Experiment # 1: Determination of Total Solid in Waste Water Sample Total Solids
Experiment # 1: Determination of Total Solid in Waste Water Sample Total Solids
Total Solids
ny solid residue which is left behind after evaporation and drying the water at 103 to 105C.
ENVIRONMENTAL SIGNIFICANCE
1. Water and Waste water:-
For drinking water total dissolved solids should be less than 1000 mg/l. There should
not be total suspended solids in the drinking water. If TSS are present and TDS are
greater than 1000 mg/l then we should treat the water.
For waste water total dissolved solids should be less than 3500 mg/l. Total suspended
solids should be less than 150 mg/l.
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2. Aquatic life:-
Total solids also affect the aquatic life. It has harmful effects on the aquatic life. Due to
total solids an algal layer is formed on the surface of the water. This layer does not
permit to pass the sunlight. Due to low penetration of sunlight no oxygen is delivered to
the aquatic life.
3. Corrosion in pipes:-
Total solids also causes the corrosion in pipes. Total solids that cause corrosion
are different types of salts like salts of iron. It produces blockage of pipes that disturb
the water distribution system. It can also make the water polluted.
APPARATUS
China dish.
A Water Bath.
Desiccator.
An Oven.
Weight measuring instrument.
Water Sample (UET TAXILA).
PROCEDURE
2
Take 50 ml water in a pre-weighted china dish . Pre-weighted china dish is a china dish
that weight has been calculated before. Evaporate the water sample in the oven at 103 to
105 *C for 1hr. the oven should be pre heated to ensure complete draying. after draying
take the dish out of the oven and cool at a room temperature in desiccator. Weight the
dish.
CALCULATIONS
Initial weight of China Dish=W1=51.043 g
PRECAUTIONS
Non-representative particles such as leaves, sticks, fish and lumps of fecal matter should
be excluded from the sample if it is determined that their inclusion is not desired in the
final result.
Floating oil and grease, if present, should be included in the sample and dispersed by a
blender device before sub sampling.
Highly mineralized water containing significant concentration of calcium magnesium,
chloride and sulphate may be hygroscopic. Hence prolonged drying, desiccation and
rapid weighing.
EXPERIMENT # 2
Determination of total dissolved solids in waste water.
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THEORY
They can also be referred to as the solid materials which are completely dissolved in water and
are filterable in nature. It is defined as the residue upon evaporation of filterable sample.
Total dissolved solids (TDS) comprise inorganic salts and small amounts of organic matter that
are dissolved in water. The principal constituents are usually the cations calcium, magnesium,
sodium and potassium and the anions carbonate, bicarbonate, chloride, sulphate and, particularly
in groundwater, nitrate (from agricultural use).
ENVIRONMENTAL SIGNIFICANCE
1. Water and Waste water:-
For drinking water total dissolved solids should be less than 1000 mg/l. There
should not be total suspended solids in the drinking water. If TSS are present and TDS
are greater than 1000 mg/l then we should treat the water.
For waste water total dissolved solids should be less than 3500 mg/l. Total
suspended solids should be less than 150 mg/l.
2. Aquatic life:-
Total solids also affect the aquatic life. It has harmful effects on the aquatic life. Due to
total solids an algal layer is formed on the surface of the water. This layer does not
permit to pass the sunlight. Due to low penetration of sunlight no oxygen is delivered to
the aquatic life.
3. Corrosion in pipes:-
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Total solids also causes the corrosion in pipes. Total solids that cause corrosion are
different types of salts like salts of iron. It produces blockage of pipes that disturb the
water distribution system. It can also make the water polluted.
APPARATUS
Weight Balance
Oven
Desiccator
China Dish
Vacuum Filtration Assembly
Conical Flash
PROCEDURE
Connect the clean and dry filter flask to the filter holder. Then place the 47mm filter paper in the
filter holder with wrinkled surface upward. after that mix the sample well and take 50ml in
measuring cylinder filter the above 50ml of sample. Apply vaccume for 2-3 min after the sample
passed then disconnect the vaccume.
Pore the filtrate in pre weighed china dish and dry at 180*C. after draying it cool at in desicator.
5
ml of sample (ml)
CALCULATIONS
Initial weight of China Dish=W1=55.104 grams
RESULT
The total dissolved solids in the given sample of waste water have been determined to be
PRECAUTIONS
Water or wastewater samples which contain high concentration of calcium, chloride,
magnesium or sulphate can rapidly absorb moisture from the air. Such sample may need
to be dried for a longer period of time in order to achieve a reasonable constant weight.
We should be aware that prolonged drying may result in loss of constituents, particularly
nitrates and chlorides.
Great care must be taken when taking the china dish/Petri dish out of the oven, as it is
usually very hot. The use of dish tongs is preferred.
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EXPERIMENT # 3
Determination of total suspended solids in waste water.
THEORY
The total suspended solids refers to the solid material in water or wastewater sample, which is
retained by a filter of 2.0 µm (or smaller) nominal size under specified conditions.
They can also be referred to as the solid materials which are not dissolved in water and are
non-filterable in nature.
They can be further classified as Settleable and Non-Settleable depending upon their settling
velocities.
ENVIRNMENTAL SIGNIFICANCE
1. Water and Waste water:-
For drinking water total dissolved solids should be less than 1000 mg/l. There
should not be total suspended solids in the drinking water. If TSS are present and TDS
are greater than 1000 mg/l then we should treat the water.
For waste water total dissolved solids should be less than 3500 mg/l. Total
suspended solids should be less than 150 mg/l.
2. Aquatic life:-
Total solids also affect the aquatic life. It has harmful effects on the aquatic life. Due to
total solids an algal layer is formed on the surface of the water. This layer does not
permit to pass the sunlight. Due to low penetration of sunlight no oxygen is delivered to
the aquatic life.
3. Corrosion in pipes:-
Total solids also causes the corrosion in pipes. Total solids that cause corrosion are
different types of salts like salts of iron. It produces blockage of pipes that disturb the
water distribution system. It can also make the water polluted.
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APPARATUS
Filtration Assembly
Patri Dish
Oven
Desiccator
Filter Paper
PROCEDURE
Take pre weight filter paper and then set it on filtration assembly after that pass
50ml water trough it by applying vacuum after that when all water passed through
it take it in china dish dish and place in oven at 103-105*C tem for 1 hr after that
weight it again.
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Con. of Total Suspended Solids ( mgL )= mlWx1000 x 1000
of sample used
RESULTS
The total suspended solids in the given sample of water have been determined to be 120 mg/L.
PRECAUTIONS
Great care must be taken when taking the china dish/Petri dish out of the oven, as it is
usually very hot. The use of dish tongs is preferred.
Forceps must always be used for handling the filter paper and it should never be handled
directly by hand.
The filter paper must be allowed to sufficiently cool to room temperature in a desiccator
to get an accurate measurement of weight.
EXPERIMENT # 4
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Determination of settleable solids in waste water sample
THEORY
The term "settleable solids" refers to material of any size that will not remain suspended or
dissolved in a holding tank not subject to motion, and excludes both TDS and TSS.
Settleable solids are defined as the quantity of solids that will settle out of suspension in a
water-solid mixture within a defined amount of time (one hour) and can be determined by
volumetric and gravimetric measurements.
Settleable solids may include larger particulate matter or insoluble molecules. The ability for
solids to settle out of suspension is a function of the particle density, shape, and size.
ENVIRONMENTAL SIGNIFICANCE
Total suspended solids are a significant factor in observing water clarity. The more solids
present in the water, the less clear the water will be. Some suspended solids can settle out into
sediment at the bottom of a body of water over a period of time. Heavier particles, such as
gravel and sand, often settle out when they enter an area of low or no water flow. Although this
settling improves water clarity, the increased silt can smother benthic organisms and eggs.
Settleable solids are also known as bedded sediments, or bed load. These sediments can vary
from larger sand and gravel to fine silt and clay, depending on the flow rate of water. Sometimes
these sediments can move downstream even without rejoining the suspended solids
concentration. When settleable solids are moved along the bottom of a body of water by a strong
flow, it is called bed load transport.
APPARATUS
Imhoff cone with stand
Glass rod for stirring
PROCEDURE
1. Fill an imhoff cone to 1 liter mark with a well mixed sample.
2. Provide settling for 45 minutes than gently agitate the sample near the side of cone with
the help of glass rod.
3. Provide 15 min more settling.
4. Record the volume of settleable solids in the cone as (mL/L)
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Figure 4.1: Settling of Solids in imhoff cone
RESULTS
The total settleable solids in the given sample of water have been determined to be 5 mL/L.
PRECAUTIONS
Remember to stir the water sample in the Imhoff cone after 45 minutes of settlement,
gently so that the already settled solids are not suspended.
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Do not disturb the Imhoff cone during the course of the test, except only once as
specified in the above procedure.
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EXPERIMENT # 5
To determine the Dissolved oxygen in waste water sample by azide
modification of winklers method.
THEORY
The term Dissolved Oxygen is used to describe the amount of oxygen dissolved in a unit volume
of water.
The dissolved oxygen content of water is influenced by the source, raw water temperature,
treatment and chemical or biological processes taking place in the distribution system.
The presence of oxygen in water is a good sign. Depletion of dissolved oxygen in water supplies
can encourage the microbial reduction of nitrate to nitrite and sulfate to sulfide.
Hence, analysis of dissolved oxygen is an important step in water pollution control and
wastewater treatment process control. There are various methods available to measure Dissolved
Oxygen, which we will discuss in detail.
In a healthy body of water such as a lake, river, or stream, the dissolved oxygen is about 8 parts
per million. The minimum DO level of 4 to 5 mg/L or ppm is desirable for survival of aquatic
life.
Now imagine that a source of oxygen demanding wastes, such as feed lot, a paper mill or a food
processing plant, is built besides the river. The facility begins operating and discharging wastes
into the river.
This increases the BOD and affects the concentration of DO in the waters downstream.
The wastes serve as the food for certain aerobic bacteria. As it moves downstream, the conc. of
bacteria increases. Because these bacteria remove oxygen from water, their population increase
causes a decline in the amount of DO.
Beyond certain point, most of the wastes break down. The conc. of DO rises as the river
recovers oxygen from the atmosphere and aquatic plants. Thus DO test is the basis for BOD test
which is an important parameter to evaluate organic pollution potential of a waste.
It is necessary for all aerobic biological wastewater treatment processes to control the rate of
aeration.
ENVIRMENTAL SIGNIFICANCE
1. Existence of aquatic life
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DO test will tell us whether aquatic life exist in water or not. DO test is used to control
stream pollution, to maintain the favoratable condition for aquatic life.
DO test tells us whether aerobic condition occurs in the stream or an aerobic condition. It is
used to maintain the aerobic condition in the streams.
3. Insulation in boilers
Boilers are used to provide heat to the water. DO present in water will cause precipitation
that will stick into the boiler and causes insulation which reduces the energy of water.
4. Evaluation of Strength
The primary source of oxygen for a pond is from microscopic algae or submerged plants. In
the presence of sunlight, these produce oxygen through photosynthesis and release this
oxygen into the pond water. At night and on very cloudy days, algae and submerged plants
remove oxygen from the water for respiration. During daylight hours plants normally
produce more oxygen than they consume, thus providing oxygen for the fish and other
organisms in the pond.
2) Atmosphere
There is a higher concentration of oxygen in the atmosphere (air) than water; oxygen
diffuses into the surface of the lake from the atmosphere.
P ∝ DO
2) Temperature
1
T∝
DO
3) Salinity
1
S∝
DO
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PRINCIPLE
The test depends upon the fact that oxygen oxidize Mn+2 ion to a higher state of valency. Under
alkaline condition, magnese at higher state of valency is capable of oxidizing iodide ion to
iodine under acidic condition .Thus the amount of iodine released is equal to dissolved oxygen
actually present.
The iodine is measured with titrant sodium thiosulphate solution and interpretant in terms of
DO.
METHODS TO DETERMINE DO
1) DO meter test
2) Winklers Method
3) Azide Modification of Winklers Method
WINKLER REACTIONS
1
N 2 O 2+ O 2 + H 2 O → 2 N O−1 +¿ ¿
2 +2 H
2
+¿ ¿
Na N 3 + H +¿ → H N +N a
3 ¿
+¿ →N 2+ N 2 O + H2 O¿
H N 3+ N O −¿+
2
H ¿
APPARATUS
Titration Assembly
Pipette
Burette
Titration flask
BOD bottle
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REAGENTS
Manganese Sulphate (MnSO4)
Alkali Azide (NaN3)
Conc. Sulphuric Acid (H2SO4)
Starch Indicator
0.025N Sodium Thiosulphate (Na2S2O3)
PROCEDURE
1) Collect the sample in 300ml BOD bottle taking special care to avoid adding air to the
liquid been collected.
2) Fill the bottle completely and add stopper.
3) Remove BOD bottle stopper and add 1 ml of manganese sulphate to it and mix it
uniformly with the help of pipette.
4) Add 1 ml of alkaline potassium iodide sodium azide solution in water.
5) If white precipitates appear than there is no dissolved oxygen and if brown precipitates
occurs it indicates DO.
6) Shake the bottle upside down 20 times.
7) Allow the precipitates to settle down.
8) When the precipitates moves two inch below the stopper then add 1 ml sulphuric acid.
9) Again shake the bottle to dissolve the precipitates.
10) Now add 200 ml sample from the bottle in titration flask, then titrate it with sodium
thiosulphate (0.025N),till light yellow color appear and add 1 ml of starch.
11) Further titrate till the appearance of colorless solution.
12) Note the volume and put it in the formula.
Volume of titrant used × N × Eq . wt . of oxygen × 1000
DO ( mg/ L )=
Volume of sample used∈ml
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Figure 5.1: Change of colour from light yellow to colourless
Where
RESULTS
The dissolve oxygen found in the waste water is 1.5 mg/L
PRECAUTIONS
Make sure there are absolutely no air bubbles in the BOD bottles.
Perform titration slowly drop-by-drop, noting the color carefully, otherwise the sample
may have to be discarded.
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EXPERIMENT # 6
To determine the biochemical oxygen demand in the wastewater sample.
THEORY
The biochemical oxygen demand determination is a chemical procedure for determining the
amount of dissolved oxygen needed by aerobic organisms in a water body to break the organic
materials present in the given water sample at certain temperature over a specific period of time.
BOD of water or polluted water is the amount of oxygen required for the biological
decomposition of dissolved organic matter to occur under standard condition at a standardized
time and temperature. Usually, the time is taken as 5 days and the temperature is 20°C.
The test measures the molecular oxygen utilized during a specified incubation period for the
biochemical degradation of organic material (carbonaceous demand) and the oxygen used to
oxidize inorganic material such as sulfides and ferrous ion. It also may measure the amount of
oxygen used to oxidize reduced forms of nitrogen (nitrogenous demand).
ENVIROMENTAL SIGNIFICANCE
1) Existence of aquatic life
DO test will tell us whether aquatic life exist in water or not. DO test is used to control
stream pollution, to maintain the favoratable condition for aquatic life.
DO test tells us whether aerobic condition occurs in the stream or an aerobic condition. It is
used to maintain the aerobic condition in the streams.
3) Insulation in boilers
Boilers are used to provide heat to the water. DO present in water will cause precipitation
that will stick into the boiler and causes insulation which reduces the energy of water.
4) Evaluation of Strength
Efficiency of any treatment plant can be judged by considering influent BOD and the effluent
BOD and so also the organic loading on the unit.
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Application of the test to organic waste discharges allows calculation of the effect of the
discharges on the oxygen resources of the receiving water. Data from BOD tests are used for the
development of engineering criteria for the design of wastewater treatment plants.
Ordinary domestic sewage may have a BOD of 200 mg/L. Any effluent to be discharged into
natural bodies of water should have BOD less than 30 mg/L.
This is important parameter to assess the pollution of surface waters and ground waters where
contamination occurred due to disposal of domestic and industrial effluents.
The determination of BOD is used in studies to measure the self-purification capacity of streams
and serves regulatory authorities as a means of checking on the quality of effluents discharged to
stream waters.
The determination of the BOD of wastes is useful in the design of treatment facilities.
It is the only parameter, to give an idea of the biodegradability of any sample and self-
purification capacity of rivers and streams.
The BOD test is among the most important method in sanitary analysis to determine the
polluting power, or strength of sewage, industrial wastes or polluted water.
It serves as a measure of the amount of clean diluting water required for the successful disposal
of sewage by dilution.
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2) Domestic waste water: - Waste water from domestic use. It is totally organic ,no need for
seeding.
APPARATUS
Titration Assembly
Pipette
Burette
Titration flask
BOD bottles
Incubator
Figure 6.1: Samples in BOD bottles Figure 6.2: Reagents (MnSO4 and Azide)
REAGENTS
Manganese Sulphate (MnSO4)
Alkali Azide (NaN3)
Conc. Sulphuric Acid (H2SO4)
Starch Indicator
0.025N Sodium Thiosulphate (Na2S2O3)
PROCEDURE
1) It is important to know the source of water.
2) Take 9 BOD bottles, note their numbers and arrange them in three groups.
3) Fill each bottle with the dilution water.
4) Add 2ml of domestic waste water in first group of bottle, 5ml in second group of bottle
and 10 ml in third group of bottle.
5) Completely fill the bottle with dilution water and add stopper.
6) Take one bottle from each group and measure its DO.
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7) Place the remaining 6 bottles in incubator at 20 C for 5 days and measure its DO after 5
days again.
8) After 5 days consider correct which gives oxygen depletion at least 2mg/L and which
have at least DO of 0.5 mg/L
9) Calculate the BOD by using formula
1
BOD=( DO ¿ ¿ 0−DO5 ) ¿
P
Volume of sample used
P=
Volume of total sample
P=2/300 =6.6x10^-3
PRECAUTIONS
Make sure there are absolutely no air bubbles in the BOD bottles.
Perform titration slowly drop-by-drop, noting the color carefully, otherwise the sample
may have to be discarded.
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EXPERIMENT # 7
THEORY
The chemical oxygen demand (COD) test is commonly used to indirectly measure the amount of
organic compounds in water. Most applications of COD determine the amount of organic
pollutants found in surface water (e.g. lakes and rivers), making COD a useful measure of water
quality. It is expressed in milligrams per liter (mg/L), which indicates the mass of oxygen
consumed per liter of solution.
COD is the measurement of the amount of oxygen in water consumed for chemical oxidation of
pollutants.
COD determines the quantity of oxygen required to oxidize the organic matter in water or waste
water sample, under specific conditions of oxidizing agent, temperature, and time.
ENVIRNMENTAL SIGNIFICANCE
COD values are particularly important in the surveys designed to determine and control the
losses to sewer systems.
The ratio of BOD to COD is useful to assess the amenability of waste for biological treatment.
Ratio of BOD to COD greater than or equal to 0.8 indicates that wastewater highly polluted and
amenable to the biological treatment.
COD can be related to TOC, however, does not account for oxidation state of the organic matter.
BOD value is always lower than COD value. For domestic and some industrial wastewater,
COD value is about 2.5 times BOD value.
APPARATUS
COD Digester
Burette & Burette stand
COD Vials with stand
250 mL conical flask
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Pipettes
Pipette bulb
Tissue papers
Wash Bottle
REAGENTS
Potassium dichromate
Sulfuric acid
Ferrous ammonium sulphate
Silver sulphate
Mercury sulphate
Ferroin indicator
Organic free distilled water
PROCEDURE
1. Place 50 ml sample in 500ml flask.
2. Add 1g mercury sulphate to avoid interference.
3. Add slowly 5ml of sulphuric acid to dissolve mercury sulphate.
4. Add 25ml, 0.25N potassium dichromate solution and mix it properly.
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5. Attach the flask to the condenser and add 70ml sulphuric acid through open end of
condenser. Reflux the mixer for 2 hrs and dilute it with almost twice of its volume with
distilled water.
6. Add indicator that will blue green color.
7. Titrate the sample with ferrous aluminum sulphate till the appearance of reddish color.
8. Repeat the procedure for blank.
9. Apply the following formula:
RESULT
The amount of COD found in the waste water sample is 28(mg/L).
PRECAUTIONS
Chlorides are quantitatively oxidized by dichromate and represent a positive
interference. Mercuric sulfate is added to the digestion tubes to complex the chlorides
so that it does not interfere in the determination.
Traces of organic material either from the glassware or atmosphere may cause a
positive error. Extreme care should be exercised to avoid inclusion of organic materials
in the distilled water used for reagent preparation or sample dilution.
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