Al- Balqa' Applied University

Civil Engineering Department

Sanitary Engineering Lab.

Eng.Iman Alshaer
 Table of contents

Introduction ……………………………………………………………………….. 1

EXP.1: Sampling and Physical Measurements..………………..….......................... 5

EXP.2: Odor Test ...…………………………………………….…......................... 8

EXP.3: Solids Determination Test …………………..…………………………….. 10

EXP.4: Turbidity Test ……………………………………..…………………...…. 14

EXP.5: Coagulation Test (Jar Test) ………………………………..………………. 17

EXP.6: Hardness Test ……………………………………………………..…….… 19

EXP.7: Alkalinity Determination Test …………………………………………….. 22

EXP.8: Dissolved Oxygen Determination Test ……………………………...……. 25

EXP.9: BOD Test ………………………………………….……………………… 28

EXP.10: COD Test ………………………………………….…………………….. 32

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Introduction

Water, the natural compound of the one oxygen and two hydrogen atoms, is the compound
that is mostly being used by humans. Every day Millions of cubic meters are used by
humans in all life aspects including domestic purposes like drinking and cleaning,
recreational activities like swimming, agricultural, and industrial activities such as cooling
processes in energy production plants, food production, etc.

The Environment (water, air and soil) in our blue planet is subjected to pollution due to
natural disasters like earthquakes, volcanoes and floods; however the most hazardous
pollution of the environment occurs due to human activities like:
1- Industry which deteriorates the water (surface and ground) by chemicals and solids.
It is also responsible for the air pollution including acidic rain, gases emission and
the increasing CO2 content in the air. The increasing salinity in the soil is justified
partially due to discharging of industrial solids.
2- Daily domestic activities that generate wastewater which pollutes the water and the
soil. Human excreta may contribute in a health risk due to pathogens transport to
surface and ground water.
3- Agriculture through which many fertilizers destroy the soil natural composition and
increase its salinity. Not only, but also these harmful materials contain chemicals
can penetrate the soil and eventually deteriorate the clean groundwater sources and
can increase the chemicals concentration in the surface water bodies.

Water pollution is defined as the presence of impurities in water in quantities and nature to
make it improper for human use. In order to judge the suitability of water for human use in
terms of the quality, standard tests are required. The tests of water quality are classified into
three main categories:
1- Physical water quality tests, mainly consist of pH and temperature test, color test,
taste and odor test, turbidity test, concentration of solids test.
2- Chemical water quality tests, like dissolved Oxygen, B.O.D test, C.O.D test,
coagulation test, alkalinity test, hardness, CO 2 content, metals content.
3- Biological water quality tests, Pathogen and indicators, MPN, etc.

Referring to the International and Jordanian water standards, the results of these tests should
enable us to take a decision of what to do with the water under question, i.e. to choose the

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most proper and economical way to treat the water. In Jordan, if clean water is used in
efficient way achieving minimum losses and if wastewater is well treated then the water
scarcity problem will be reduced compared to present situations and in that case the clean
groundwater will be saved for the next generations.

Sampling from water and wastewater sources

The objective of the sampling is to collect a portion of the tested water or wastewater small
enough in volume to be conveniently transported and handled in the laboratory while still
accurately represents the water or wastewater being sampled. This implies that, the sample
concentration and components should remain unchanged in comparison to the original
material being sampled, and that the sample must be handled in such way that no
significant changes in the compositions occur before the test is performed.

Sampling techniques

In literature, there are three main techniques of sampling:

1- Grab or catch sampling, which represents the source at that time and place. If the
source is known to have time and place stable compositions, then the sample represents
the source regardless of its time and place.
2- Composite sampling, it refers to the technique where mixture of grab samples are
collected at the same sampling point but at different times. It can be used to observe and
find the average value of the subjected water or wastewater quality.
3- Integrated samples, it refers to a mixture of grab samples collected from different
points simultaneously. Such sampling techniques can be applied to monitor the water
quality in rivers where compositions may vary across the river width or depth.

The question that appears in mind: what sample size and what are the handling
requirements to be considered when sampling is needed. Usually water and wastewater
quality standard tests specified the sample size and the handling requirements and in that
case the randomness in sampling procedure ends. Table 1.1 shows a summary of sampling
and handling requirements for some water and wastewater quality tests.

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Table 1.1: Sampling and handling requirements for some water and wastewater quality tests.
Test Container* Min. sample Handling / storage
size (ML)
Alkalinity P, G(B) 100 24 hrs or refrigerate
BOD P, G (colored) 1000 6 hrs or refrigerate
Analyze as soon as possible or
COD P, G 100
add H2SO4 to pH ≤ 2
Carbon Dioxide P, G 100 Analyze immediately
Color G 500 ---------
Analyze as soon as possible or
NH3 P, G 500 add 0.8 ml conc H2SO4/l or
refrigerate
Analyze as soon as possible or
Odor G 500
refrigerate
Dissolved G, BOD Analyze immediately
300
Oxygen bottle
Turbidity P, G ----- Analyze same day
Solids content G ----- Analyze same day
* P: stands for plastic, G(B) for borosilicate glass, G for glass.

Precautions
There are some precautions to be considered during sampling:
1- Use proper container if the test sample is sensitive to outside conditions.
2- The sample container should be clean, and it is preferable to be rinsed with the
source material before sampling.
3- Make records of time, name and number for every sample using labels.
4- Make sure that the sample well represents the source, for example collect samples
from groundwater wells only after the well has been pumped for sufficient time.
5- For sampling, make sure to avoid the depth and location variation.

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 EXP.1: Sampling and Physical Measurements

This experiment aims at carrying out sampling and taking primary observations of the
color, odor, temperature and pH of water. Sampling technique and the handling of samples
is so sensitive such that mistakes will cause significant changes in the compositions and
may lead to faulty results due to sample deterioration for instance. Thus, care should be
taken of what purpose the sample is being collected and how to handle that sample. It is
important to label samples with primary information like the number and the name of the
sample. In a separate sheet, information of the date, time, place of sample including
location and the name of the person who collects the sample should be filled.

Temperature and pH readings of the sample, as primary measurements, are very important.
For example, the pH measurements are used to calculate the concentration of the alkalinity
forming species, and to determine CO 2 content in the water using mono-graphs, while
temperature is useful to study the saturation and stability of the Calcium Carbonate and
calculate the salinity in water.

Primary physical measurements of water including color, taste and odor give a clue about
the water physical quality recalling that drinking water should be colorless, tasteless and
odorless. The presence or absence of suspended solids can be used as a primary measure of
water quality.

Equipments:

1- Sampling equipment:
Transparent glass beaker of 500 ml.
Stickers for labeling.
Information sheet.

2- Primary measuring equipments:

Thermometer of 0.1 C accuracy with range 0.0 – 45.0C.
pH meter of 0.1 accuracy.

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Procedure:

1- Discuss with your group what sampling technique (grab, composite or integrated
sample) is needed to sample tap water for primary observations of color, odor, pH and
temperature.

2- For tap water sampling, let the tap to discharge water for nearly 1 minute to make sure
of obtaining steady state compositions.

3- Use reagents wherever needed.

4- For tap water, fill the 500ml beaker after rinsing with the same water from source.

5- Label the required data.

6- Take primary physical measurements of temperature and pH. Observe the presence or
absence of other physical quality parameters like the color and odor.

7- Fill the data on the sheet paper provided.

8- Repeat the experiment 5 times.

Data Analysis:

- Mention sampling technique you have used.

- Comment on the sample observations.
- Calculate the average temperature and pH readings.

Discussion

Discuss your results and comment on the accuracy of readings. Discuss the effect of not
following the proper sampling procedure. Discuss the importance of taking primary
measurements, and do you prefer to take instantaneous temperature and pH readings or
after time has passed?

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 AL-AHLIYYA AMMAN UNIVERSITY / SANITARY ENGINEERG LAB.
PRIMARY MEASUREMENTS DATA SHEET

Location:……………….
Test name:………. Date:/ / Sampling point:………..
……………………… Time: Name of person:………..
Sample #
Physical parameter
1 2 3 4 5

Color (Yes, No)

Odor (Yes, No)

Temperature C

pH value

Other observations

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 EXP.2: Odor Test

This experiment aims at measuring quantitatively the odor as a physical water quality
parameter. Water quality standards require that drinking water should be odorless. Odor in
water affects inversely the acceptability of the water for drinking purposes, food production
and the use of water for recreational purposes (swimming pools). Odor in water is caused
due to the presence and deterioration of organic and inorganic materials such as:
1- Industrial wastes from food production industry (organic source), tanning industry
(inorganic source) and many others.
2- Human wastes when contact with water sources (surface and groundwater).
3- Living plants and microbial activities, for example Algae causes odor in surface water
storages.
4- Extra chlorine dosage in drinking water. Chlorine compounds are used to disinfect
drinking water from pathogens and harmful microorganisms. Chlorine it self has a
disagreeable smell. In addition to that, if the water contains NH 3 (Ammonia), the extra
chlorine content reacts with the Ammonia forming a compound called Trichloramine
(NCL3). This compound causes a disagreeable taste and odor in water.

Odor can be measured experimentally employing the human sense of odor. A panel of at
least five persons will physically test odorous water diluted to 200ml sample. Odor is
measured by calculating the Threshold Odor Number (TON) that is defined as the ratio of
odorous sample diluted with odor free water to a volume of 200ml to the volume of
odorous water used such that odor is just detected. The TON is calculated as:
20
TON
0

A
where A: volume of odorous water used (ml).

Odor can be removed from water by aeration, treating water using activated carbon filters,
ozonation of water containing odor (very efficient, but expensive).

Sample and Reagents:

For the odor test, odorous water samples will be provided by the lab instructor. Distilled
water will be used as odor free water to dilute the odorous samples to 200ml.

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Equipments:

- Graduated cylinders of different sizes.

- Beakers.

- Colored bottles of 300 ml.

Procedure:

1- Take a grab sample of the odorous water prepared in the lab. The instructor will divide
students into groups of 6 persons (panel of 5 testers and one person will prepare the
dilutions). Note that aromatic materials used by the panel persons as fragrance could
affect the results.

2- Rinse the test bottles several times with distilled water. Place 10ml of odorous water
(A) in the test bottle and dilute it to 200ml using distilled water.

3- Fill two clean bottles with distilled water to 200ml volume each for comparison.
Arrange the three bottles in random order.

4- Let the panel detect the existence of odor. If they couldn’t recognize the bottle
containing the odorous water, record the volume A. Rinse the bottle containing the
odorous sample very well with distilled water.

5- Prepare new odorous sample by increasing the volume A (use 10ml increments) dilute it
to 200ml using distilled water. Repeat steps 4 and 5 to a point such that the panel
recognize the bottle containing the odorous water.

Data Analysis

Find the TON of the water sample tested.

Discussion

Discuss your results and compare results with water quality standards. Discuss why it is
recommended to use colored bottles for the odor test?

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 EXP.3: Solids Determination Test

This experiment aims at measuring quantitatively the solids content in water as a physical water
quality parameter. Solids in water appear naturally due to the solvent action of the water on the
soil and rocks. Part of the solids can be found in the water as dissolved material due to the
2+
small solid size (less than 0.001m), for example the Calcium (Ca ). Such dissolved solids
pass an internationally defined filter paper of 0.45m. On the other hand, the suspended solids
retain on the 0.45m filter paper (the solid size is greater than 0.45m).

The presence of the suspended solids in water is a physical indicator of the water pollution
(water is not acceptable for drinking purposes). The presence of dissolved solids in water
indicates water pollution due to the increasing water salinity. For drinking purposes, the
Total Dissolved Solids (TDS) should not exceed 500 mg/L (ppm) according to EPA
standards and not to exceed 1000 mg/L according to the Jordanian standards. Excessive
amounts of dissolved solids cause problems to kidney patients and cause damage to the
energy industry and central heating systems.

The term Total Solids (TS) refers to the combination of the Suspended Solids (SS) and the
Dissolved Solids (DS). The total solids (TS) can be determined experimentally by
evaporating a known volume of water at 103-105C. TS can be either organic or inorganic
by origin, in that case if solids are heated to 550C, the organic content will be converted to
CO2 and H2O, i.e. volatile solids. The non volatile (inorganic) solids remain after ignition
at 550C. Figure 3.1 shows a schematic plot of solids determination.

Water vapor volatile solids

Dish + Water sample

Dish + Total solids Dish + non volatile solids

after drying at 103-105C after ignition at 550C

Fig (3.1): Total solids and non volatile total (fixed) solids determination.

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The suspended solids can be removed from the water partially by sedimentation (physical
process based on size of the particles). Filtration process using sand filters is used also to
remove suspended solids. Moreover microorganisms can degrade (remove) the organic part
of the suspended solids.

The removal of the dissolved solid is more difficult than that for the suspended solids. The
dissolved solids need complicated removal mechanisms due to its solubility. DS can be
removed by: biologically where bacteria can degrade the soluble organics, using nano-
filtration, reverse osmosis and ion exchange for inorganic part of DS.

Sample and Reagent:

Laboratory prepared sample will be used to determine solids content. Distilled water will be
used for cleaning and flushing any solids on surfaces.

Equipments:

The following equipments are needed to conduct the experiment:

- Graduated cylinders.
- Porcelain evaporating dish to contain a sample of 100ml.
- Drying oven (103-105C).
- Desiccator.
- Muffle furnace supplies 550C.
- Electrical balance of 0.1mg sensitivity.
- Filtration apparatus with vacuum source
- Filter paper of 0.45m opening size.
- Tweezers.

Procedure:
Total solids determination

1- Ignite the evaporating dish in the muffle furnace for 1hr and cool it in a desiccator.
2- Measure the gram weight of the empty dish.
3- Replace 50ml of the sample in the evaporating dish and transfer the dish with the
contents to the drying oven. Dry for 24hrs at 103-105C.

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4- Remove the dish and its content from the oven and place it directly in the desiccator.
5- Cool the dish to room temperature, gram weigh the dish with the contents. Record the
total solids gram weight (A).

Total volatile solids

1- Ignite the dish with its content in the muffle furnace at 550°C for 15 min.
2- Cool the dish in the desiccator to room temperature, weigh the dish with its contents.
3- Record the fixed solids gram weight and let that B.

Dissolved solids (fixed + volatile)

1- With tweezers gram weigh the dry filter paper and record value.
2- Place a clean pre-dried filter paper on the filtration apparatus.
3- Pour the 50mL water sample in increments. Switch on the vacuum apparatus to ensure
the passage of all dissolved solids. Collect water that passes the filter paper.
4- Wash the sample container and the filter with distilled water to ensure that all sticky
dissolved material passes the filter paper.
5- Similar to the total solids content determination steps discussed previously, determine
the dissolved solids gram weight and record it as C.
6- Similar to the volatile solids content determination steps discussed previously,
determine the fixed dissolved solids gram weight and record it as D.

Data Analysis:

Calculate the total solids and total volatile solids in mg/L or (ppm) as follow:

Total Solids (TS) = A × 1000 (mg/L)

V

Total Fixed Solids = B × 1000 (mg/L)

V

The Total Volatile Solids (mg/L) =

= Total Solids (mg/L) – Total Fixed Solids (mg/L)
where V: sample volume in ml.

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Calculate the Total Dissolved Solids as follow:

Total Dissolved Solids = C × 1000 (mg/L)

V

Fixed Dissolved Solids = D × 1000 (mg/L)

V
The Volatile Dissolved solids (mg/L) =
= Total Dissolved Solids (mg/L) – Fixed Dissolved Solids (mg/L)

The Total Suspended Solids = Total Solids –Total Dissolved Solids.

The Volatile Suspended Solids = Total Volatile Solids –Volatile Dissolved Solids

Discussion:

Discuss your results and comment on possible inaccurate measurements. Compare all
results with the standards. Note that all results should be expressed in units of mg/l = ppm.

Questions

1- Why is it preferable to use a balance of 0.1mg accuracy rather than 1mg accuracy?
2- Instead of cooling in the desiccator, what would happen if you weigh the dish and its
content while they are hot?

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 EXP.4: Turbidity Test

This experiment aims at measuring quantitatively the turbidity as a physical water quality
parameter. Turbidity is an expression of the optical property that causes light to be scattered
and adsorbed rather than transmitted in straight lines through the sample. Drinking water
should not be turbid, since consumers assume the presence of turbidity in drinking water as
a contamination indicator.

Turbidity in water is caused due to the existence of suspended and/or colloidal particles
such as clay particles, silt and the fine organic and inorganic particles. Figure 5.1
demonstrates the phenomenon of light scattering due to turbid water.

Light from
source

Turbid water

Scattered light
Fig (4.1): Turbid water scatters light streams.

In general, as the particle concentration increases, the turbidity may increase, since there is
no clear correlation between the turbidity and the particle concentration as a result of:
1- Particle shape effect, where rounded shape particles have a different scattering effect
from the sharp edged particles.
2- Size effect.
3- Refractive index differences.

In the past, the turbidity in water was measured using Jackson candle turbidimeter, by which
graduated cylinder replaced over a special candle. During the gradual filling of the turbid water,
the reading at which the light just disappeared was referred as the Jackson Turbidity Unit
(JTU). Nowadays, the turbidity is measured directly and easily using the Nephelometric
turbidity device. The mechanism of such device is based on a comparison of the intensity of

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the light scattered by the turbid water with the intensity of the light scattered by a reference
solution (Formazin polymer solution).

The turbidity readings of the Nephelometric turbidity device are more accurate than the
Jackson candle turbidimeter. The later depends on the human sight (light sensors) which
may differ from one person to the other, while the first depends on light detectors
surrounding the turbid water sample.

Turbidity in water can be removed by:

1- Sedimentation when turbidity is due to the existence of suspended particles.
2- Coagulation followed by sedimentation when turbidity is due to the existence of the
colloidal particles.
3- Filtration.
4- Biologically when turbidity is due to the existence of organic solids.

Sample and Reagents:

A laboratory prepared turbid water (A & B) will be used in the test, where:
- Water A: contains suspended solids.
- Water B: contains colloidal particles. Different dilutions of water B will be prepared
and tested by students. The dilutions are:
zero dilution (100% sample),
25% dilution (75% sample),
50% dilution (50% sample),
75% dilution (25% sample).

Equipments:

- Nephelometric Turbidity meter of readings range:

0 - 20 NTU with accuracy of 0.01 NTU.
20 – 200 NTU with accuracy of 0.1 NTU.
200 – 1000 NTU with accuracy of 1 NTU.

- Standard solutions of known turbidity.

- Beakers.

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Procedure:

1- Switch on the apparatus for 5 -10 minutes to allow for warming up.
2- Using the standard solution of known turbidity, adjust the device if needed.
3- For water A samples, place the sample container in the chamber and close the chamber,
then read the turbidity. Take 5 readings for the turbidity at 5min interval.
4- For water B samples, place the sample container in the chamber and close the chamber,
then read the turbidity. Take 5 readings for the turbidity at 5min interval for each
dilution.
5- Shake all diluted samples of water B and take readings of the turbidity.

Data Analysis:

For water A (suspended solids), draw the turbidity on y-axis and time on x-axis.
For water B (colloidal solids), plot the turbidity on y-axis and time on x-axis.
For all diluted samples of water B, plot the turbidity on y-axis and the concentration
expressed as % of the original sample (100%) on the x-axis.

Discussion:

Discuss your results and comment on the resulted graphs. Compare results (turbidity
values) with the standards of drinking water.

Questions:

Would the water color if exists affect the turbidity results?

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 EXP.5: Coagulation test (Jar Test)

This experiment aims at introducing the coagulants and their rule in enhancing the
sedimentation of smaller particles exist in water like the colloidal particles. Such particles
like proteins and humic acids have small size (less than 1m) and can be removed from
water using coagulants followed by sedimentation or using Nano-filtration.

In water, colloidal particles stay in suspension (do not settle down) due to the existence of a
surface negative charge that creates repulsive forces causing the particles to move in all
directions instead of settling down, i.e. colloidal particles are stable. Coagulation is a
process by which the colloidal particles are de-stabilized (the surface charge is neutralized)
by adding chemicals like Aluminum and Iron salts (positive charge). If the de-stabilized
colloidal particles are mixed well (flocculation process), then such particles will collide and
stick to each other forming large flocs which will settle down eventually as follows:

Colloidal particles + Coagulant + Flocculation Large flocs

In the past, Normalli seeds were used as coagulants. Currently Aluminum salts like
Al2(SO4)3.18H2O, NaAlO2, and Na2Al2O4 and Iron salts like FeCl3.6H2O, FeSO4.7H2O,
and Fe2(SO4)3.9H2O are used as coagulants.

The coagulation process is affected by:

1- Water pH and alkalinity content: high pH and high alkalinity content will lead to the
formation of the soluble complex compound [Al(H 2O)3(OH)3] that will precipitate
eventually, i.e. no coagulation occurs.
2- Water ionic strength: in general cations have positive charge that will neutralize the
charge of the colloidal particle, i.e. the high ionic strength of the water enhances the
coagulation process.
3- Temperature.
4- Type and the dosage of the coagulant.
5- Mixing conditions.

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Sample and Reagents:

A laboratory prepared water sample containing colloidal particles will be used in this test.
Alum coagulant.

Equipments:

- Flocculation device with slow and rapid mixing abilities.

- Beakers of 500ml volume
- pH meter, thermometer and timer.
- Nephlometeric turbidity meter.

Procedure:

1- From the water sample prepared in the lab, take 5 samples each of 500ml volume.
2- Make 1 sample of 500ml distilled water for comparison.
3- Add 5 different dosages of the coagulant as one dose per sample (use 2, 4, 6, 8 and
10mg/L). Measure the pH and the temperature for each sample.
4- Place the six samples on the flocculation device for 1 minute at high mixing speed (150
rpm) and for 15 minutes at low mixing speed (50 rpm).
5- Let the sample to rest for 30 minutes. Visually compare the results.
6- Measure the turbidity for each sample.

Data Analysis:

Visually compare the results of the test.

Plot the turbidity on y-axis with its corresponding coagulant dose on x-axis.
Determine the coagulant optimum dose from the plot of the turbidity.

Discussion:

Discuss your results and comment on the effect of the coagulant on the water sample
containing colloidal particles.

Questions:

What is the value behind finding the optimum coagulant dose to be used in water treatment?

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 EXP.6: Hardness Determination Test

This experiment aims at determining the hardness of water as a chemical water quality
parameter. Scientifically the hardness in water is defined as the total concentration of the
2+ 2+
multi-valent ions like the Calcium (Ca ) and Magnesium (Mg ) ions. It is also defined as
+
the water ability to precipitate soap. In general, the soap consists of Na salts that when
added to water the soluble compound C 15H33COOH (palmatic acid) forms. Such soluble
compound sticks to pollutants in clothes and the combination stays in water after rinsing the
2+ 2+
clothes. When the soap is added to hard water, the multi-valent ions Ca and Mg replace
+ 2+ 2+
the Na forming a precipitative Ca and Mg compounds rather than the soluble
compound C15H33COOH, i.e. the soap does no action on pollutants in the clothes.

2+ 2+
When hard water is used, then the Calcium (Ca ) and Magnesium (Mg ) ions react with
other compounds forming a solid precipitate called the Scale. If compounds like the
- 2-
Bicarbonate (HCO3 ) and the carbonate (CO3 ) exist in water with the existence of the
2+
Ca ions then the following reaction occurs (increases with the heat):

2+ 2-
Ca + CO3 CaCO3 (precipitate)

and at high pH values the following reaction occurs:

2+ -
Mg + OH Mg(OH)2 (precipitate)

The formation of the insoluble compounds like CaCO 3 or Mg(OH)2 is called the scale
formation. The scale formation will reduce the efficiency of heating systems and ultimately
destroy such systems.

2+ 2+
The term total hardness is defined as the total concentration of the Ca and Mg ions in
water expressed in unit of mg/L as CaCO 3 (standard unit). The term carbonate hardness is
associated to the part of the total hardness that is equivalent to the alkalinity (Bicarbonate
- 2-
HCO3 and carbonate CO3 ). The non-carbonate hardness is associated to the existence of
compounds like CaCl2, CaSO4, etc. The sum of the carbonate and the non-carbonate
hardness is the total hardness.

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Hardness in water is treated (softened) through the full or partial removal of the Ca2+ and
2+
Mg ions by:

1- Adding lime Ca(OH)2 to remove the carbonate and CO2 hardness.

2- Adding Soda Na2CO3 to remove the non-carbonate hardness.
3- Using ion exchange (Na+ resin), in that case the Ca2+ and Mg2+ ions replace the Na+ ion.
4- Using reverse osmosis.

The experimental determination of hardness relies on using the chemical compound called
Ethylene Diamine Tetra-Acetic Acid (EDTA). In addition to that, Ammonia buffer solution
(pH of 10) is used in the experiment to prevent the precipitation of the complex compound
formed by the EDTA and metal ions. As result of the high pH value, EDTA will combine
2+ 2+
with the Ca ions first and later with Mg ions as follows:

2+ 2+
EDTA + Ca EDTA-Ca

2+ 2+
EDTA + Mg EDTA-Ca

Sample and Reagents:

Tap water will be tested for the hardness determination. The following reagents will be
needed:
- Ammonia buffer solution (pH of 10).
- Sodium hydroxide solution.
- Erichrome blank T indicator (EBT).
- Methyl red indicator.
- 0.01M EDTA solution.
- Murexide (Ammonium purpurite).

Equipments:

- Pipette.
- Volumetric flask.
- Erlenmeyer flask.
- Magnetic stirrer.

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Procedure:

1- Take a representative sample from tap water and place 50ml into 125ml Erlenmeyer flask.
2- Add 1 – 2ml of Ammonia buffer solution.
3- Add 1 – 2 drops of the EBT indicator.
4- In 5 minutes maximum, titrate with 0.01M EDTA solution until blue color just appears,
record the EDTA solution volume used for calculating the total hardness.
5- Add 1 – 2 ml of Sodium hydroxide solution and 0.2g of murexide indicator to a 50ml
sample and then titrate slowly with EDTA until the solution color becomes purple to
2+
violet, record the EDTA volume for calculating the Ca hardness.

Data Analysis:

Calculate the hardness as:

A × B × 1000
Hardness as mg/L CaCO3 =
V

where
A: EDTA ml used,
B: mg CaCO3 equivalent to 1 ml EDTA (B = 1 for 0.01 M EDTA solution),
V: sample volume (ml).

2+ 2+
Calculate the Ca hardness and Mg hardness.

Discussion:

Discuss your results and comment on the water sample hardness, compare results with
standards.

Questions:

What is the value behind softening the hard water?

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 EXP.7: Alkalinity Determination Test

This experiment aims at determining the alkalinity of water as a chemical water quality
parameter. The water alkalinity is defined as the water ability to neutralize acidity, i.e. the
ability of water to maintain a relatively constant pH when acid materials (hydrogen ions) are
added to water. The alkalinity in water is useful to counter act the acidic environment occurs in
wastewater transporting systems (sanitary sewers) due to the chemical and biological reactions.
Such alkalinity will reduce the corrosion of the sewers. Moreover, the presence of alkalinity in
surface water bodies is important for fish and aquatic life because it protects or buffers against
rapid pH changes when acidic materials are dumped in surface waters.

Alkalinity in water exists naturally due to the presence of natural compounds like the
- 2- -
Bicarbonate (HCO3 ), the Carbonate (CO3 ) and the Hydroxides OH . Such compounds
may exist naturally or due to the dissolved CO 2 in water. The following reactions
demonstrate how the alkalinity forms from the dissolved CO 2,

CO2 + H2O H2CO3 (carbonic acid)

+ -
H2CO3 H + HCO3 (bicarbonate) pH increases

- + 2-
HCO3 H + CO3 (carbonate)

2- - -
CO3 + H2O HCO3 + OH (hydroxide)

The alkalinity in water is measured experimentally through titrating the water sample with
standard Sulfuric acid of 0.02 normality (0.02N H 2SO4). For a water sample of 1L volume,
each ml of acid used in the titration is equivalent to 1mg of alkalinity expressed as mg/L as
CaCO3 (standard unit). The total water alkalinity equals to the amount of ml acid used to
bring down the water pH to 4.5.

Referring to the alkalinity standard titration curves, it can be seen that for water of pH > 8.3
-
the water alkalinity is due to the presence of the Bicarbonate (HCO 3 ), the Carbonate
2- -
(CO3 ) and the Hydroxides OH . For water with pH ≤ 8.3, the water alkalinity is mainly
-
due to the presence of the Bicarbonate (HCO 3 ).

- 22 -
The presence of alkalinity may have negative impact on water. Usually water with high
2+ 2+
alkalinity level has a bitter taste. Moreover, the existence of the Ca and Mg ions in
- 2-
water will react with the alkalinity forming species (Bicarbonate HCO 3 , Carbonate CO3
-
and Hydroxide OH ) leading to the formation of the solid precipitate (scale) that has
negative impact to the energy industry as discussed previously in the hardness test.

Sample and Reagents:

Tap water will be tested for the alkalinity determination test. The following reagents will be
needed:
- Standard sulfuric acid (0.02N).
- Phenolphthalein.
- Mixed indicator (Bromocresol green, methyl red, Ethyl alcohol).
- Distilled water.

Equipments:

- Pipette.
- 250ml Erlenmeyer flask.
- Measuring cylinders.
- Beakers and flasks

Procedure:

1- Rinse the pipette with 0.02N sulfuric acid and discard the solution. Adjust the reading on
the pipette to read 0.
2- Using a measuring cylinder, measure exactly 100ml of the water sample and place it in
the 250ml Erlenmeyer flask. Measure and record the water sample pH and temperature.
3- Add few drops of the Phenolphthalein indicator to the flask contents. If the color of the
-
solution turns pink, then alkalinity due to the hydroxide (OH ) exists. Titrate the sample
with the standard 0.02N sulfuric acid until the pink color just disappears. Record the ml
-
acid used (call it VH) to neutralize the alkalinity due to the hydroxide (OH ).
4- To the same sample solution, add few drops of the mixed indicator. The solution color
- 2-
will become blue, i.e. the Bicarbonate HCO 3 and Carbonate CO3 ions exist.
5- Continue the titration until the solution becomes red. Record the final ml acid used (call
it VT) to neutralize the total alkalinity.

- 23 -
Data Analysis:
-
Calculate the OH alkalinity as:
-
OH alkalinity as mg/L CaCO3 = VH × 10
-
where VH: ml acid used to neutralize OH alkalinity,

Calculate the total alkalinity as:

Total alkalinity as mg/L CaCO3 = VT × 10

where VT: ml acid used to neutralize the total alkalinity.

- 2-
Recall that if VH = 0, then OH alkalinity = 0 and the CO3 alkalinity = 0, and the total
-
alkalinity = HCO3 alkalinity which is the case when the water pH ≤ 8.3.

Discussion:

Discuss your results and comment on the water sample alkalinity, compare results with
standards if existed.

Questions:

Alkalinity existence in drinking water is preferred, explain why?

- 24 -
 EXP.8: Dissolved Oxygen Determination Test

This experiment aims at determining the amount of Dissolved Oxygen (DO) in the water or
wastewater for treatment necessity. Gases, including the oxygen itself, can dissolve easily
in the water and their solubility depends on many factors like the nature of the gas, the
pressure, the temperature and the saturation concentration. The following graph
demonstrates the oxygen gas solubility versus the temperature at sea level.

16
14
12

DO(mg/L) 10
8
6
4
2
0
0 5 10 15 20 25 30 35 40
o
Temperature ( C)

Fig (8.1): DO level versus the temperature at sea level.

Since domestic wastewater contains considerable content of the organic matter, then as time
proceeds, the micro-organisms living in the wastewater will consume the dissolved oxygen
in the wastewater to produce energy from the organic material content. The more the
energy produced, the more DO consumed leaving the wastewater with nearly zero DO
level. The DO level in wastewater can be measured experimentally through:
1- The iodometric method (Winkler method).
2- The electrometric method using oxidimeter.

Compared to the electrometric method, the Winkler method is used for its accuracy. In the
Winkler method, Manganese sulfate (MnSO 4) and the Sodium hydroxide (NaOH) are used
to explore the presence of the DO. If the water sample does not contain Oxygen, then the
following reaction occurs,

MnSO4 + 2NaOH Mn(OH)2 (white precipitate) + Na2SO4

- 25 -
If Oxygen presents in the wastewater, then the following reaction occurs,

MnSO4 + 2NaOH+1/2O2 MnO2 (brown solution) + Na2SO4 + H2O

The MnO2 (brown solution) will oxidize the iodide ions in the Alkli-Iodide-Azide solution
(NaOH + NaI + NaN3) under acidic environment provided by the sulfuric acid (H 2SO4) as
follows,

+ - 2+
MnO2 + 4H + 2I I2 + Mn + 2H2O (Yellow solution)

Where the amount of the free Iodine (I2) released is equivalent to the amount of O 2
presents. If the solution is titrated with Sodium thiosulfate (Na 2S2O3), the Iodine ions will
be released as follows,

+ 2- -
2Na2S2O3 + I2 4Na + S4O6 + 2I (pale straw)

The released Iodine is detected using the starch solution. The last two reactions above
simply tell that the Oxygen amount presents in the water is equivalent to the amount of the
thiosulfate used in the titration. It should be noted that, if the water sample contains nitrate,
then the nitrate will react with the free Iodine which will affect the results, therefore the
sodium Azide solution is added to prevent such reaction.

Sample and Reagents:

Tap water will be tested for the dissolved Oxygen determination test. The following
reagents will be needed:
- Manganese sulfate (MnSO4) solution.
- Alkli-Iodide-Azide solution (NaOH + NaI + NaN3).
- Sulfuric acid H2SO4.
- Starch solution.
- Sodium thiosulfate (Na2S2O3) solution.

- 26 -
Equipments:

- BOD bottles.
- Pipette.
- Measuring cylinders.
- Beakers and flask.

Procedure:

1- Fill the BOD bottles with 200ml of the sample.

2- Add 2ml of Manganese sulfate (MnSO 4) solution and then add 2ml of Alkli-Iodide-
Azide solution (NaOH + NaI + NaN3).
3- Mix the bottle content well through inverting the bottle several times and let the bottle
rests.
4- If the settled flocs have white color, then the DO level is zero. If the flocs have brown
color, add 2ml of Sulfuric acid (H 2SO4) and shake the bottle until clear yellow color
appears.
5- Transfer the bottle contents to the Erlenmeyer flask and titrate the solution with the
Sodium thiosulfate (Na2S2O3) to have pale straw color solution.
6- Add 1ml of starch solution and continue titrating the solution with the Sodium
thiosulfate until the blue color just disappeared. Record the ml of the Sodium thiosulfate
solution used in the titration.

Data Analysis:

Calculate the DO amount as:

DO in mg/L = (ml of the titrant × normality of titrant×8000)/Sample volume.

Discussion:

Discuss your results and comment on errors that could happen.

Questions:

Why the sulfuric acid is used in the experiment?

Would the measured DO level be higher or lower than the actual DO value if the Sodium
Azide was not used?

- 27 -
 EXP.9: Biological Oxygen Demand (BOD) Test

This experiment aims at determining the Biological Oxygen Demand (BOD) in wastewater
sample. The BOD is defined as the amount of Oxygen that is needed by micro-organisms to
decompose the soluble organic material for energy production and cells build up. The
organic material, as a major component, is presented in domestic wastewater due to human
daily activities like food consumption.

As mentioned previously, the organic material forms the major source to produce energy
for bacteria (micro-organism), therefore the higher the organic material content in the
wastewater, the more oxygen is needed to produce energy under aerobic conditions. In
conclusion, it can be said that the BOD is an indirect measure of the organic material
concentration in water and wastewater. The following simple reaction represents the
relation between the organic material content and the amount of oxygen consumed,

Organic matter + O2 + Bacteria Energy + H2O + CO2

It should be noted that the BOD value in wastewater is affected by the wastewater
temperature, the higher the temperature is the more active bacteria will be, and
consequently more oxygen will be consumed. Therefore to unify the BOD test procedure,
the BOD5 has been introduced. The BOD5 is a standard test that is defined as the amount of
Oxygen that is needed by micro-organisms to decompose the soluble organic material over
5 consecutive days at 20 C.

Based on BOD5 values, the wastewater is generally classified into: high strength
wastewater when the BOD5 > 300mg/L, medium strength wastewater when the BOD 5 is
around 200mg/L and low strength wastewater when the BOD 5 < 100mg/L. Since the BOD
is an oxygen determination test, the Winkler method is used in such test.

In practice, domestic wastewater could have high strength and may contain nitrogen
compounds, therefore care should be taken to reduce the strength of the tested sample and to
account for the amount of oxygen needed for the nitrification process, i.e. the oxygen needed to
oxidize nitrogen. In the BOD5 test, a dilute water solution of zero organic material content

- 28 -
is used to account for the oxygen needed for the nitrification process if exists and to reduce
the strength (dilute the original wastewater sample) of the tested wastewater to reach the
level of the oxygen dissolved naturally in water.

Sample and Reagents:

A lab prepared wastewater sample to simulate the dairy industry will be tested for the BOD 5
determination. In addition to the DO test reagents, the following reagents will be needed:
- Phosphate buffer solution.
- Magnesium sulfate solution (MgSO4).
- Calcium chloride solution (CaCl2).
- Ferric chloride solution (FeCl3).
- Distilled water.

Equipments:

- BOD bottles.
- Pipette.
- Measuring cylinders.
- Beakers and flask.
- BOD incubator.

Procedure:

1- To prepare the dilute water solution, take 2L distilled water and add 2ml each of
phosphate buffer, MgSO4, CaCl2 and FeCl3. The dilute water will be needed to prepare
the blank sample to account for the effect of the nitrification and to reduce the strength
of the wastewater sample. The dilute water samples should be prepared 3 – 5 days and
aerated well before the BOD 5 test. If the dilute water sample shows microbial growth, it
should be discarded.
2- Fill 2 BOD bottles with the blank solution (dilute water) to the full mark (make sure no
air bubbles exist) and close samples with stopper. Test one of the blank samples
immediately after preparation to determine the initial DO content. The other sample will
be tested after 5 consecutive days of incubation at 20 C.

- 29 -
3- Fill 2 BOD bottles each with 30ml of the original wastewater sample and dilute both
samples to 300ml using the dilute water solution prepared previously (make sure no air
bubbles exist) and close samples with stopper. Test one sample immediately after
preparation to determine the initial DO content in the sample.
4- Incubate one blank sample and one wastewater diluted sample for 5 consecutive days at
20 C.

5- After the 5 days, test the blank sample and the wastewater diluted sample for the 5 days
DO content.

Data Analysis:

Calculate the BOD5 amount as:

BOD5 in mg/L =

= [S0 – S5 – (B0- B5)] × volume of the diluted sample / ml of the original sample taken.

S0: diluted sample initial DO.

S5: diluted sample DO after the 5 days.
B0: blank sample initial DO.
B5: blank sample DO after the 5 days.
Volume of the diluted sample: volume tested for the DO test = 200ml.
ml of the original sample taken = 30ml in our test.

Discussion:

Discuss your results and comment on possible errors that could happen.

Questions:

What is the purpose of the blank solution?

Which is the greater, the 20 C 4 days BOD or the 20 C 6 days BOD? Why?

- 30 -
 EXP.10: Chemical Oxygen Demand (COD) Test

This experiment aims at determining the Chemical Oxygen Demand (COD) in wastewater
sample. The COD is defined as the amount of Oxygen that is needed chemically to oxidize
the organic material in the wastewater sample. Based on the definition, the COD test
indirectly measures the organic material content in the wastewater.

Since the BOD5 requires 5 days to provide results in relation to treatment quality that it is
too long time when a decision is needed to be taken, the COD test offers a quick result (in
the order of 2 hours). Therefore for treatment plant operation and control, the COD test is
more useful in comparison to the BOD5.

In the COD test, the oxidation of the organic material is utilized using either Potassium
permanganate (KMnO4) or Potassium dichromate (K2Cr2O7) that is considered the best
oxidizing agent. The following reaction simplifies the COD reaction process,

+ 3+
Organic material + K2Cr2O7 + H + heat CO2 + H2O + Cr

+
The H ions are provided from using H 2SO4 that plays as a catalyst, while the heat will
speed up the organic material digestion process. In the reaction above the organic material
+6 +3
is oxidized to CO2 and H2O, while the chromate Cr2 is reduced to Cr2 . The dichromate
consumed by the sample is equivalent to the amount of the oxygen required to oxidize the
organic material.

It should be noted that the BOD 5 measures the amount of the oxygen needed to biologically
oxidize the soluble and bio-degradable part of the organic material (the ready for microbial
consumption), however the non-biodegradable part of the organics is not measured in the
BOD5 test. The COD test procedure with its digestion ability (employing the H 2SO4 with
heat) will enable us to measure all the organic material content. In reality the COD test
always gives results higher than the BOD5 test.

- 31 -
Sample and Reagents:

A lab prepared wastewater sample to simulate the dairy industry will be tested for the COD
determination. The following reagents will be needed:
- Potassium dichromate (K2Cr2O7).
- Sulfuric acid (H2SO4).
- Ferrous ammonium sulfate.
- Silver sulfate (AgSO4).
- Mercury sulfate (HgSO4).
- Ferroin indicator
- Distilled water.

Equipments:

- COD digester and COD tubes (vials).

- Pipette.
- Measuring cylinders.
- 250ml Erlenmeyer flask.
- Wash bottle.

Procedure:

1- Take 2 COD tubes. Add 2.5ml of the wastewater sample to one COD tube and 2.5ml of
distilled water (blank) to the other COD tube.
2- Add 1.5ml of Potassium dichromate to both tubes.
3- Carefully add 3.5ml of sulfuric acid to both tubes. Close both tubes with the cover.
4- Place both tubes (sample and blank) in the COD digester to 2 hours at 150 C.

5- Cool both tubes to room temperature and later transfer the content to the 250ml
Erlenmeyer flask.
6- Add 2 drops of Ferroin indicator where the color becomes bluish green, and then titrate the
contents with Ferrous ammonium sulfate until the color is changed to reddish brown.

- 32 -
Data Analysis:

Calculate the COD amount as:

COD in mg/L = [B – S] × N × 8000/ ml of the original sample taken.

B: volume of ferrous Ammonium sulfate for plank sample.

S: volume of ferrous Ammonium sulfate for wastewater sample.
N: normality of ferrous Ammonium sulfate = 0.1N.

Discussion:

Discuss your results and comment on possible errors that could happen.

Questions:

What is the purpose of the Potassium dichromate in the COD test?

What is the purpose of the COD digester?

- 33 -