Waste Water Treatment Lab

Submitted to:
Muhammad sulaiman
Submitted by:
Usman Nisar
2018-BET-CHEM-01
Chemical, Polymer & Composite Materials Engineering
Department
University of Engineering & Technology, Lahore
(New Campus)
Session 18

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Table of contents:
Abstract……………………………………………………3
Experiment#1……………………………………………...4
Experiment#2……………………………………………...11
Experiment#3………………………………………………19
Experiment#4………………………………………………21
Experiment#5………………………………………………25
Experiment#6………………………………………………29
Experiment#7………………………………………………31
Experiment#8………………………………………………36
Experiment#9………………………………………………41
References…………………………………………………45

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Abstract:
The objective of this lab is to cover all the treatments which are used to clean the
waste water the major aim of wastewater treatment is to remove as much of the
suspended solids as possible before the remaining water, called effluent, is
discharged back to the environment. As solid material decays, it uses up oxygen,
which is needed by the plants and animals living in the water. The report included
following treatment filtration and sedimentation of waste water in which particles
settle down by gravit,conductivity and turbidity of waste water, determination ppm
of total alkalinity, estimation of total solids, then we determine total hardness and
calcium hardness in waste water, coagulation and flocuation,find BOD and COD
test of given sample of waste water treatment. His principal objective of wastewater
treatment is generally to allow human and industrial effluents to be disposed of
without danger to human health or unacceptable damage to the natural environment.
Irrigation with wastewater is both disposal and utilization and indeed is an effective
form of wastewater disposal (as in slow-rate land treatment). However, some degree
of treatment must normally be provided to raw municipal wastewater before it can
be used for agricultural or landscape irrigation or for aquaculture. The quality of
treated effluent used in agriculture has a great influence on the operation and
performance of the wastewatersoil-plant or aquaculture system. In the case of
irrigation, the required quality of effluent will depend on the crop or crops to be
irrigated, the soil conditions and the system of effluent distribution adopted. Through
crop restriction and selection of irrigation systems which minimize health risk, the
degree of pre-application wastewater treatment can be reduced. A similar approach
is not feasible in aquaculture systems and more reliance will have to be placed on
control through wastewater treatment.

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 Industrial Waste Water Analysis
EXPERIMENT# 01

Objective:

1. Sedimentation
2. Filtration

Apparatus:

Beaker (sedimentation tank), Stop watch, Filter paper, Funnel, Flask.

Reagents:

1. Industrial waste water

Theory:

Sedimentation
Sedimentation is a physical water treatment process using gravity to remove suspended solids from
water. Solid particles entrained by the turbulence of moving water may be removed naturally by
sedimentation in the still water of lakes and oceans. Settling basins are ponds constructed for the
purpose of removing entrained solids by sedimentation. Clarifiers are tanks built with mechanical
means for continuous removal of solids being deposited by sedimentation. Clarification does not
remove dissolved species. Sedimentation is the act of depositing sediment.

Settling of discrete particles:

Unhindered settling is a process that removes the discrete particles in a very low concentration
without interference from nearby particles. In general, if the concentration of the solutions is lower
than 500 mg/L total suspended solids, sedimentation will be considered discrete. Concentrations
of raceway effluent total suspended solids (TSS) in the west are usually less than 5 mg/L net.

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Settlement of flocculent particles:

In a horizontal sedimentation tank, some particles may not follow the diagonal line while settling
faster as they grow. So this says that particles can grow and develop a higher settling velocity if a
greater depth with longer retention time. However, the collision chance would be even greater if
the same retention time were spread over a longer, shallower tank. In fact, in order to avoid
hydraulic short-circuiting, tanks usually are made 3–6 m deep with retention times of a few hours.

Zone-settling behaviour:

As the concentration of particles in a suspension is increased, a point is reached where particles

are so close together that they no longer settle independently of one another and the velocity fields
of the fluid displaced by adjacent particles, overlap. There is also a net upward flow of liquid
displaced by the settling particles. This results in a reduced particle-settling velocity and the effect
is known as hindered settling.

Applications:

Potable water treatment:

Sedimentation in potable water treatment generally follows a step of chemical coagulation and
flocculation, which allows grouping particles together into flocs of a bigger size. This increases
the settling speed of suspended solids and allows settling colloids.

Filtration:
Filtration is a process used to separate solids from liquids or gases using a filter medium that allows
the fluid to pass through but not the solid. The term "filtration" applies whether the filter is
mechanical, biological, or physical. The fluid that passes through the filter is called the filtrate.
The filter medium may be a surface filter, which is a solid that traps solid particles, or a depth
filter, which is a bed of material that traps the solid.

Filtration is typically an imperfect process. Some fluid remains on the feed side of the filter or
embedded in the filter media and some small solid particulates find their way through the filter.
As a chemistry and engineering technique, there is always some lost product, whether it's the liquid
or solid being collected.

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Examples of Filtration:

While filtration is an important separation technique in a laboratory, it's also common in

everyday life.

• Brewing coffee involves passing hot water through the ground coffee and a filter.
The liquid coffee is the filtrate. Steeping tea is much the same, whether you use a
tea bag (paper filter) or tea ball (usually, a metal filter).
• The kidneys are an example of a biological filter. Blood is filtered by the
glomerulus. Essential molecules are reabsorbed back into the blood.
• Air conditioners and many vacuum cleaners use HEPA filters to remove dust and
pollen from the air.
• Many aquariums use filters containing fibers that capture particulates.
• Belt filters recover precious metals during mining.
• Water in an aquifer is relatively pure because it has been filtered through sand and
permeable rock in the ground.

Filtration Methods:

There are different types of filtration. Which method is used depends largely on whether the
solid is a particulate (suspended) or dissolved in the fluid.

General Filtration:

The most basic form of filtration is using gravity to filter a mixture. The mixture is poured from
above onto a filter medium (e.g., filter paper) and gravity pulls the liquid down. The solid is left
on the filter, while the liquid flows below it.

Vacuum Filtration:

A Büchner flask and hose are used to create a vacuum to suck the fluid through the filter
(usually with the aid of gravity). This greatly speeds the separation and can be used to dry the

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solid. A related technique uses a pump to form a pressure difference on both sides of the filter.
Pump filters do not need to be vertical because gravity is not the source of the pressure
difference on the sides of the filter.

Cold Filtration:

Cold filtration is used to quickly cool a solution, prompting the formation of small crystals. This
is a method used when the solid is initially dissolved. A common method is to place the
container with the solution in an ice bath prior to filtration.

Hot Filtration:

In hot filtration, the solution, filter, and funnel are heated to minimize crystal formation during
filtration. Stemless funnels are useful because there is less surface area for crystal growth. This
method is used when crystals would clog the funnel or prevent crystallization of the second
component in a mixture.

Sometimes filter aids are used to improve flow through a filter. Examples of filter aids are silica,
diatomaceous earth, perlite, and cellulose. Filter aids may be placed on the filter prior to filtration
or mixed with the liquid. The aids can help prevent the filter from clogging and can increase the
porosity of the "cake" or feed into the filter.

Filtration vs. Sieving:

A related separation technique is sieving. Sieving refers to use of a single mesh or perforated
layer to retain large particles while allowing the passage of smaller ones. In contrast, during
filtration, the filter is a lattice or has multiple layers. Fluids follow channels in the medium to
pass through a filter.

Alternatives to Filtration:

There are more effective separation methods than filtration for some applications. For example,
for very small samples in which it's important to collect the filtrate, the filter medium may soak

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up too much of the fluid. In other cases, too much of the solid can become trapped in the filter
medium

Two other processes that can be used to separate solids from fluids are decantation and
centrifugation. Centrifugation involves spinning a sample, which forces the heavier solid to the
bottom of a container. In decantation, the fluid is siphoned or poured off of the solid after it has
fallen out of solution. Decantation can be used following centrifugation or on its own.

Procedure:

Sedimentation:

1. Take 50ml of sample water.

2. Fill it in clean and dry beaker and start the stop watch.
3. Place it on a table for sedimentation.

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 4. Note the time when all the suspended solids are settled.

Filtration:

1. Take a clean and dry filter paper and make a conical shape.
2. Place it in the funnel and place the funnel on conical flask.
3. Now add the sample water slowly and fill it to the edges of the filter paper.

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Calculations Observation:
Time required for the sediments to settle down = 30min
Time taken for filtration of 100ml = 30min
Observe the cleanness of water after filtration and sedimentation

Figure 1Sample water after filtration

Figure 2Sample water after sedimentation

Results:

When we place the sample for filtration it takes 30min to sattle down the suspended particals and
filtration also takes 30min to fitrate the 100ml of sample water. You see in in above images that
filtered water is more clean than sendimentation water.

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 EXPERIMENT# 02

Objectives:

1. Determine the PH of the water sample by using PH paper

2. Determine the ppm of total alkalinity in the given sample of water.
3. Point out the type of alkalinity in the given sample of water.

Apparatus:

Measuring flask, burette and funnel PH paper.

Reagents:

N/50 HCl, methyl orange, phenolphthalein, water sample.

Theory:

Alkalinity and pH:

Alkalinity and pH are two important factors in determining the suitability of water for irrigating
plants. pH is a measure of the concentration of hydrogen ions (H+) in water or other liquids. In
general, water for irrigation should have a pH b etween 5.0 and 7.0. Water with pH below 7.0 is
termed "acidic" and water with pH above 7.0 is termed "basic"; pH 7.0 is "neutral". Sometimes
the term "alkaline" is used instead of "basic" and often "alkaline" is confused with "alkalinity".
Alkalinity is a measure of the water's ability to neutralize acidity. An alkalinity test measures the
level of bicarbonates, carbonates, and hydroxides in water and test results are generally expressed
as "ppm of calcium carbonate (CaCO3)". The desirable range f or irrigation water is 0 to 100 ppm
calcium carbonate. Levels between 30 and 60 ppm are considered optimum for most plants.

Irrigation water tests should always include both pH and alkalinity tests. A pH test by itself is not
an indication of alkalinity. Water with high alkalinity (i.e., high levels of bicarbonates or
carbonates) always has a pH value ÷7 or above, but water with high pH doesn't always have high
alkalinity. This is important because high alkalinity exerts the most significant effects on growing
medium fertility and plant nutrition.

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High pH and High Alkalinity Effects on Plant Nutrition:

Potential adverse effects. In most cases irrigating with water having a "high pH" ( 7) causes no
problems as long as the alkalinity is low. This water will probably have little effect on growing
medium pH because it has little ability to neutralize acidity. This situation is typical for many
growers using municipal water in Massachusetts, including water originating from the Quabbin
Reservoir.

Of greater concern is the case where water having both high pH and high alkalinity is used for
irrigation. In Massachusetts this situation is most common in Berkshire county. One result is that
the pH of the growing medium may increase signifi cantly with time. This increase may be so large
that normal lime rates must be reduced by as much as 50%. In effect the water acts as a dilute
solution of limestone! The problem is most serious when plants are grown in small containers
because small volum es of soil are poorly buffered to pH change. Therefore, the combination of
high pH and high alkalinity is of particular concern in plug seedling trays. Trace element
deficiencies and imbalances of calcium (Ca) and magnesium (Mg) can result from irrigating with
high alkalinity water.

It is much more difficult to predict the effects of irrigating outdoor flower crops, gardens, and
landscape plants with water having high pH and high alkalinity. On the one hand, in some parts of
the United States, long-term irrigation of crops with wa ter high in bicarbonates and carbonates
has led to yield-limiting trace element deficiencies which must be corrected with special fertilizers.
On the other hand, in New England, several factors probably act together to partially offset the
effects of high alkalinity water. First, rainfall levels are relatively high and historically this has
caused Ca and Mg ions to leach from the soil. These are replaced with H+ and the result is acidic
soil. Second, this acidification may be helped along by the rather ac idic rainfall common in this
region in more recent times. Third, acid-forming fertilizers also help counteract high pH and
alkalinity.

Potential beneficial effects. For some greenhouse operators, water with moderate levels of
alkalinity (30-60 ppm) can be an important source of Ca and Mg. With the exception of Peter's
EXCEL and a few other fertilizers, most water soluble fertil izers do not supply Ca and Mg. Also,
the Ca and Mg from limestone may be inadequate for some plants. Moderately alkaline water

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could be beneficial as a source of extra Ca and Mg for crops prone to Ca and Mg deficiencies (e.g.,
poinsettia).

Other Effects of High pH and High Alkalinity:

In addition to nutritional disorders of plants, water with high alkalinity can cause other problems.
Bicarbonates and carbonates can clog the nozzles of pesticide sprayers and drip tube irrigation
systems with obvious effects. The activity of some pestici des, floral preservatives, and growth
regulators is markedly reduced by high alkalinity. When some pesticides are mixed with water
they must acidify the solution to be completely effective. Additional acidifier may be needed to
neutralize all of the alkal inity. To determine if a chemical is affected by high alkalinity, carefully
review the product's label. Unfortunately this potentially important information is not always
printed on the label, so considerable extra effort may be necessary to find the inf ormation. A call
to the manufacturer will probably be needed for most chemicals.

Acidification of High Alkalinity Water:

Many greenhouse operators inject acid (e.g., phosphoric, nitric, or sulfuric acid) into water with
problematic high levels of alkalinity. Acidification of water having high pH but low alkalinity is
rarely necessary. The use of acid injection sh ould be considered very carefully for several reasons.
First, it is an extra step in production which will require additional materials and equipment.
Second, acids are dangerous to handle and may damage some injectors and piping systems. Third,
phosphori c or nitric acid are sources of P and NO3, so the regular fertilizer program may need to
be modified to take into account the addition of these nutrients. This would depend on how much
acid must be used to neutralize the alkalinity and reduce pH. Fourth, sometimes acid injection
causes the solubilization of normally precipitated (unavailable) forms of trace elements resulting
in levels toxic to plants.

The amount of acid required to reach the desired pH (i.e., neutralize alkalinity) is determined by
laboratory titration of a water sample with the appropriate acid or by a calculation procedure. Some
"fine-tuning" may be needed later when actual inject ion is started. Acid is always injected prior
to the addition of fertilizer or other chemicals.

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Determination of PH:

1. Take sample water in small beaker.

Figure 4Water Sample

2. Dip the small part of pH paper in sample and record the reading according to the pH table
by comparing the color.

Figure 3Finding pH

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Record the reading after and before the filtration.

No. of Obs. pH after the filtration pH before the filtration

1. 8 8
2. 8 8
Results:

The pH of the industrial waste water is 8 which shows that it is basic. It is basic due to the
presence of NaOH

Total Alkalinity Procedure:

1. Clean the burette and fill almost to the top with

N/50 HCL. Then run some acid to waste until
the "zero" mark is reached. This should leave
the stopcock and tip of the burette full of the
solution.
2. Measure out 100 ml of the water to be tested and
pour into a clean white porcelain evaporating
dish.
Figure: 5 100 ml of water to be tested

3. Add 2 or 3 drops of methyl orange or methyl

purple indicator to the sample and stir. When
alkalinity is present, the solution becomes
yellow when methyl orange is added or
becomes green when methyl purple is added.
(Note: When high chlorine residual is present,
the chlorine bleaches the color and makes the
determination of endpoint difficult. The
chlorine may be removed using sodium

Figure 6 when methyl orang is added

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 thiosulfate, or an additional indicator may be added.
4. Slowly and carefully add N/50 HCL. from the
burette to the contents of the dish until the faintest
pink coloration appears - that is, until the color of the
solution is no longer yellow. While adding the acid,
the solution should be gently stirred with the stirring
rod. It is often advantageous to set up two 10 ml
samples, adding methyl orange to each and acid to
only one while the other is held alongside so that the
colors may be compared and the color change to pink
can be better recognized. (Note: When using methyl
purple, the color is changed to purple. A gray tint
precedes the end point and warns the operator of its
approach.)
Figure 7 After titrating with HCl

5. Record the volume of HCL used to reach the endpoint.

No. Obs. Initial volume of HCl (ml) Fina volume of HCl (ml) Volume used (ml)
1. 35.1 39.9 5.0
2. 39.9 34.8 5.1
3. 34.8 29.9 4.9

Calculation:

T. alk = (ml of acid) × (10 ppm/ml)

As 5 ml of acid were used in the titration, so the total alkalinity would be:

T. alk. = (5) × (10) = 50 ppm CaCO3

Result:

In the industrial water there is 50mg of CaCO3 is present in 1L of the water

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Phenolphthalein Alkalinity Procedure:

1. Clean the burette and fill almost to the

top with N/50 sulfuric acid. Then run
some acid to waste until the "zero" mark
is reached. This should leave the
stopcock and tip of the burette full of the
solution.
2. Measure out 100 ml of the water to be
tested and pour into a clean white
porcelain evaporating dish. Stir the
sample.

Figure 8 100ml sample

3. With a dropping bottle, add 5 drops of phenolphthalein indicator to the sample and stir.
When phenolphthalein alkalinity is present, the solution becomes pink. No color
indicates the phenolphthalein alkalinity is zero and that the test is complete. No color
also indicates that free carbon dioxide is present, and the same sample may be used to
test for carbon dioxide.

Figure 9 After adding phenolphthalein

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 4. If pink color results after the indicator is added, slowly and carefully add N/50
sulfuric acid from the burette to the contents of the dish until the coloration
disappears. While adding the acid, the solution should be gently stirred with the
stirring rod.

Figure 10 After titrating against HCl

5. Record the volume of sulfuric acid used to reach the end point.

No. Obs. Initial volume of HCl (ml) Fina volume of HCl (ml) Volume used (ml)
1. 31.0 32.4 1.4
2. 32.4 33.9 1.5
3. 33.9 35.1 1.2

Calculations:

Calculate the phenolphthalein alkalinity, in ppm, as follows:

P. alk. = (ml of acid) × (10 ppm/ml)

As, 1.36 ml of acid were used, the phenolphthalein alkalinity would be:

P. alk. = (1.35) × (10) = 13.5 ppm CaCO3

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Result:

So, there is 13.5ppm of CaCO3 are present it means that 13.6mg of CaCO3 are present in 1L of
sample water.

EXPERIMENT# 03
Objective:
• Estimation of total solids (expressed as ppm.) in a tap water sample by Gravimetric
method.

Equipment Setup / Apparatus:

Oven, Petri Dish, Weight Balance
Reagents:

Waste Water.

Theory:

Total solids:

Total solids are dissolved solids plus suspended and settleable solids in water. In stream water,
dissolved solids consist of calcium, chlorides, nitrate, phosphorus, iron, sulfur, and other ions
particles that will pass through a filter with pores of around 2 microns (0.002 cm) in size.
Suspended solids include silt and clay particles, plankton, algae, fine organic debris, and other
particulate matter. These are particles that will not pass through a 2-micron filter.

The concentration of total dissolved solids affects the water balance in the cells of aquatic
organisms. An organism placed in water with a very low level of solids, such as distilled water,
will swell up because water will tend to move into its cells, which have a higher concentration of
solids. An organism placed in water with a high concentration of solids will shrink somewhat
because the water in its cells will tend to move out. This will in turn affect the organism's ability
to maintain the proper cell density, making it difficult to keep its position in the water column. It
might float up or sink down to a depth to which it is not adapted, and it might not survive.

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Higher concentrations of suspended solids can serve as carriers of toxics, which readily cling to
suspended particles. This is particularly a concern where pesticides are being used on irrigated
crops. Where solids are high, pesticide concentrations may increase well beyond those of the
original application as the irrigation water travels down irrigation ditches. Higher levels of solids
can also clog irrigation devices and might become so high that irrigated plant roots will lose water
rather than gain it.

A high concentration of total solids will make drinking water unpalatable and might have an
adverse effect on people who are not used to drinking such water. Levels of total solids that are
too high or too low can also reduce the efficiency of wastewater treatment plants, as well as the
operation of industrial processes that use raw water.

Total solids also affect water clarity. Higher solids decrease the passage of light through water,
thereby slowing photosynthesis by aquatic plants. Water will heat up more rapidly and hold more
heat; this, in turn, might adversely affect aquatic life that has adapted to a lower temperature
regime.

Sources of total solids include industrial discharges, sewage, fertilizers, road runoff, and soil
erosion. Total solids are measured in milligrams per liter (mg/L).

Procedure:
1. Find the mass of a clean dry 250 cm3 beaker.

2. Add 100cm3 the mass of the cool dry beaker.

3. The total dissolved solids in the water sample in mg/l (ppm.) of a filtered water sample to
the beaker.
4. Evaporate to dryness in a dust-free oven at 105 o C. Find the mass of cool dry beaker.

5. Calculate the total dissolved solids in water sample in mg/l (ppm).

Data Analysis:
Initial Weight (Weight of Empty Petri Dish) = X 52 grams

Final Weight (Weight of Petri Dish + Solids) = Y 72.607 grams

Increase in Weight (Weight of Total Solids) = Y-X = Z 1 grams

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 Volume of Sample = 20.607 ml

EXPERIMENT# 04
Objective:
To find the ppm of Cl-1 ions in the sample water.

Apparatus required:
Beaker, Test tube, Burner, Graduated Cylinder, Stirrer, Water bath, filter paper.

Reagents:
Standard AgNO3 solution, silver nitrate, nitric acid or sodium, hydroxide, 0.25M potassium
chromate

Theory:
Chloride in the form of chloride (Cl- ) ion is one of the major inorganic anions in water and
wastewater. The chloride concentration is higher in wastewater than in raw water because sodium
chloride is a common article of diet and passes unchanged through the digestive system (Average
estimate of excretion: 6 g of chlorides/person/day; additional chloride burden due to human
consumption on wastewater: 15 mg/L). Along the sea coast chloride may be present in high
concentration because of leakage of salt water into the sewage system. It also may be increased by
industrial process. In potable water, the salty taste produced by chloride concentration is variable
and depends on the chemical composition of water. Some waters containing 250 mg/L Cl- may
have a detectable salty taste if sodium cation is present. On the other hand, the typical salty taste
may be absent in waters containing as much as 1000 mg/L when the predominant cations are
calcium and magnesium. In addition, a high chloride contents may harm metallic pipes and
structures as well as growing plants. The measured chloride ions can be used to know salinity of
different water sources. For brackish water (or sea water or industrial brine solution), it is an
important parameter and indicates the extent of desalting of apparatus required. It also interferes

21
with COD determination and thus it requires a correction to be made on the basis of amount present
or else a complexing agent, such as HgSO4 can be added. Further, chloride ions are used as tracer
ions in column studies to model fate of different contaminants in soil and liquid media.

Procedure:
1. First make a 0.075M standard AgNO3 solution by mixing 3.0g of silver nitrate with 250ml
of distilled in an Erlenmeyer flask. Set aside for later use.
2. To determine the concentration of chloride, first pipette 10ml of filtered water sample into
a 250ml Erlenmeyer flask and dilute by adding 65ml of distilled water.
3. Test the pH of the diluted water sample with pH test paper. If the pH is not between a pH
of 6 and 8, then use nitric acid or sodium hydroxide to bring the pH to an appropriate level.
4. Then add 1ml of 0.25M potassium chromate to the flask. Rinse and fill a burette with the
standard AgNO3 solution.

Figure 11After adding potassium chromate

5. After that, titrate the water sample by adding the AgNO3 solution slowly while stirring the
sample using a magnetic bar and stir plate.
6. The end point will be indicated by the persistence of a red-brown color through the yellow
solution for about 30 seconds.
7. Repeat the titration two more times and average the amount of AgNO3 used to reach the
endpoint.

22
 Figure 12After titrating against AgNO3

8. Then titrate a blank using the same procedure above. For the blank use distilled water in
place of the environmental water sample.
9. Subtract the volume of AgNO3 for the blank from the average used for the sample. This
volume will be the one used to determine the concentration of Chloride in the water sample.
10. Keep in mind when doing final calculations that the silver and chloride react in a one-to-
one ratio.
Observation and calculation:

For distilled warer:

No. Initial volume(ml) Final volume(ml) Volume used(ml)

1 0.0 1.9 1.9
2 1.9 3.9 2.0
3 3.9 6.0 2.1

Average volume if AgNO3 used = 2.0ml

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For Sample water:

No. Initial volume(ml) Final volume(ml) Volume used (ml)

1 0.0 3.7 3.7
2 3.7 7.2 3.5
3 7.2 11.1 3.9

Average volume of AgNO3 used = 3.7ml

(A × N × 35.45)1000
chloride ion concentration =
Vsample

where:

A = volume of titrant used = 3.7 – 2.0 = 1.7 ml

N = normality of AgNO3 used = 0.01

V sample = 10ml

1.7 × 0.01 × 35.45 × 1000

𝐶ℎ𝑙𝑜𝑟𝑖𝑑𝑒 𝑖𝑜𝑛 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 =
10

𝐶ℎ𝑙𝑜𝑟𝑖𝑑𝑒 𝑖𝑜𝑛𝑠 = 60.265mg/L

Result:
Above calculation shoes that there is 60.265mg of Cl-1 ions are present in 1L of sample water. It
means that there is 60.265ppm of chloride ions are present in industrial waste water.

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 EXPERIMENT# 05
Objectives:
Determine the total ppm of total hardness in water.

Equipment Setup/Apparatus:
Conical flask, Burette, Pipette, Iron stand, Oven.

Reagents:
EDTA solution, Erichrome Black-T, normal buffer solution, water.

Theory:
Hard water is water that has high mineral content (in contrast with "soft water"). Hard water is
formed when water percolates through deposits of limestone, chalk or gypsum which are largely
made up of calcium and magnesium carbonates, bicarbonates and sulfates. Iron oxides or iron
carbonates can give a reddish brown coloration to hard water deposits.

Hard drinking water may have moderate health benefits. It can pose critical problems in industrial
settings, where water hardness is monitored to avoid costly breakdowns in boilers, cooling towers,
and other equipment that handles water. In domestic settings, hard water is often indicated by a
lack of foam formation when soap is agitated in water, and by the formation of lime scale in kettles
and water heaters. Wherever water hardness is a concern, water softening is commonly used to
reduce hard water's adverse effects.

Water Hardness Classification:

Hardness, mg CaCO3/L Hardness
<15 Very soft
15-50 Soft
50-100 Medium hard
100-200 Hard
>200 Very hard

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Permanent Hardness:
The permanent hardness of water is determined by the concentration of multivalent cations in the
water. Multivalent cations are positively charged metal complexes with a charge greater than 1+.
Usually, the cations have the charge of 2+. Common cations found in hard water include Ca2+ and
Mg2+. These ions enter a water supply by leaching from minerals within an aquifer.
Common calcium-containing minerals are calcite and gypsum. A common magnesium mineral
is dolomite (which also contains calcium). Rainwater and distilled water are soft, because they
contain few ions

The following equilibrium reaction describes the dissolving and formation of calcium
carbonate and calcium bicarbonate (on the right):

CaCO3 (s) + CO2 (aq) + H2O (l) ⇌ Ca2+ (aq) + 2 HCO−3 (aq)

The reaction can go in either direction. Rain containing dissolved carbon dioxide can react with
calcium carbonate and carry calcium ions away with it. The calcium carbonate may be re-deposited
as calcite as the carbon dioxide is lost to atmosphere, sometimes forming stalactites and
stalagmites.

Calcium and magnesium ions can sometimes be removed by water softeners.

Permanent hardness (mineral content) is generally difficult to remove by boiling. If this occurs, it
is usually caused by the presence of calcium sulfate/calcium chloride and/or magnesium
sulfate/magnesium chloride in the water, which do not precipitate out as the temperature increases.
Ions causing permanent hardness of water can be removed using a water softener, or ion
exchange column.

Temporary hardness:
Temporary hardness is caused by the presence of dissolved bicarbonate minerals (calcium
bicarbonate and magnesium bicarbonate). When dissolved, these type of minerals yield calcium
and magnesium cations (Ca2+, Mg2+) and carbonate and bicarbonate anions (CO2−3 and HCO−3).
The presence of the metal cations makes the water hard. However, unlike the permanent
hardness caused by sulfate and chloride compounds, this "temporary" hardness can be reduced
either by boiling the water, or by the addition of lime (calcium hydroxide) through the process

26
of lime softening.[8] Boiling promotes the formation of carbonate from the bicarbonate and
precipitates calcium carbonate out of solution, leaving water that is softer upon cooling.

Water Softening:
It is often desirable to soften hard water. Most detergents contain ingredients that counteract the
effects of hard water on the surfactants. For this reason, water softening is often unnecessary.
Where softening is practiced, it is often recommended to soften only the water sent to domestic
hot water systems so as to prevent or delay inefficiencies and damage due to scale formation in
water heaters. A common method for water softening involves the use of ion exchange resins,
which replace ions like Ca2+ by twice the number of mono cations such
as sodium or potassium ions.

Washing soda (sodium carbonate, Na2CO3) is easily obtained and has long been used as a water
softener for domestic laundry, in conjunction with the usual soap or detergent.

Water that has been treated by a water softening may be termed termed softened water. In these
cases the water may also contain elevated levels of sodium or potassium and bicarbonate or
chloride ions.

Procedure:

1. Pipette out 50 ml of water sample in a conical flask, add 5ml of pH 10 buffer solution &
then add 5 drops of Eriochrome black-T indicator.
2. Titrate the wine red colored solution against EDTA solution taken in burette till the color
changes to blue at the end point.
3. Repeat the same titration for 2 times and note the constant burette reading as ‘Y’ ml.
4. Using this value calculate the total hardness of water sample.

27
Figure 14After Adding Eriochrome black-T
indicator. Figure 13After titrating against EDTA

Observation and calculation:

No. Initial volume(ml) Final volume(ml) Volume used(ml)

1. 0.4 5.4 5.0
2. 5.4 10.7 5.3
3. 10.7 15.6 4.9

Average volume of EDTA used = 5.4ml

Using EDTA molarity 0.008M we titerate 10ml of sample by using 5.4 ml of EDTA the
concentration of Ca2+ ions will be:

𝑚𝑜𝑙𝑒𝑠 𝐶𝑎2 + 𝑖𝑜𝑛𝑠 (𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝐸𝐷𝑇𝐴)(𝑚𝑙 𝐸𝐷𝑇𝐴 𝑎𝑑𝑑𝑒𝑑)

=
1𝐿 10𝑚𝑙 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑤𝑎𝑡𝑒𝑟 𝑢𝑠𝑒𝑑

𝑚𝑜𝑙𝑒𝑠 𝐶𝑎2 + 𝑖𝑜𝑛𝑠 (0.0080𝑀)(5.4𝑀𝐿)

= = 0.004𝑀
1𝐿 10𝑚𝑙

Result:

The above calculation shows that there is 0.004M of Ca2+ ions are present in given sample of
industrial water, which shows that 400ppm of CaCO3 hardness is present in water.

28
 EXPERIMENT# 06

Objective:

Estimation of calcium hardness in water sample.

Equipment Setup / Apparatus:

Conical flask, Burette, Pipette, Iron stand, Oven.

Reagents:

Hard Water, EDTA Solution, Murexide Indicator, Buffer Solution.

Theory:

What is calcium hardness in water?

Calcium hardness is a measure of the amount of calcium ions present in the water. Water hardness
is an integral part of the water balance calculation, along with pH, alkalinity, and sometimes TDS
and temperature. Calcium hardness is present in a variety of applications.

General guidelines for classification of waters are: 0 to 60 mg/L (milligrams per liter) as calcium
carbonate is classified as soft; 61 to 120 mg/L as moderately hard; 121 to 180 mg/L as hard; and
more than 180 mg/L as very hard.

Procedure:

1. Take 25 ml of hard water in conical titration flask.

2. Add a few ml of Murexide Indicator into it.
3. Buffer Solution of PH 10 is also added in a quantity of 5-6 ml.
4. Titrate this solution against standard EDTA solution taken in burette while stirring the
flask.
5. The end point is pink color is changed to violet.
6. Then note the reading.
7. In the same way, other readings will be taken.

29
 Figure 16After titration against EDTA
Figure 15After adding Murexide Indicator

Data Analysis:

Volume of water taken = X = 25 ml

No. Initial volume(ml) Final volume (ml) Volume used (ml)

1. 30.3 31.8 1.5
2. 31.8 33.2 1.4
3. 33.2 34.8 1.6
Volume of EDTA used = Y = 1.5ml

0.01M EDTA Solution = 0.01M CaCO3 Solution

1ml of 0.01M EDTA solution = (0.01×100)/1000 grams (CaCO3 in titrated volume of solution)
Then, Calcium Hardness in terms of mg/liter or ppm of CaCO3

0.01 × 100 × 1000000 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐸𝐷𝑇𝐴

𝐶𝑎𝑐𝑖𝑢𝑚 𝐻𝑎𝑟𝑑𝑛𝑒𝑠𝑠 = ×
1000 𝑉𝑜𝑢𝑙𝑚𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟

1.5𝑚𝑙
𝐶𝑎𝑙𝑐𝑖𝑢𝑚 𝐻𝑎𝑟𝑑𝑛𝑒𝑠𝑠 = 1000 = 60𝑝𝑝𝑚
25𝑚𝑙

30
Result:

The calcium hardness of industrial waste water is 60ppm of CaCO3

EXPERIMENT# 07

Objective:

• To observe the phenominan of coagulation and flocculation by adding different amount

of coagulant

Apparatus:

50ml beakers, stirrer, weight balance,

Theory:

Coagulation and Flocculation:

Groundwater and surface water contain both dissolved and suspended particles. Coagulation and
flocculation are used to separate the suspended solids portion from the water. Suspended particles
vary in source, charge, particle size, shape, and density. Correct application of coagulation and
flocculation depends upon these factors. Suspended solids in water have a negative charge and
since they have the same type of surface charge, they repel each other when they come close
together. Therefore, suspended solids will remain in suspension and will not clump together and
settle out of the water, unless proper coagulation and flocculation is used. Coagulation and
flocculation occurs in successive steps, allowing particle collision and growth of floc. This is then
followed by sedimentation (see Sedimentation Chapter). If coagulation is incomplete, flocculation
step will be unsuccessful, and if flocculation is incomplete, sedimentation will be unsuccessful.
Coagulation:

Coagulant chemicals with charges opposite those of the suspended solids are added to the water to
neutralize the negative charges on non-settlable solids (such as clay and color-producing organic
substances). Once the charge is neutralized, the small suspended particles are capable of sticking
together. These slightly larger particles are called microflocs, and are not visible to the naked eye.
Water surrounding the newly formed microflocs should be clear. If not, coagulation and some of

31
the particles charge have not been neutralized. More coagulant chemicals may need to be added.
A high-energy, rapid-mix to properly disperse coagulant and promote particle collisions is needed
to achieve good coagulation. Over-mixing does not affect coagulation, but insufficient mixing will
leave this step incomplete. Contact time in the rapid-mix chamber is typically 1 to 3 minutes.

Flocculation:

Flocculation, a gentle mixing stage, increases the particle size from submicroscopic microfloc to
visible suspended particles. Microfloc particles collide, causing them to bond to produce larger,
visible flocs called pinflocs. Floc size continues to build with additional collisions and interaction
with added inorganic polymers (coagulant) or organic polymers. Macroflocs are formed and high
molecular weight polymers, called coagulant aids, may be added to help bridge, bind, and
strengthen the floc, add weight, and increase settling rate. Once floc has reached it optimum size
and strength, water is ready for sedimentation. Design contact times for flocculation range from
15 or 20 minutes to an hour or more, and flocculation requires careful attention to the mixing
velocity and amount of mix energy. To prevent floc from tearing apart or shearing, the mixing
velocity and energy are usually tapered off as the size of floc increases. Once flocs are torn apart,
it is difficult to get them to reform to their optimum size and strength. The amount of operator
control available in flocculation is highly dependent upon the type and design of the equipment.

Alum:

Alum is one of the most widely used coagulants in the water treatment industry. For water and
wastewater treatment, the coagulants used more frequently are the inorganic salts of aluminum.
When added to water, Al ions hydrolyze rapidly and form a range of metal hydrolysis species.
These cationic species adsorb onto the negatively charged particles and neutralize the charge. In
this mechanism, particles get destabilized and aggregation occurs.

Coagulation depends on:

Coagulation depends on coagulant dosage and also the ph. Almost all of the colloids in water are
negatively charged and because of electrical repulsion they may remain stable. Destabilization
could be made by addition of salts or cations that will interact with negative colloids to neutralize
their charge. Upon hydrolysis, aluminum hydroxide precipitate is formed, this precipitate sweeps

32
the colloidal particles from the suspension and is called the sweep-floc coagulation. Since it does
not involve any charge reversal this is more popularly used in water treatment.

Wastewater Treatment

Physical-chemical treatment of wastewater was widely practiced until the late 19th century, until
the advent of the trickling filter for biological treatment. The early 1970s saw a partial revival of
interest that has continued to the present day, particularly for treatment plants that are overloaded
during peak flow events. The addition of coagulant chemicals to primary clarifiers, or to other
dedicated physical separation processes, is an effective way of reducing the load to downstream
biological processes, or in some cases for direct discharge. This practice is generally referred to as
chemically enhanced primary treatment, or CEPT.

Principal disadvantages that might preclude a wholly physical-chemical solution to wastewater

treatment are the problems associated with the highly putrescible sludgeproduced, and the high
operating costs of chemical addition. However, much of the current interests in physical-chemical
treatment stem from its suitability for treatment under emergency measures; for seasonal
applications, to avoid excess wastewater discharges during storm events; and for primary treatment
before biological treatment, where the above disadvantages become of lesser impact.

CEPT can also be an effective first step for pollution control in developing countries – particularly
in large urban areas that have evolved with sewerage systems but without centralized wastewater
treatment, and have limited financial resources for more complete, but capital intensive biological
treatment options such as activatedsludge systems. Such urban developments also may not have
the areas available for appropriate technology options such as stabilization pond processes.

The efficiency of CEPT, in terms of BOD or COD removal, depends on wastewater characteristics.
With CEPT, one can expect to remove particulate components, together with some portion of the
colloidal components. Therefore, with such a wastewater, it is feasible to achieve removals of more
than: 95-percent TSS; 65-percent COD; 50-percent BOD; 20-percent nitrogen; and 95-percent
phosphorus. In practice, removals may be lower or higher: for example, in warmer climates, with
larger collection systems, and relatively flat sewers, one would expect a higher degree of
hydrolysis of particulate matter resulting in higher soluble fractions, and lower overall removals

33
with CEPT. On the other hand, if the collection system is relatively small, the climate is cold, and
wastewater is relatively fresh, there may be a higher proportion of particulate material, and CEPT
removals could be higher.

Staged coagulation-flocculation can enhance CEPT performance. For example, at primary clarifier
overflow rates of over 6 m/h (3,600 gpd/ft2) during peak flow treatment, TSS and BOD removals
of 80 to 95%, and 58 to 68% were achieved, respectively, using 60 mg/l ferric chloride, followed
by 15 mg/l polyaluminum chloride, followed by 0.5 mg/l anionic polymer. The total reaction time
from the point of ferric chloride addition to entering the primary clarifiers was approximately 8
minutes at peak flow.

Procedure:

1. Take three dry and clean beakers of 50ml and fill them up to 40ml of sample water.
2. Add 0.2g 0.4g and 0.6g Alum in beaker 1, 2 and 3.
3. Give them 5min for flocculation process and allow them to sattle down.

Figure 17After adding different amount of Alum

4. And then filtrate the treated water separately.

34
 Figure 18After filtration

Observation and calculation:

1. In beaker 1 we add 0.5 % Alum by weight

2. In beaker 2 we add 1.0% Alum by weight
3. In beaker 3 we add 1.5% Alum by weight

Result:
When we add 0.5% Alum in beaker it takes longer time to sediment the suspended particals
than 1.0% and 1.0% than 1.5% so it means that if we add more amount of coagulant in
sample water and make it well mixed then the suspended particals sattle down more rapidly
and make the water clean

35
 EXPERIMENT# 08

Objective:

Deter mine the dissolve oxygen, Conductivity and turbidity before and after the addition
of coagulant.

Apparatus:

50ml Beakers, DO Meter, Turbidity Meter, Conductivity Meter.

Reagents:

Alum, Tap Water, Distilled Water, Industrial sample water.

Theory:

Dissolve Oxygen in Water:

The level of dissolved oxygen in water is one of the most important parameters in determining its
quality, because it indirectly indicates whether there is some kind of pollution. Common processes
that pollute surface waters include the discharge of organic matter derived from municipal sewage
or industrial wastes, and runoff from agricultural lots and livestock feedlots. In addition, the release
of warm or hot discharges from industrial cooling towers induces what is known as thermal
pollution. Such discharges directly affect the level of dissolved oxygen in water bodies, which is
crucial for the survival of aerobic organisms and aquatic fauna such as fish; in fact, excessive
pollution has caused massive fish deaths. In the long run, the discharges of organics or of nutrients
favor the accelerated eutrophication or productivity process with algal blooms. As a consequence,
there will be a lowering of the dissolved oxygen content (or DO level) and the “death” of the
aquatic system.

The measurement of the DO is also important to determine whether a water system is

predominantly aerobic or anaerobic, predict the survival of aquatic organisms, and predict whether
aerobic biological processes can take place for transforming the biodegradable organic
contaminants discharged in water. When there is an organic discharge, the DO decreases rapidly
due to the action of the aerobic microorganisms that consume oxygen during the metabolic

36
degradation of organic matter. Consequently, the presence of dissolved oxygen is critical for the
self-cleansing of the water system, and in combination with the presence of CO2, it is also critical
for the determination of the corrosive character of water on materials such as iron and other metals.
The DO depends on water temperature, dissolved salts, atmospheric pressure (and therefore of
altitude), the presence of reducing compounds, suspended matter, and living species. The aquatic
flora and fauna can contribute to the consumption or to the production of oxygen in water. For the
aquatic flora, the photosynthesis process is responsible for the generation of oxygen in the presence
of light; this explains the DO fluctuations during the day/night cycles and in the different seasons.
The presence of microorganisms and biodegradation processes affect the DO level as well. This
can also vary vertically, decreasing in the water column in lakes, large deep rivers, or the ocean
due to stratification. By contrast, in rivers and streams it can vary horizontally along the course of
the river flow increasing where there are waterfalls or rapids, and decreasing in the slow-moving
portions of the river and in those with organic discharges or microbial activity. Since the
dissolution of air in water is an interface mass-transfer phenomenon, the degree of contact and of
mixing with water is also important.

Effects:

Dissolved oxygen (DO) is one of the most important indicators of water quality. It is essential for
the survival of fish and other aquatic organisms. Oxygen dissolves in surface water due to the
aerating action of winds. Oxygen is also introduced into the water as a byproduct of aquatic plant
photosynthesis. When dissolved oxygen becomes too low, fish and other aquatic organisms cannot
survive.

The colder water is, the more oxygen it can hold. As the water becomes warmer, less oxygen can
be dissolved in the water. Salinity is also an important factor in determining the amount of oxygen
a body of water can hold; fresh water can absorb more oxygen than salt water.

Oxygen levels also may be reduced when there are too many bacteria or algae in water
(see Biochemical Oxygen Demand). After the algae complete their life cycle and die, they are
consumed by bacteria. During this decay process the bacteria also consume the oxygen dissolved
in the water. This can lead to decreased levels of biologically available oxygen, in some cases
leading to fish kills and death to other aquatic organisms.

37
Turbidity

Turbidity is the measure of relative clarity of a liquid. It is an optical characteristic of water and is
a measurement of the amount of light that is scattered by material in the water when a light is
shined through the water sample. The higher the intensity of scattered light, the higher the turbidity.
Material that causes water to be turbid include clay, silt, very tiny inorganic and organic matter,
algae, dissolved colored organic compounds, and plankton and other microscopic organisms.

Turbidity makes water cloudy or opaque. The picture to the right shows a U.S. Geological Survey
(USGS) hydrologist sampling highly turbid water in the Colorado River in Arizona. The water
collected in a bottle will be used to find out the turbidity, which is measured by shining a light
through the water and is reported in nephelometric turbidity units (NTU). During periods of low
flow (base flow), many rivers are a clear green color, and turbidities are low, usually less than 10
NTU. During a rainstorm, particles from the surrounding land are washed into the river making
the water a muddy brown color, indicating water that has higher turbidity values. Also, during high
flows, water velocities are faster and water volumes are higher, which can more easily stir up and
suspend material from the stream bed, causing higher turbidities.

Water conductivity

Pure water is not a good conductor of electricity. Ordinary distilled water in equilibrium with
carbon dioxide of the air has a conductivity of about 10 x 10-6 W-1*m-1 (20 dS/m). Because the
electrical current is transported by the ions in solution, the conductivity increases as the
concentration of ions increases. Thus, conductivity increases as water dissolved ionic species.

Procedure:

1. Take 50ml beakers and fill it with sample water.

2. Add 0.5% 1.0% and 1.5% Alum as coagulant in three different beakers filled with waste
water sample.
3. Give them 5min to sellte down all the suspended particals.
4. Filtrate the water sample by using filter paper.

38
5. Now check the dissolve oxygen by using DO meter of these three sample and also for tap
water and distilled water.

Figure 19DO meter

6. Find the tuebidity using turbidity meter TB400.

Figure 20 Turbidity meter

39
 7. Find the Conductivity by using conductivity meter.

Observation and calculation:

Sample of water Turbidity(ntu) DO (mg/L) Conductivity (mS)

Using 0.5% Alum 16.33 0.6
Using 1.0% Alum 16.14 0.6
Using 1.5% Alum 12.55 0.7
Tap water 0.074 0.8
Distilled water 0.066 0.5

Result:

If we add more Alum then the turbidity is low because by adding more alum the water is more
purified by suspended particals and turbidity of distilled water is less than tap water.

Conductivity depends upon the suspended and dissolved ions in the water so if we remove them
then the conductivity becomes low that’s why the conductivity of tap water is more than distilled
water.

40
 EXPERIMENT# 09

Objective:

Determination if BOD and COD of industrial waste water

Apparatus:

pH meter, BOD bottle, BOD incubator, pipette, flask

Reagents:

1. water sample
2. 1N acid and 1N alkali solutions (1 N sulphuric acid is prepared by adding 2.8 ml of conc.
H2SO4 to 100 ml of BOD-free distilled water, whereas 1 N sodium hydroxide is prepared
by adding 4 gm. of NaOH in 100 ml of distilled water
3. Allylthiourea
4. BOD-free distilled water

Theory:

Biological Oxygen Demand (BOD):

Biochemical oxygen demand (BOD) represents the amount of oxygen consumed by bacteria and
other microorganisms while they decompose organic matter under aerobic (oxygen is present)
conditions at a specified temperature.

When you look at water in a lake the one thing you don't see is oxygen. In a way, we think that
water is the opposite of air, but the common lake or stream does contain small amounts of oxygen,
in the form of dissolved oxygen. Although the amount of dissolved oxygen is small, up to about
ten molecules of oxygen per million of water, it is a crucial component of natural water bodies;
the presence of a sufficient concentration of dissolved oxygen is critical to maintaining the aquatic
life and aesthetic quality of streams and lakes.

41
The presence of a sufficient concentration of dissolved oxygen is critical to maintaining the aquatic
life and aesthetic quality of streams and lakes. Determining how organic matter affects the
concentration of dissolved oxygen (DO) in a stream or lake is integral to water- quality
management. The decay of organic matter in water is measured as biochemical or chemical oxygen
demand. Oxygen demand is a measure of the amount of oxidizable substances in a water sample
that can lower DO concentrations.

Certain environmental stresses (hot summer temperatures) and other human-induced factors
(introduction of excess fertilizers to a water body) can lessen the amount of dissolved oxygen in a
water body, resulting in stresses on the local aquatic life. One water analysis that is utilized in
order to better understand the effect of bacteria and other microorganisms on the amount of oxygen
they consume as they decompose organic matter under aerobic (oxygen is present) is the measure
of biochemical oxygen demand (BOD).

Determining how organic matter affects the concentration of dissolved oxygen in a stream or lake
is integral to water-quality management. BOD is a measure of the amount of oxygen required to
remove waste organic matter from water in the process of decomposition by aerobic bacteria (those
bacteria that live only in an environment containing oxygen). The waste organic matter is stabilized
or made unobjectionable through its decomposition by living bacterial organisms which need
oxygen to do their work. BOD is used, often in wastewater-treatment plants, as an index of the
degree of organic pollution in water.

chemical oxygen demand (COD)

The chemical oxygen demand (COD) is a measure of water and wastewater quality. The COD test
is often used to monitor water treatment plant efficiency. This test is based on the fact that a strong
oxidizing agent, under acidic conditions, can fully oxidize almost any organic compound to carbon
dioxide. The COD is the amount of oxygen consumed to chemically oxidize organic water
contaminants to inorganic end products.

The COD is often measured using a strong oxidant (e.g. potassium dichromate, potassium iodate,
potassium permanganate) under acidic conditions. A known excess amount of the oxidant is added
to the sample. Once oxidation is complete, the concentration of organics in the sample is calculated
by measuring the amount of oxidant remaining in the solution. This is usually done by titration,

42
using an indicator solution. COD is expressed in mg/L, which indicates the mass of oxygen
consumed per liter of solution.

The COD test only requires 2-3 hours, while the Biochemical (or Biological) Oxygen Demand
(BOD) test requires 5 days. It measures all organic contaminants, including those that are not
biodegradable. There is a relationship between BOD and COD for each specific sample, but it
must be established empirically. COD test results can then be used to estimate the BOD of a given
sample. Unlike for the BOD test, toxic compounds (such as heavy metals and cyanides) in the
samples to be analyzed do not have an effect on the oxidants used in the COD test. Therefore, the
COD test can be used to measure the strength of wastes that are too toxic for the BOD test. Some
organic molecules (e.g., benzene, pyridine) are relatively resistant to dichromate oxidation and
may give a falsely low COD.

BOD Test Procedures:

To ensure proper biological activity during the BOD test, a wastewater sample:

• Must be free of chlorine. If chlorine is present in the sample, a dichlorination chemical

(e.g, sodium sulfite) must be added prior to testing.
• Needs to be in the pH range of 6.5-7.5 S.U. If the sample is outside this range, then
acid or base must be added as needed.
• Needs to have an existing adequate microbiological population. If the microbial
population is inadequate or unknown, a "seed" solution of bacteria is added along with
an essential nutrient buffer solution that ensures bacteria population vitality.
1. Specialized 300 mL BOD bottles designed to allow full filling with no air space and
provide an airtight seal are used. The bottles are filled with the sample to be tested or
dilution (distilled or deionized) water and various amounts of the wastewater sample are
added to reflect different dilutions. At least one bottle is filled only with dilution water as
a control or "blank."
2. A DO meter is used to measure the initial dissolved oxygen concentration (mg/L) in each
bottle, which should be a least 8.0 mg/L. Each bottle in then placed into a dark incubator
at 20°C for five days.

43
 3. After five days (± 3 hours) the DO meter is used again to measure a final dissolved oxygen
concentration (mg/L), which ideally will be a reduction of at least 4.0 mg/L.
4. The final DO reading is then subtracted from the initial DO reading and the result is the
BOD concentration (mg/L). If the wastewater sample required dilution, the BOD
concentration reading is multiplied by the dilution factor

COD test procedure:

1. Prior to completing the COD test, a series of known standards are prepared using KHP
(potassium hydrogen phthalate). Most wastewater samples will fall in the high range, so
standards of 100, 250, 500 and 1000 mg/L are typically prepared. COD standards can also
be purchased.
2. A COD reactor/heating (150°C) block and a colorimeter are turned on so that both
instruments are allowed to stabilize.
3. Pre-prepared low-range (3-50 ppm) or high-range (20-1500 ppm) vials are selected for the
COD test based on expected results. Both ranges can be used if expected results are
unknown.
4. One vial is marked as a “blank,” and three or four vials are marked with known standard
levels. Two vials are then marked for the wastewater sample to make a duplicate run. Note:
If multiple wastewater samples are being run, at least 10% of samples are duplicated.
5. 2 mL of liquid are added to each vial. In the case of the “blank,” 2 mL of DI water are
added. 2 mL of each standard are added to the corresponding vials. If the wastewater
sample is tested at full strength, then 2 mL is added to the corresponding vial. If dilution is
required, then serial dilutions are performed and 2 mL of the diluted sample are added to
the corresponding vial.
6. Each vial is mixed well and placed into the reactor block for two hours. After two hours,
the vials are removed from the block to a cooling rack for about 15 minutes.
7. The colorimeter is set and calibrated per the specific instructions for that unit (i.e., proper
wavelength, blank and standards) and each vial is placed in the unit and the COD
concentration read.
8. If the sample was diluted, the corresponding multiplication is made

44
References:

1. "Hard water". National Groundwater Association. Retrieved 28 June 2019.

2. World Health Organization Hardness in Drinking-Water, 2003 c Weingärtner, Herman]
(December 2006). Ullmann's Encyclopedia of Industrial
3. Chemistry - Water. Weinheim: Wiley–VCH
4. lair N. Sawyer; Perry L. McCarty; Gene F. Parkin (2003). Chemistry for Environmental
5. Engineering and Science (5th ed.). New York: McGraw-Hill. ISBN 978-0-07-248066-
6. Goldman, Charles R.; Horne, Alexander J. (1983). Limnology. McGraw-Hill. pp. 88, 267.
ISBN 0-07-023651-8.
7. Jump up to: a b Reid, George K. (1961). Ecology of Inland Waters and Estuaries. Van
Nostrand Reinhold. pp. 317–320.
8. Norton, John F. Standard Methods for the Examination of Water and Sewage 9th Ed.
(1946) American Public Health Association p.139
9. Urquhart, Leonard Church Civil Engineering Handbook 4th Ed. (1959) McGraw-Hill p. 9–
40

45