𝑔/𝑚𝑜𝑙)
0.210 (𝑚𝑜𝑙𝑒𝑠)
𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 = = .280 𝑀
0.75 (𝐿)

2. Molality "m"
The molality of a solution is calculated by taking the moles of solute and dividing by the
kilograms of solvent.

𝑀𝑜𝑙𝑎𝑙𝑖𝑡𝑦 =
𝑘𝑖𝑙𝑜𝑔𝑟𝑎𝑚𝑠 𝑜𝑓 𝑠𝑜𝑙𝑣𝑒𝑛𝑡 (𝐾𝑔)
o Examples
- Ex#1:
Suppose you had 2.00 moles of solute dissolved into 1.00 L of solvent (water).
What's the molality?

𝑀𝑜𝑙𝑎𝑙𝑖𝑡𝑦 =
𝑘𝑖𝑙𝑜𝑔𝑟𝑎𝑚𝑠 𝑜𝑓 𝑠𝑜𝑙𝑣𝑒𝑛𝑡 (𝐾𝑔)
𝑚𝑎𝑠𝑠 (𝑔) 𝑔 𝑚𝑎𝑠𝑠

𝑑𝑒𝑛𝑠𝑖𝑡𝑦 = = 1000 = → 𝑚𝑎𝑠𝑠 = 1000𝑔 = 1 𝑘𝑔
𝑣𝑜𝑙𝑢𝑚𝑒 (𝑙) 𝑙 1𝑙
2 (𝑚𝑜𝑙𝑒𝑠)
𝑚𝑜𝑙𝑎𝑙𝑖𝑡𝑦 = = 2𝑚
1 (𝐾𝑔)
- Ex#2:
80.0 grams of glucose (C6H12O6, mol. wt = 180. g/mol) is dissolved in1.00 kg of

water. Calculate the molality.
𝑚𝑎𝑠𝑠 (𝑔) 80 (𝑔)
𝑚𝑜𝑙𝑒𝑠 = = = 0.444 𝑚𝑜𝑙
𝑀. 𝑚 (𝑔/𝑚𝑜𝑙) 180 (𝑔/𝑚𝑜𝑙)
0.444(𝑚𝑜𝑙𝑒𝑠)
𝑀𝑜𝑙𝑎𝑙𝑖𝑡𝑦 = = .444 𝑚
1 (𝑘𝑔)
3. Normality (N)
The normality of a solution is the gram equivalent weight of a solute per liter of solution. A
gram equivalent weight or equivalent is a measure of the reactive capacity of a given chemical
species (ion, molecule, etc.). Normality is the only concentration unit that is reaction dependent.
# 𝑜𝑓 𝑒𝑞. 𝑤𝑡
𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦 =
1 𝐿 𝑜𝑓 𝑠𝑜𝑙𝑣𝑒𝑛𝑡
𝑀. 𝑤
𝑒𝑞. 𝑤𝑡 =
𝑐ℎ𝑎𝑟𝑔𝑒

o Examples
- Ex#1:
1 M sulfuric acid (H2SO4) is 2 N for acid-base reactions because each mole of sulfuric acid
provides 2 moles of H+ ions.
4. Percent by weight
Another similar way of expressing the concentration of a solution is to express it in weight

percent.
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒
𝑊𝑒𝑖𝑔ℎ𝑡 𝑝𝑒𝑟𝑐𝑒𝑛𝑡 = ∗ 100%
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛
o Examples
- Ex#1:
What is the weight percent of glucose in a solution made by dissolving 4.6 g of glucose in 145.2
g of water?
4.6 𝑔
𝑊𝑒𝑖𝑔ℎ𝑡 𝑝𝑒𝑟𝑐𝑒𝑛𝑡 = ∗ 100% = 3.1𝑔𝑙𝑢𝑐𝑜𝑠𝑒
(4.6 + 145.2)𝑔
5. Percent by volume
Volume percent is usually used when the solution is made by mixing two liquids
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒
𝑣𝑜𝑙𝑢𝑚𝑒 𝑝𝑒𝑟𝑐𝑒𝑛𝑡 = ∗ 100%
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛
- Ex#1:
Rubbing alcohol is generally 70% by volume isopropyl alcohol. That means that 100 ml of
solution contains 70 ml of isopropyl alcohol. That also means that a liter (or 1000 ml) of this
solution has 700 ml of isopropyl alcohol plus enough water to bring it up a total volume of 1
liter, or 1000 ml.
 Dilution of solution

To dilute a solution means to add more solvent without the addition of more solute. Of
course, the resulting solution is thoroughly mixed so as to ensure that all parts of the solution
are identical. The fact that the solute amount stays constant allows us to develop calculation
techniques.
𝑚𝑜𝑙𝑒𝑠 𝑠𝑜𝑙𝑢𝑡𝑒 𝑏𝑒𝑓𝑜𝑟𝑒 𝑑𝑖𝑙𝑢𝑡𝑖𝑜𝑛 = 𝑚𝑜𝑙𝑒𝑠 𝑠𝑜𝑙𝑢𝑡𝑒 𝑎𝑓𝑡𝑒𝑟 𝑑𝑖𝑙𝑢𝑡𝑖𝑜𝑛
From rearranging the equation that defines molarity, we know that the moles of solute equals
the molarity times the volume. (Calculating the moles of solute from molarity times volume
will be very useful in other areas of chemistry, particularly acid base. Remember that the
volume must be in liters.So we can substitute MV (molarity times volume) into the above
equation, like this:
𝑀1𝑉1 = 𝑀2𝑉2
The "sub one" refers to the situation before dilution and the "sub two" refers to after dilution.
Example #1:
53.4 mL of a 1.50 M solution of NaCl is on hand, but you need some 0.800 M solution. How
many mL of 0.800 M can you make?
Using the dilution equation,:
(1.50 𝑚𝑜𝑙/𝐿) (53.4 𝑚𝐿) = (0.800 𝑚𝑜𝑙/𝐿) (𝑥)
𝑥 = 100. 𝑚𝐿
 Dilution factor
Dilution factor refers to the ratio of the volume of the initial (concentrated) solution to the
volume of the final (dilute) solution
𝑉𝑓
𝐷. 𝐹 =
𝑉𝑖
What is the dilution factor if you add a 0.1 mL aliquot of a specimen to 9.9 mL of diluent?
𝑉𝑓 0.1 + 9.9
𝐷. 𝐹 = = = 100
𝑉𝑖 0.1

Determination of Solids in
Water Samples

Experiment #2: Determination of Solids in Water Samples
• Introduction & principle

‘Total solids’ is the term applied to the material left in the vessel after evaporation of a sample
of water/waste water and its subsequent drying in an oven at a definite temperature. Total solids
include “total suspended solids” the portion of total solids retained by a filter and “total
dissolved solids” the portion that passes through the filter. Fixed solids is the residue remaining
after ignition for 1 hour at 550°C. The solid portion that is volatilised during ignition is called
volatile solids. It will be mostly organic matter. Waters that are low in organic matter and total
mineral content and are intended for human consumption may be examined under 103–105°C
or 179–181°C. But water containing considerable organic matter or those with pH over 9.0
should be dried at 179–181°C. In any case, the report should indicate the drying temperature.
The sample is filtered and the filtrate evaporate in a weighed dish on a steam bath, the residue
left after evaporation is dried to constant weight in an oven at either 103–105°C or 179–181°C.
The increase in weight over that of the empty dish represents total dissolved solids and includes
all materials, liquid or solid, in solution or otherwise, which passes through the filter and not
volatilised during the drying process. The difference between the total solids and the total
dissolved solids will give the total suspended solids. The dishes with the residue
retained after completion of the tests for total solids and total dissolved solids are
subjected to heat for 1 hour in a muffle furnace held at 550°C. The increase in weight
over that of the ignited empty vessel represents fixed solids in each instance. The
difference between the total dissolved/total suspended solids and the corresponding
fixed solids will give volatile solids in each instance. All the quantities should be
expressed in mg/L. Settleable matter in surface and saline waters as well as domestic
and industrial wastes may be determined and reported on a volume basis as
millilitre per litre.
• Aim
The aim of the experiments is to determine the following types of solids in the given
sample:
- Total Solids (TS)
- Total Fixed (inorganic) Solids (TFS)
- Total Volatile (organic) Solids (TVS)
- -Total Dissolved Solids (TDS)
- Total Suspended Solids (TSS)

• Apparatus & tools
1. Porcelain evaporating dishes of 150–200 mL capacity
2. Crucible 25-50 ml capacity
3. Drying oven
4. Desiccators
5. Analytical balance or monopan balance
6. Filter paper (preferably of glass fibre)
7. Electric muffle furnace
8. funnel and side arm flask
9. measuring cylinder 50 ml capacity
10. filter paper
11. vacuum pump

• Procedure
 Part #1: TS, TFS, TVS
 (Total solids TS)
1. Switch on the balance
2. Note down the initial day weight of crucible (W1)
3. Take water sample in crucible (V)
4. Place the crucible inside the draying oven at 103 CO
5. After draying in the oven cool in room temperature in desiccators
6. Note down the final drying weight of crucible (W2)
𝑊2 −𝑊1
❖ Total Solid (TS) (g/L) = 𝑉

(Total Fixed Solids TFS)
1. Note down the final day weight of crucible (W2)
2. Place the crucible inside the muffle furnace at 550 CO
3. After draying in the oven cool to room temperature in desiccators
4. Note down the final drying weight of crucible (W3)
𝑊3 −𝑊1
❖ Total Fixed Solid (TFS) (inorganic matter) (g/mL) = 𝑉
𝑊2 −𝑊3
❖ (TVS) (Organic matter) (g/L) = 𝑉
❖ TS=TFS+TVS

 Part #2 TSS, TDS
 ( Total Dissolved Solids TDS)
2. Note down the initial dry weight of evaporating dish (W1)
3. Filter the water sample using whattman filter paper
4. Take volume of filtered water sample in the dish
5. Place the dish in the drying oven at 103 Co
7. Note down the final dry weight of dish (W2)
𝑊2 −𝑊1
❖ Total Dissolved Solid (TDS) (g/L) (evaporating dish) = 𝑉

 ( Total Suspended Solids TDS)
2. Note down the initial dry weight of filter paper (W1)
3. Filter the water sample using whattman filter paper
4. Take the filter paper and place it of in the dish
5. Place the dish in the drying oven at 103 Co
7. Note down the final dry weight of the filter paper (W2)
𝑊2 −𝑊1
❖ Total Suspended Solid (TSS) (filter paper) (/L) = 𝑉

Beer’s law and
spectrophotometric analysis

Experiment #3: Beer’s law and spectrophotometric analysis
• Introduction
Some solutions absorb light at certain visible wavelengths more than others. This
property gives the solution a colour which can be observed by the eye. Copper sulphate
is blue in solution, since the Cu2+ ions absorb the red (longer wavelength) light which
pass through. The amount of light absorbed is proportional to the concentration of the
solution, and the path length through which the light passes. This is shown by the
Lambert-Beer law:
𝐴 = 𝜀 ∗ 𝑙∗ 𝑐
where A is the absorbance, c the concentration (in molar), l the length in cm, and ε is a
constant (think of the unit), known as the molar extinction coefficient. In order to
measure absorbance, a spectrophotometer is used. The spectrophotometer can be set to
a precise light wavelength, for example 600 nm for red light, and zeroed using a solution
which does not absorb at the wavelength of interest, for example water. To measure the
absorbance of a coloured solution, the solution is first transferred into a cuvette in which
the path length (l) is known precisely. The cuvettes we used were 1 cm in length. Plastic
cuvettes are OK when measuring using visible light, but for measuring at UV
wavelengths, special quartz glass cuvettes are required. The extinction coefficient for a
certain solution can be determined as follows. Using a solution of known concentration,
a series of known dilutions is made and the absorbance measured. A plot of absorbance
vs. concentration (in molar) gives a straight line whose equation is given by the
Lambert-Beer law. The slope of the line is the molar extinction coefficient. The reason
for taking many measurements rather than just one is to reduce the possible errors in
dilution and measurement.

• Principle
❖ The diagram below shows a cuvette with initial light P0, directed at a sample
solution. The sample absorbs the initial light P0 and radiates the remaining light P.
The amount of light absorbed can be measured in a few ways:
- 𝑇𝑟𝑎𝑛𝑠𝑚𝑖𝑡𝑡𝑎𝑛𝑐𝑒, (𝑇) = 𝑃 / 𝑃0
- % 𝑇𝑟𝑎𝑛𝑠𝑚𝑖𝑡𝑡𝑎𝑛𝑐𝑒, %𝑇 = 100 𝑇
- 𝐴𝑏𝑠𝑜𝑟𝑏𝑎𝑛𝑐𝑒 (𝐴) = −𝑙𝑜𝑔 10 𝑇
- Absorbance (𝐴) = 𝜀 ∗ 𝑙 ∗ 𝑐
The relationship between absorbance and transmittance is illustrated in the following

diagram:
So, if all the light passes through a solution without any absorption, then absorbance is
zero, and percent transmittance is 100%. If all the light is absorbed, then percent
transmittance is zero, and absorption is infinite.
❖ For preparing different samples, from the 0.4 M stock solution we made 10
dilutions by taking 1 ml, 2 ml, 3 ml, ..., 10ml and then making the total volume up to
10 ml using distillation water. Different volumes of pipette are used in this
experiment. The absorbance of each solution is measured in a plastic cuvette with 1
cm path length using a spectrophotometer (DR- Absorption device) at a wavelength
of (600-630) nm. The spectrophotometer is first zeroed at this wavelength using water
blank. For preparing 0.4M of CuSO4, use the following equation:
𝑚
# 𝑜𝑓 𝑚𝑜𝑙𝑒𝑠 = =𝑀×𝑉
𝑚𝑤
• Aim
- Prepare and test the absorbance of five standard copper (II) sulfate solutions.

- Calculate a standard curve from the test results of the standard solutions.
- Test the absorbance of a copper (II) sulfate solution of unknown molar
concentration
- Calculate the molar concentration of the unknown copper (II) sulfate solution
• Apparatus &Materials
- CuSO4 as solid matter
- Distilled water
- Bottles
- Pipettes and pipette wheel
- Cuvette
- Spectrophotometer
- Beakers
- Test tubes
- Magnetic stirrer
- Glass stirrer
- Analytical balance

• Procedure
1. Obtain small volumes of 0.40 M CuSO4 solution and distilled water in separate
beakers.
2. Label five clean, dry, test tubes 1–5. Use pipettes to prepare five standard
solutions according to the table below (total volume of the solution =10 ml)
Thoroughly mix each solution with a stirring rod. Clean and dry the stirring rod
between uses.
 Note (use dilution principle to find concentration of standard solution)
𝑀1𝑉1 = 𝑀2𝑉2
3. Prepare a blank by filling a cuvette 3/4 full with distilled water. To correctly
use cuvettes, remember:
a. Wipe the outside of each cuvette with a lint-free tissue.
b. Handle cuvettes only by the top edge of the ribbed sides.
c. Dislodge any bubbles by gently tapping the cuvette on a hard surface.
d. Always position the cuvette so the light passes through the clear sides.
4. Read and record absorbance value for each sample.
5. Plot standard liner curve between absorbance (A) vs. concentration (C)
6. Find slope and standard molar coefficient then find the molar concentration of
the unknown copper (II) sulfate solution

Acid-Base
Titration

Experiment #4: Acid-Base Titration
• Introduction
Titration is an analytical method used to determine the exact amount of a substance by
reacting that substance with a known amount of another substance. . The completed
reaction of a titration is usually indicated by a color change or an electrical
measurement. An acid/base neutralization reaction will yield salt and water. In an acid-
base titration, the neutralization reaction between the acid and base can be measured
with either a color indicator or a pH meter.
𝐴𝑐𝑖𝑑 + 𝐵𝑎𝑠𝑒 → 𝑆𝑎𝑙𝑡 + 𝑊𝑎𝑡𝑒𝑟
Phenolphthalein color indicator will be used in this experiment. Phenolphthalein is

colorless in acidic solutions and pink in basic solutions. Phenolphthalein is also used in
forensic crime scene analysis to detect the presence of blood, Kastle-Meyer test. In the
Kastle-Meyer test, hemoglobin catalyzes the oxidation of the colorless form of
phenolphthalein to its bright pink form.
Definitions
✓ The analyte (titrand) is the solution with an unknown molarity (solution in

conical flask)
✓ The reagent (titrant) is the solution with a known molarity that will react with
the analyte. (solution in burette)
✓ Indictor is a chemical reagent used to recognize the attainment of end point or
equivalent point in a titration. After the reaction between the substance and the
standard solution is complete, the indicator should give a clear colour change.
❖ Different methods to determine the endpoint include:
✓ pH indicator:
A pH indicator is a substance that it changes its colour in response to a chemical

change. An acid-base indicator changes its colour depending on the pH
• Indicators Used for Various Titrations:

Reaction Type Suitable Indicators
Strong Acid against a Strong
methyl orange, methyl red and phenolphthalein
Base
Weak Acid against Strong Base
Phenolphthalein
Strong Acid against Weak Base:
methyl orange
✓ pH meter:
It is a potentiometer that uses an electrode whose potential depends on the amount

of H+ ion present in the solution. (It is an example of an ion-selective electrode.)
This allows the pH of the solution to be measured throughout the titration. At the
endpoint, there will be a sudden change in the measured pH. This method is more
accurate than the indicator method and is very easily automated.
✓ Colour change:
In some reactions, the solution changes colour without any added indicator. This is
often seen in redox titrations, for instance, when the different oxidation states of the
product and reactant produce different colour
• Aim
The main aim of this experiment is to find the equivalent and end points and to draw
titration curve for "strong acid -strong base" reaction by using titration technique where
this technique can be defined as an analytical method used to determine the exact
amount of a substance by reacting that substance with a known amount of another
substance.
• Principle
pH (Titration) Curves
1. Titration curves for strong acid v strong base
𝑁𝑎𝑂𝐻 + 𝐻𝐶𝐿 → 𝑁𝑎𝐶𝐿 + 𝐻2 𝑂
- Case I: Running acid into the alkali
You can see that the pH only falls a very small amount until quite near the equivalence
point. Then there is a really steep plunge. If you calculate the values, the pH falls all the
way from 11.3 when you have added 24.9 cm3 to 2.7 when you have added 25.1 cm3.

- Case II: Running alkali into the acid
This is very similar to the previous curve except, of course, that the pH starts off low and
increases as you add more sodium hydroxide solution. Again, the pH doesn't change very much
until you get close to the equivalence point. Then it surges upwards very steeply.
2. Titration curves for strong acid v weak base

This time we are going to use hydrochloric acid as the strong acid and ammonia solution as the
weak base.
Because you have got a weak base, the beginning of the curve is obviously going to be
different. However, once you have got an excess of acid, the curve is essentially the same
as before. attached
At the very beginning of the curve, the pH starts by falling quite quickly as the acid is added,
but the curve very soon gets less steep. This is because a buffer solution is being set up -
composed of the excess ammonia and the ammonium chloride being formed.

Notice that the equivalence point is now somewhat acidic ( a bit less than pH 5), because pure
ammonium chloride isn't neutral.
At the beginning of this titration, you have an excess of hydrochloric acid. The shape of the
curve will be the same as when you had an excess of acid at the start of a titration running
sodium hydroxide solution into the acid.
3. Titration curves for weak acid v strong base
We'll take ethanoic acid and sodium hydroxide as typical of a weak acid and a strong
base.

4. Titration curves for weak acid v weak base
The common example of this would be ethanoic acid and ammonia.
It so happens that these two are both about equally weak - in that case, the equivalence
point is approximately pH 7.
This is really just a combination of graphs you have already seen. Up to the equivalence
point it is similar to the ammonia - HCl case. After the equivalence point it is like the
end of the ethanoic acid - NaOH curve.

Notice that there isn't any steep bit on this graph. Instead, there is just what is known as
a "point of inflexion". That lack of a steep bit means that it is difficult to do a titration
of a weak acid against a weak base.
 Note: for equilibrium chemical equation at equivalence point (# of

moles of acid=# of moles of base), # 𝒐𝒇 𝒎𝒐𝒍𝒆𝒔 = 𝑪 ∗ 𝑽
 Example 1
Evaluate [H+] and pH in the titration of 10.0 mL 1.0 M HCl solution with 1.0 M
NaOH solution, and plot the titration curve.
Solution
𝑇ℎ𝑒 𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑎𝑐𝑖𝑑 𝑝𝑟𝑒𝑠𝑒𝑛𝑡 = 𝑉𝑎 ∗ 𝐶𝑎
= 10.0 mL * 1.0 mol/1000 mL
= 10 mmol (mili-mole)
𝑇ℎ𝑒 𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑏𝑎𝑠𝑒 𝑁𝑎𝑂𝐻 𝑎𝑑𝑑𝑒𝑑 = 𝑉𝑏 ∗ 𝐶𝑏
𝑇ℎ𝑒 𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑎𝑐𝑖𝑑 𝑙𝑒𝑓𝑡 = 𝑉𝑎 ∗ 𝐶𝑎 − 𝑉𝑏 ∗ 𝐶𝑏
- 𝑇ℎ𝑒 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑎𝑐𝑖𝑑 𝑎𝑛𝑑 𝑡ℎ𝑢𝑠 [𝐻+] =

[𝑉𝑎 ∗ 𝐶𝑎 − 𝑉𝑏 ∗ 𝐶𝑏]
(𝑉𝑎 + 𝑉𝑏)
- 𝑝𝐻 = −𝑙𝑜𝑔 [𝐻+]
𝑎𝑓𝑡𝑒𝑟 𝑒𝑞. 𝑝𝑜𝑖𝑛𝑡 𝑖𝑛 𝑡ℎ𝑖𝑠 𝑐𝑎𝑠𝑒, 𝑇ℎ𝑒 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑏𝑎𝑠𝑒 𝑎𝑛𝑑 𝑡ℎ𝑢𝑠 [𝑂𝐻 −] =
[𝑉𝑏 ∗ 𝐶𝑏 − 𝑉𝑎 ∗ 𝐶𝑎]

- 𝑝𝑂𝐻 = −𝑙𝑜𝑔 [𝑂𝐻−]
- 𝑝𝐻 + 𝑝𝑂𝐻 = 14
With the above formulation, we can built a table for various values as shown.
Base added [H+] pH

0 1.0 0.0
1.0 9/11 0.087
2.0 8/12 0.176
5.0 5/15 0.477
Half-equivalent point
8.0 2/18 0.954
9.0 1/19 1.279
9.3 0.7/19.3 1.440
9.5 0.5/19.5 1.591
9.7 0.3/19.7 1.817
9.8 0.2/19.8 2.0
9.9 0.1/19.9 2.300
9.95 0.05/19.95 2.60
10 H2O=H++OH- pH = 7
NaCl neutral salt
Base [OH-] pH
added
10.05 0.05/20.05 11.397
10.10 0.5/20.1 11.697
11.0 1/21 12.678
15.0 5/25 13.301
20.0 20/30 13.924

Note: before conducting the experiment, it can predicate at any volume of
base the equivalence point will occur. Using this principle
# of moles of acid=# of moles of base
• Apparatus and solutions
- Burette with stand
- Pipette
- Conical flask
- Beakers
- Measuring cylinders
- Wash bottles
- Magnetic stirrer
- 0.01M HCL
- 0.01M NaOH
- Phenolphthalein indictor

• Procedure
1. Pipette out volume of acid (known concentration) in conical flask using
pipette and pipette wheel.
2. Add 2-3 drops of phenolphthalein indictor ( the solution will be colorless)
3. Fill the burette with base (known concentration).
4. Open the burette to run base to acid slowly (run base with certain volume for
each trail to calculate pH for the solution) (titrate acid with base)
5. When the color of solution chances from colorless to light pink close the
burette (this is the equivalence point).
6. Record this point (volume of change color) and compare it with calculation.
7. Open again the burette to run base to acid to obtain dark pink color (this is the
end point). (continue the titration)
8. Draw pH curve for the reaction and determine end and equivalence points.

Determination of Water Alkalinity

Experiment #5: Determination of Alkalinity of Water
• Introduction& principle
Alkalinity is defined as a measure of the buffering capacity of water to neutralize strong acid. This
capacity is attributed to bases that are present in natural waters including OH-, HCO3-, and CO32-.
More alkalinity in your water sample means more buffering capacity of your water sample. In order to
determine Alkalinity of samples, samples will be titrated with sulfuric acid or hydrochloric acid to a
certain pH end point (pH 8.3 for Phenolphthalein Alkalinity and pH 4.5 for Total Alkalinity), and the
volume of the acid used for the titration will be recorded.
The following reactions are occurring during titration;

pH range above 8.3
OH- + H+ → H2O
CO32- + H+ → HCO3-
pH range between 8.3 and 4.5
HCO3- + H+ → H2CO3
For samples whose initial pH is above 8.3, the titration is conducted in two steps. In the
first step, the titration is conducted until the pH is lowered to 8.2, the point at which
phenolphthalein indicator turns from pink to colorless. This value corresponds to the
points for conversion of carbonate to bicarbonate ion. The second phase of titration is
conducted until the pH is lowered to 4.5, corresponds to mixed indictor end point, which
corresponds to the equivalence points for the conversion of bicarbonate ion to carbonic
acid as shown in the figure below.

Phenolphthalein alkalinity and total alkalinity can be measured as follows
𝑉 ∗𝑁 ∗50∗1000
- Phenolphthalein alkalinity as mg/L CaCO3 = 𝑉𝑎𝑐𝑖𝑑 𝑎𝑐𝑖𝑑
𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 𝑠𝑎𝑚𝑝𝑙𝑒
𝑉𝑎𝑐𝑖𝑑 = 𝑃 → 𝑖𝑛 𝑓𝑖𝑟𝑠𝑡 𝑠𝑡𝑎𝑔𝑒
𝑉𝑎𝑐𝑖𝑑 ∗𝑁𝑎𝑐𝑖𝑑 ∗50∗1000

- Total alkalinity as mg/L CaCO3 = 𝑉 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
𝑉𝑎𝑐𝑖𝑑 = 𝑇 → 𝑖𝑛 𝑡𝑤𝑜 𝑠𝑡𝑎𝑔𝑒𝑠
Different types of alkalinities present in the samples can be calculated using the
equations given in the following table. This table is available for volume of water
sample (100ml).
Values of P and T Hydroxide alkalinity Carbonate alkalinity Bicarbonate alkalinity

𝑃 = 0 0 0 T *10
𝑃 < 𝑇/2 0 2P*10 (T-2P) *10
𝑃 = 𝑇/2 0 T*10 0
𝑃 > 𝑇/2 (2P-T) *10 2(T-P) * 10 0
𝑃=𝑇 P*10 0 0
For any volume of sample, the following table can be used
Values of P and T Hydroxide alkalinity Carbonate alkalinity Bicarbonate alkalinity

𝑃 = 0 𝑇 ∗1000
0 0 or Total Alk.
𝑉𝑠
𝑃 < 𝑇/2
(𝑇−2𝑃) ∗1000
2𝑃∗1000 or
0 or 2*Phenolp.alk. 𝑉𝑠
𝑉𝑠
Total alk. -2*Phenolp.alk.
𝑃 = 𝑇/2 0
𝑇 ∗1000
or Total Alk. 0
𝑉𝑠
𝑃 > 𝑇/2 (2𝑃−𝑇) ∗1000 2(𝑇−𝑃) ∗ 1000
or or
𝑉𝑠 𝑉𝑠 0
2*Phenolp.alk- Total alk. 2( Total alk. -Phenolp.alk)
𝑃∗1000
𝑃=𝑇 or = Total alk. or
𝑉𝑠 0 0
Phenolp.alk.
Alkalinity is significant in many uses and treatments of natural waters and wastewaters.
As alkalinity of many surface waters constitute of carbonates, bicarbonate and
hydroxide contents, it is assumed to be an indicator of these constituents as well.
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.
• Aim
The main purpose of this experiment is to measure phenolphthalein alkalinity and total
alkalinity in water samples and to calculate different types of alkalinity (hydroxide, carbonate
and bicarbonate alkalinity). In addition, this experiment aims to study effects of alkalinity in
water in order to understand the significant it in the environment.
• Apparatus and chemicals

- Burette with burette stand, Pipette and pipette wheels, Conical flask (250 ml),
- Measuring cylinder (250 ml), Wash bottle, Beaker
- Standard sulpharic acid, Distilled water, Phenolphthalein indictor, Methyl red,
Methyl alcohol, Bromocresol green indictor

• Procedure
1. Pipette out volume of the field water sample in conical flask.
2. Add 2-3 drops of phenolphthalein indictor into water sample (the color changes
to pink).
3. Fill the burette with sulphuric acid (H2SO4).
4. Titrate the water sample with sulphuric acid.
5. Continue the titration till the color changes to colorless.
6. Record volume of sulphuric acid (v1=P)
7. Add 2-3 drops of mixed indictor (the color changes to blue) and continue the
titration with sulphuric acid.
8. Continue the titration till the color changes to red.
9. Record volume of sulphuric acid (v2) (T= v1 + v2)
10. Calculate different types of alkalinity.

Determination of Water Hardness

Experiment #6: Determination of Hardness
• Introduction &Principle
Originally, the hardness of water was understood to be a measure of the capacity of water for
precipitating soap. Soap is precipitated chiefly by the calcium and magnesium ions commonly
present in water, but may also be precipitated by ions of other polyvalent metals, such as
aluminium, iron, manganese, strontium and zinc, and by hydrogen ions. Because, all but the
first two are usually present in insignificant concentrations in natural waters, hardness is
defined as a characteristic of water, which represents the total concentration of just the
calcium and the magnesium ions expressed as calcium carbonate. However, if present in
significant amounts, other hardness producing metallic ions should be included. When the
hardness is numerically greater than the sum of the carbonate alkalinity and the bicarbonate
alkalinity, the amount of hardness, which is equivalent to the total alkalinity, is called
carbonate hardness; the amount of hardness in excess of this is called non-carbonate
hardness. When the hardness is numerically equal to or less than the sum of carbonate and
bicarbonate alkalinity all of the hardness is carbonate hardness and there is no noncarbonated
hardness. The hardness may range from zero to hundreds of milligrams per litre in terms of
calcium carbonate, depending on the source and treatment to which the water has been
subjected. Ethylenediamine tetra-acetic acid and its sodium salts (EDTA) form a chelated
soluble complex when added to a solution of certain metal cations. If a small amount of a dye
such as Eriochrome black T is added to an aqueous solution containing calcium and
magnesium ions at a pH of 10 ± 0.1, the solution will become wine red (violet). If EDTA is
then added as a titrant, the calcium and magnesium will be complexed. After sufficient EDTA
has been added to complex all the magnesium and calcium, the solution will turn from wine
red to blue. This is the end point of the titration.
𝑉𝐸𝐷𝑇𝐴 ∗𝑁𝐸𝐷𝑇𝐴 ∗50∗1000
- Total hardness as (Unboiling) mg/L CaCO3 = 𝑉 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 𝑠𝑎𝑚𝑝𝑙𝑒
𝑉𝐸𝐷𝑇𝐴 ∗𝑁𝐸𝐷𝑇𝐴 ∗50∗1000

- Permanent hardness (Boiling) as mg/L CaCO3 = 𝑉 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 𝑠𝑎𝑚𝑝𝑙𝑒
- Temporary hardness = Total hardness – Permanent hardness
• Aim
To determine the total hardness of the given samples by EDTA titrimetric method

• Apparatus and Reagents
✓ Burette
✓ Pipette, pipette wheel
✓ measuring cylinder, beakers
✓ conical flask, bottles
✓ heating source
✓ Standard EDTA titrant (0.01 M)
✓ Eriochrome black T indicator
✓ Ammonia buffer solution

• Procedure
1. Pipette out volume of the field water sample in conical flask.
2. Add 2-3 drops of EBT indictor into water sample (the color changes to wine red
"violet").
3. Fill the burette with EDTA.
4. Titrate the water sample with EDTA.
5. Continue the titration till the color changes to dark blue.
6. Record volume of EDTA.
7. Calculate the total hardness.
8. For permanent hardness, use boiling water sample and redo steps 1-7

pH, Turbidity and Electrical
Conductivity (EC)

Experiment #7: pH, Turbidity and Electrical Conductivity (EC)
❖ Part #1 (PH)
pH value of water indicates the hydrogen ion concentration in water and concept of pH was
put forward by Sorenson (1909). pH is expressed as the logarithm of the reciprocal of the
hydrogen ion concentration in moles/ litre at a given temperature. The pH scale extends
from 0 (very acidic) to 14 (very alkaline) with 7 corresponding to exact neutrality at 25°C.
pH is used in the calculation of carbonate, and bicarbonate, corrosion and stability index
etc. While the alkalinity or acidity measures the total resistance to the pH change or
buffering capacity, the pH gives the hydrogen ion activity. pH can be measured
colorimetrically or electrometrically. Colorimetric method is used only for rough
estimation. It can be done either by using universal indicator or by using pH paper. The
hydrogen electrode is the absolute standard for the measurement of pH. They range from
portable battery operated units to highly precise instruments.
• Aim
To determine the pH of given samples using digital pH meter.
• Apparatus
- pH meter
- Buffer solutions of pH (4.0,7.0, 10.0)
- Bottle whish
- Beakers
- Solution samples

• Procedure
1. Switch on the pH meter
2. Prepare the buffer solution 4.0, 7.0 and 10.0
3. Calibrate the pH meter to 10.0 using the buffer solution and by adjusting the calibration
knob.
knob.
knob.
6. Read the pH meter by inserting the sample.

❖ Part #2 (Turbidity)
The method presented below is based on a comparison of the intensity of light scattered
by the sample in specific conditions with the intensity of light scattered by standard
reference suspension under the same condition. The higher the intensity of scattered
lights, higher the turbidity. Formazine polymer, which has gained acceptance as the
turbidity standard reference suspension is used as a reference turbidity standard
suspension for water. It is easy to prepare and is more reproducible in its lights
scattering properties than the clay or turbid natural water standards previously used.
The turbidity of a given concentration of formazine has an approximate turbidity of 100
NTU, when measured on candle turbidity meter. Nephelometric turbidity units based
on formazine preparation will have approximate units derived from Jackson candle
turbidimeter but will not be identical to them.
• Aim
To determine the turbidity of the given samples using Nephelometer in NTU.

• Apparatus
Nephelometer (turbidity meter) with accessories
• Procedure
1. Switch on the turbidity meter.
2. Calibrate the turbidity meter using 0.02, 10, and 1000 NTU standard
solution.
3. Read the turbidity meter by inserting the sample.

❖ Part #3 (Electrical Conductivity EC)
• Introduction and Principle
Conductivity is a measure of the ability of water to pass an electrical current. Conductivity in

water is affected by the presence of inorganic dissolved solids such as chloride, nitrate, sulfate,
and phosphate anions (ions that carry a negative charge) or sodium, magnesium, calcium, iron,
and aluminum cations (ions that carry a positive charge). Organic compounds like oil, phenol,
alcohol, and sugar do not conduct electrical current very well and therefore have a low
conductivity when in water. Conductivity is also affected by temperature: the warmer the water,
the higher the conductivity. For this reason, conductivity is reported as conductivity at 25
degrees Celsius (25 C). The basic unit of measurement of conductivity is the mho or siemens.
Conductivity is measured in micromhos per centimeter (μmhos/cm) or microsiemens per
centimeter (μs/cm). Distilled water has a conductivity in the range of 0.5 to 3 μmhos/cm.
• Aim
To determine the electrical conductivity of the given water samples using conductivity meter
in µs/cm
• Apparatus
Conductivity meter with accessories
• Procedure
1. Switch on the conductivity meter.
2. Prepare 0.1N potassium chloride standard solution (KCl)
3. Calibrate the conductivity meter using the standard solution and by adjusting the
calibration knob.
4. Read the conductivity meter by inserting the sample

Jar Test for Determining Optimum Coagulant Dosage

Experiment #8: Jar Test for Determining Optimum Coagulant Dosage
Coagulation and flocculation are important unit processes in water and wastewater
treatment plants. The purpose of coagulation/flocculation is to remove suspended
matter, turbidity, color, micro organisms, and odor producing substances. Coagulation
involves the addition of chemicals to destabilize [allow them to agglome rate] the
suspended particles, colloidal materials, and macromolecules. Some common
coagulants used are aluminum sulfate (alum) and ferric sulfate. Flocculation is usually
defined as the aggregation of destabilized particles into larger flocs under slow mixing
conditions. The flocs formed are subsequently removed by sedimentation and/or
filtration.
Coagulants are used in water treatment plants

(i) to remove natural suspended and colloidal matter,
(ii) to remove material which do not settle in plain sedimentation, and
(iii) to assist in filtration.
Alum [Al2(SO4)3. 18H2O] is the most widely used coagulant. When alum solution is
added to water, the molecules dissociate to yield SO- and Al . The +ve species combine
2
4
3+
with negatively charged colloidal to neutralize part of the charge on the colloidal
particle. Thus, agglomeration takes place. Coagulation is a quite complex phenomenon
and the coagulant should be distributed uniformly throughout the solution. A flash mix
accomplishes this. Jar test is simple device used to determine this optimum coagulant
dose required.

The jar test, device consists of a number of stirrers (4 to 6) provided with paddles. The
paddles can be rotated with varying speed with the help of a motor and regulator.
Samples will be taken in jars or beakers and varying dose of coagulant will be added
simultaneously to all the jars. The paddles will be rotated at 250 rpm for 2-3 minutes
and at 25 rpm for 20 to 30 minutes, corresponding to the flash mixing and slow mixing
in the flocculator of the treatment plant. After 30 minutes settling, supernatant will be
taken carefully from all the jars to measure turbidity. The dose, which gives the least
turbidity, is taken as the optimum coagulant dose.
• Aim
To determine the optimum coagulant dosage for clarifying the given sample of water
by using alum as the coagulant and performing the jar test experiment.
• Apparatus
1. Jar test apparatus
2. Glass beakers
3. Pipette
4. Nephelometer (turbidity meter)
• Reagents
1. Alum solution (1mL containing 10 mg of alum)

• Procedure
1. Take (6) 1-litre beakers and fill them with sample up to the mark.
2. Keep each beaker below each paddle and lower the paddles, such that each one
is about 1cm above the bottom.
3. Pipette different dosage of the alum solution into the test samples.
4. Immediately run the paddles at 250 rpm for 2-3 minute.
5. Reduce the speed to 25 rpm and run at this rate for 20-30 minutes.
6. Stop the machine, lift out the paddles and allow settling for 30 minutes.
7. Find the residual turbidity of the supernatant using nephelometer.
8. Plot a graph with alum dosage along x-axis and turbidity along y-axis.
9. Plot a graph with alum dosage along x-axis and percentage removal along y-
axis
10. The dosage of alum, which represents least turbidity and maximum percentage
removal, gives Optimum Coagulant Dosage (O.C.D.).
11. Repeat steps 1–10 with higher dose of alum, if necessary

BOD5 Test

Experiment #9: BOD5 Test
 Definition and principle
BOD: is a measure of the amount of O2 consumed by bacteria for the oxidation of the
organic matter (OM)
OM+Microorg+O2+ nutrients...........CO2 +H2O+stable compounds
• The higher the amount of OM in water the higher the BOD value
• Various methods for BOD analysis are exist but the principle is the same.
• A volume of water sample is put in a recipient where the changes in the DO
content are measured before and after incubation at 20oc for a certain time
• if the sample is expected to have a low content of microorganisms, an inoculum
should be added
• Moreover, an extra nutrient solution may be added to ensure that the growth of
microorganisms is not limited
BOD value increase over time as OM is progressively biodegraded. However, after

5 days the majority of the OM contained in the sample has already been degraded
For that reason ...the BOD5, which is measured after 5 days of incubation,
is the most widely used method . On the other hand, if the aim is to measure the
total content of biodegradable OM ...BOD21 is measured after 21 days of incubation.
The oxidation of other compounds present in the water sample can also contribute
to the consumption of DO....

In particular , Nitrification could interfere in the measurement of BOD leading to
an overestimate of its value .... To prevent this, the use of nitrification inhibitor is
required
BOD5: Total amount of O2 consumed by microorganisms during first 5 days of

biodegradation
- Water sample in standard bottle (300 mL)

NOTE 1: Light must be kept out of the bottle! Why?
To keep algae from adding O2 by photosynthesis
NOTE 2: since O2 demand of typical wastewater is several hundred
mg/L and the saturation value ≈9.1 mg/L, it is necessary to dilute the
sample to keep final DO > 0.0
(if DO=0.0 before 5 days, the test is invalid)
- Measure DO at the beginning and after 5 days
DO i
− DO f
BOD 5
=
P
Volume .. of .. wastewater Volume .. of .. wastewater

P = =
Volume .. of . wastewater + dilution ... water 300 ml
• Example
10 mL sample of sewage mixed with enough water to fill 300 ml bottles has an DOi =
9 mg/L. To help assure an accurate test, it is desirable to have at least 2 mg/L drop in

DO during the 5 day run, and the final DO should be at least 2 mg/L. For what range of
BOD5 would this dilution produces the desired results?
Solution:
P = 10/300 to get at least 2 mg/L drop in DO
The minimum BOD5 need to be
DO i
− DO f 2
BOD 5
 = = 60 mg / L
P 10 / 300
9 − 2
BOD 5
 = 210 mg / L
10 / 300
So, the range should be 60-210 mg/L
NOTE: It is better to dilute the sample with water having microorganisms (not pure
water). Why?
To assure that there is an adequate bacterial population to carry out the

biodegradation. So, both waters have BOD
• BOD Modeling:
dL t
= − K d Lt
dt
− Kdt
Lt = L0e
Lt: amount of O2 demand left after time
Kd: BOD reaction rate constant (1/time)
L0: ultimate carbonaceous O2 demand (total amount of O2 required by

microorganisms to oxidize the carbonaceous portion of the waste to
simple CO2 and H2O
L 0 = BOD t
+ Lt
It is the sum of amount of O2 already consumed in the first t days + amount of O2
remaining to be consumed after time t.

BOD t

= L0 1 − e
−Kdt

Text book Example:
Steps:
1) First 3 bottles for initial DO
2) Calculate BOD for each bottle
3) Average BOD values = 360 mg/L
4) Use bottles 10-17 for k determination
5) Determine BOD for each bottle as above
1/3
 time 
6) plot time vs .  
 BOD 
7) Use best fit and calculate K as
B
kd = 2 . 61
A
K:rate constant (1/day)
A: intercept
B : slope

• Aim
To find the biochemical oxygen demand (BOD) at 5 days for waste water sample
• Apparatus and tools
- Dissolved oxygen meter.
- Standard 300 ml dark bottles.
- Laboratory incubator.
- Pipette and pipette wheel.
- Wastewater samples.

Data Sheets
"Determination of Solids in Water Samples"
Date Tasted:
Tested by:
Group Number:
Sample Number:
Sample Description:
❖ Part 1 (Total, Volatile, & Fixed Solids)
Description Sample #1 Sample #2 Sample #3
Initial weight of crucible

(W1) g
Weight of crucible @103-105 Co
(W2) g
Weight of crucible @550 Co
(W3) g
Volume of sample
(V) ml
✓ Sample Calculations
𝑊2 −𝑊1
Total Solid (TS) (mg/mL) = 𝑉
• Sample #1
• Sample #2
• Sample #3
𝑊2 −𝑊3
Total Volatile Solid (TVS) (organic matter) (mg/mL) = 𝑉
• Sample #1
• Sample #2
• Sample #3
𝑊3 −𝑊1
Total Fixed Solid (TFS) (inorganic matter) (mg/mL) =
𝑉
• Sample #1
• Sample #2
• Sample #3
❖ Part #2 (Total Suspended & Total Dissolved Solids)
Description Sample #1 Sample #2 Sample #3
Initial weight of evaporating dish

(W1) g
Final weight of evaporating dish
@103-105 Co
(W2) g
Initial weight of filter paper
(W1) g
Final weight of filter paper
@103-105 Co
(W2) g
Volume of sample
(V) ml
✓ Sample Calculations
𝑊2 −𝑊1
Total Suspended Solid (TSS) (filter paper) (mg/mL) = 𝑉
• Sample #1
• Sample #2
• Sample #3
𝑊2 −𝑊1
Total Dissolved Solid (TDS) (mg/mL) (evaporating dish) = 𝑉
• Sample #1
• Sample #2
• Sample #3
 Questions
1. What is the meaning of solids in water and wastewater? (Main classifications of
solids)
2. What are typical TS, TSS and TDS values of water and wastewater in Jordan?
Compare these values with your results in experiment?
3. What are the main sources of TS, TSS and TDS in surface water, ground water
and wastewater?
4. Explain the significance of determination of total solids in sanitary engineering?
5. Water can be classified by the amount of TDS into three types, mention them?
6. Explain that "ground water usually has higher total dissolved solids and surface
water has higher suspended solids"?

"Beer’s law and Spectrophotometric analysis"
Date Tasted:
Tested by:
Group Number:
Sample Number:
Sample Description:
❖ Table
V of CuSO4 V of
Tube # V of H2O (ml) solution C A
(ml)
1
2
3
4
5
6
❖ Sample calculations
- Mass of CuSO4 to prepare 0.4M in 25 ml
𝑔 𝑔 𝑔
✓ (molar mass for atoms are Cu (63.5 ) , O (16 ), S (32 )
𝑚𝑜𝑙 𝑚𝑜𝑙 𝑚𝑜𝑙
- Concentrations ( 𝑀1 𝑉1 = 𝑀2 𝑉2 )
Tube #1:
Tube #2:
Tube #3:
Tube #4:
Tube #5
Tube #6:
❖ Plot concentration vs. absorption

❖ Find beer's law equation (using standard curve of copper sulphate)
❖ Find concentration of copper in unknown sample of water (in mol/L)
 Questions
1. What is the definition of Beer's law? What is the importance of Beer's Law?
2. What is the relationship between absorbance (A) and transmittance (T)?
3. What are the main reasons of error in this experiment?
4. How does the percent of transmittance and absorbance of a solution vary (differ)
with (a) increasing concentration and (b) increasing path length?
"Acid-Base titration"
Date Tasted:
Tested by:
Group Number:
Sample Number:
Sample Description:
Burette reading V of
pH
SI. NO Initial Final NaOH [H+]
calculated
in ml
1
2
3
4
5
6
7
8
9
10
11
❖ Calculations
Calculate [H+] and pH in the titration of volume (mL) of 0.01 M HCl solution with
0.01 M NaOH solution, and plot the titration curve (identify equivalence and end
points)
By using the following equations:
- 𝑇ℎ𝑒 𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑎𝑐𝑖𝑑 𝑝𝑟𝑒𝑠𝑒𝑛𝑡 = 𝑉𝑎 ∗ 𝐶𝑎

- 𝑇ℎ𝑒 𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑏𝑎𝑠𝑒 𝑁𝑎𝑂𝐻 𝑎𝑑𝑑𝑒𝑑 = 𝑉𝑏 ∗ 𝐶𝑏
[𝑉𝑎∗𝐶𝑎 − 𝑉𝑏∗𝐶𝑏]
- 𝑇ℎ𝑒 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑎𝑐𝑖𝑑 𝑎𝑛𝑑 𝑡ℎ𝑢𝑠 [𝐻+] =
- 𝑝𝐻 = −𝑙𝑜𝑔 [𝐻+]
- 𝑝𝐻 + 𝑝𝑂𝐻 = 14
❖ Calculations
❖ Titration curve
 Questions
1. Define acid and base in Arrhenius terms?
2. What is an Acid-Base Titration? What are types of titrations?
3. How can prepare 0.01M of HCL and 0.01M of NaOH?
4. Identify the main cusses of error in this experiment?
5. Discuss the different types of pH indicators and what was happening as

they changed color. Why phenolphthalein indictor was used in this
experiment.
6. Use a chemical encyclopedia to write the difference between the indicator

endpoint for a titration and the equivalence point of the titration.
Determination of Water Alkalinity
Date Tasted:
Tested by:
Group Number:
Sample Number:
Sample Description:
❖ Table #1 (phenolphthalein alkalinity)

Burette reading (ml) Volume of
Volume of water
Trial # Initial Final sulphuric acid
sample (ml)
(ml)
1
2
3
 Calculations
- Concordant value=
- Phenolphthalein alkalinity (P) as mg/L CaCO3 =
❖ Table #2 (Total alkalinity)

Burette reading (ml) Volume of
Volume of water
Trial # Initial Final sulphuric acid
sample (ml)
(ml)
1
2
3
 Calculations
- Concordant value=
- Total alkalinity (T) as mg/L CaCO3 =

- Calculate hydroxide, carbonate and bicarbonate alkalinity according to your
results above
1. Hydroxide alkalinity [OH-]
2. Carbonate alkalinity [CO3-2]
3. Bicarbonate alkalinity[HCO3-1]
 Questions
1. What is alkalinity of water? How is it founded? what are the major forms of
alkalinity?
2. What is the significant for determining alkalinity of water (applications of
alkalinity measurement)?
3. What are the ions determined by phenolphthalein? What are the ions
determined by mixed indictor?
4. How hydroxyl ions are neutralized?
5. Can OH- CO3-2 and HCO3-1 can exist together?
6. Why alkalinity is measured in terms of CaCO3 Eq.?
7. What are the ranges of alkalinity for fresh and portable water? Compare
these ranges with your results in laboratory

Determination of Water Hardness
Date Tasted:
Tested by:
Group Number:
Sample Number:
Sample Description:
❖ Table #1 (Total Hardness (Unboiling)

Volume of water Burette reading (ml) Volume
Trial #
sample (ml) Initial Final EDTA (ml)
1
2
3
 Calculations
- Concordant value=
- Total Hardness as mg/L CaCO3 =
❖ Table #2 (Permanent Hardness (boiling)

Volume of water Burette reading (ml) Volume
Trial #
sample (ml) Initial Final EDTA (ml)
1
2
3
 Calculations
- Concordant value=
- Permeant Hardness as mg/L CaCO3 =
- Temporary hardness
 Questions
1. What is the definition of hardness? How will you classify water in terms of
degree of hardness (classification of hardness)? Compare your results with
hardness classification?
2. Explain the significance of determination of hardness of water in

environmental engineering
3. How can you remove permanent and temporary hardness from water?
pH, Turbidity and Electrical Conductivity (EC)
Date Tasted:
Tested by:
Group Number:
❖ Part #1 (pH)
pH
Sample #
pH meter pH paper
1
2
3
4
❖ Part #2 (Turbidity)
Average
Sample # Reading #1 Reading #2 Reading #3
(NTU)
1
2
3
❖ Part #3 (Electrical Conductivity)
EC TDS Temperature f
Sample #
(µs/cm) (mg/l) (C)
1
2
3
4
5
Average =
 Questions
1. Discuss the relationship between (a) pH and hydrogen ion concentration (b) pH
and hydroxide ion concentration?
2. Why is it necessary to maintain the pH of water nearly 7?
3. What is a buffer solution? Give examples.
4. Discuss the significance of determination of turbidity in sanitary engineering?
5. What is the standard unit of turbidity?
6. Determine the main factors that affect the value of conductivity?

"Jar Test for Determining Optimum Coagulant Dosage"
Date Tasted:
Tested by:
Group Number:
Beaker # Alum dose in mg/l Turbidity in NTU Percentage removal %
- Initial turbidity of the sample =---------- NTU

- Optimum coagulant dosage = ..........mg/l
Turbidityi − Turbidity2
- Percentage removal = × 100%
𝑡𝑢𝑟𝑏𝑖𝑑𝑖𝑡𝑦𝑖
- Plot a graph with alum dosage along x-axis and turbidity along y-axis
- Plot a graph with alum dosage along x-axis and percentage removal along y-
axis
 Questions
1. Why is alum preferred to other coagulants?
2. What is the difference between coagulation and flocculation?
3.What are the potential sources of error in the experiment|?
4.Are there alternative methods for determining the optimum does of coagulant? If so,
how do they compare to this method?
5. What are the potential human health and environmental effect of excess coagulant
dosage?
"BOD5 Test"
Date Tasted:
Tested by:
Group Number:
Sample Description:
Incubation Calculated
Wastewater Initial DO Final DO DO drop
Bottle # period BOD
portion (ml) (mg/l) (mg/l) (mg/l)
(days) (mg/l)
1
2
3
Average initial DO=
4
5
6
7
8
9
Average BOD5=
BOD analysis to predict k-rate
10
11
12
13
14
15
16
17
- The initial DO =------------ mg/l
- BOD5 = ---------- mg/l
- Lo(BODu)= ------------- mg/l
 Plot (time/BOD)1/3 vs. time to find k-rate

 Questions:
1. What use is made of the B.O.D. test in water pollution control?
2. List the main requirements, which must be completed with, in order to obtain
reliable B.O.D. data.
3. List the requirements of satisfactory dilution water for B.O.D. test.
4. What is the method that can be used to control nitrification in the period that is
more 5 days of B.O.D. test at 20°C?
5. What are the factors affecting the rate of biochemical oxidation in the B.O.D.
test?
The End

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"Yarmouk University"

"Hijjawi Faculty for Engineering Technology"

Introduction for preparing solutions 9

Solids determination and gravimetric analysis 14

Beer’s law and spectrophotometric analysis 21

Titration skills and acid / base chemical analyses 26

Determination of water alkalinity 36

pH, Turbidity and Electrical Conductivity (EC) 45

Jar Test and Modeling of the coagulation-flocculation process 50

Determination of 5-day BOD of wastewater samples 54

Prepared by Eng. Elham G.Al-Hamaideh 1

❖ Textbooks and Readings:

Water quality LAB Manual, assembled by Shahalam

1. Basic orientation on safety measures in the sanitary engineering LAB.

2. Solids determination and gravimetric analysis.

3. Beer’s law and spectrophotometric analysis as.

4. Titration skills and acid / base chemical analyses.

5. Determination of water alkalinity.

6. Determination of water hardness.

Prepared by Eng. Elham G.Al-Hamaideh 2

8. Jar Test and Modeling of the coagulation-flocculation process

9. Determination of 5-day BOD in influent and effluent of wastewater treatment plants

Prepared by Eng. Elham G.Al-Hamaideh 3

Basic orientation on safety measures in the sanitary

Solids determination and gravimetric analysis 1 Lab Session

Beer’s law and spectrophotometric analysis 1 Lab Session

Titration skills and acid / base chemical analyses 1 Lab Session

Determination of water alkalinity 1 Lab Session

Determination of water hardness 1 Lab Session

Determination of pH, Turbidity, EC and for different

Jar Test and Modeling of the coagulation-flocculation

Determination of 5-day BOD in influent and effluent of

Prepared by Eng. Elham G.Al-Hamaideh 4

Prepared by Eng. Elham G.Al-Hamaideh 5

Prepared by Eng. Elham G.Al-Hamaideh 6

Prepared by Eng. Elham G.Al-Hamaideh 7

Prepared by Eng. Elham G.Al-Hamaideh 8

Prepared by Eng. Elham G.Al-Hamaideh 9

• Solute - The substance which dissolves in a solution

commonly used. Some of these are listed below.

𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 (𝑚𝑜𝑙𝑒𝑠)

What is the molarity when 0.75 mol is dissolved in 2.50 L of solution?

Calculate the molarity of 25.0 grams of KBr dissolved in 750.0 mL.

𝑚𝑎𝑠𝑠 (𝑔) 25 (𝑔)

Prepared by Eng. Elham G.Al-Hamaideh 10

𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 (𝑚𝑜𝑙𝑒𝑠)

𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 (𝑚𝑜𝑙𝑒𝑠)

𝑚𝑎𝑠𝑠 (𝑔) 𝑔 𝑚𝑎𝑠𝑠

80.0 grams of glucose (C6H12O6, mol. wt = 180. g/mol) is dissolved in1.00 kg of

Prepared by Eng. Elham G.Al-Hamaideh 11

Another similar way of expressing the concentration of a solution is to express it in weight

Prepared by Eng. Elham G.Al-Hamaideh 12

𝑚𝑜𝑙𝑒𝑠 𝑠𝑜𝑙𝑢𝑡𝑒 𝑏𝑒𝑓𝑜𝑟𝑒 𝑑𝑖𝑙𝑢𝑡𝑖𝑜𝑛 = 𝑚𝑜𝑙𝑒𝑠 𝑠𝑜𝑙𝑢𝑡𝑒 𝑎𝑓𝑡𝑒𝑟 𝑑𝑖𝑙𝑢𝑡𝑖𝑜𝑛

Using the dilution equation,:

(1.50 𝑚𝑜𝑙/𝐿) (53.4 𝑚𝐿) = (0.800 𝑚𝑜𝑙/𝐿) (𝑥)

Prepared by Eng. Elham G.Al-Hamaideh 13

Prepared by Eng. Elham G.Al-Hamaideh 14

• Introduction & principle

Prepared by Eng. Elham G.Al-Hamaideh 15

Prepared by Eng. Elham G.Al-Hamaideh 16

Prepared by Eng. Elham G.Al-Hamaideh 17

Prepared by Eng. Elham G.Al-Hamaideh 18

Prepared by Eng. Elham G.Al-Hamaideh 19