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Dr.S.Sreedhar Reddy
Assistant Professor
2009-10
Introduction to Water and wastewater Laboratory
Introduction:
In the next several experiments, chemical characterization of water and wastewater
will be done. Different tools, materials and equipment will be used in order to
perform such task. Various chemicals such as buffer solutions and colorimetric
indicators as well as basic techniques like preparing primary and secondary standard
solutions, titration and pH measurements are essential for any person that will use
this facility. In any analytical laboratory it is essential to maintain stocks of solutions
of various reagents: some of these will be of accurately known concentration
(standard solutions) and correct storage of such solutions is imperative. Primary
standards are usually salts or acid salts of high purity that can be dried at some
convenient temperature without decomposing and that can be weighed both at high
degree of accuracy. Secondary standards are solutions that have been standardized
against primary standards.
Objectives:
1. To become familiar with the terminology, various materials and chemicals
used in the environmental engineering laboratory.
2. To prepare primary and secondary standards and to understand the principles
involved in their preparation.
Materials:
Analytical balance, 250-ml flask, pH meter, sodium carbonate, methyl orange
indicator, standard buffers, sulfuric acid, magnetic stirrer, volumetric flasks, funnel,
burette (50 ml), and beakers.
Experimental Procedure:
1. Prepare one liter of standard 0.02N Na2CO3 by dissolving 1.06g anhydrous
reagent grade Na2CO3, (dried at1030C for 4 hrs), in distilled water.
2. Mount a 50 ml burette and fill it to the mark with the pre-prepared acid
solution.
3. Take 50 ml of Na2CO3 solution in a flask, add 5 drops of methyl orange
indicator and place on a magnetic stirrer.
4. Add acid slowly while stirring till orange color turns to pink
5. Check the pH of the solution after titration is completed which should be
approximately 4.3
6. Record the volume of acid used.
7. Repeat titration two more times and calculate average volume of acid used.
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Calculations:
Calculate the normality of the sulfuric acid (H2SO4).
Introduction:
The concentrations of the various solids that exist in water and wastewater are
important indicators of their quality. Solids present in water and wastewater can be
broken into two categories, suspended and dissolved solids (non-filterable and
filterable, respectively). Each of the aforementioned categories is also divided into
organic (volatile) and inorganic (non-volatile) constituents. The processes that are
used to separate the different solid categories are filtration and combustion.
Total Solids is the term applied to the material residue left in the vessel after
evaporation of a sample and its subsequent drying in an oven at a defined
temperature (103-1050C). Total suspended solids refer to the non-filterable residue
retained by a standard filter disk and dried at 103-1050C. Total dissolved solids refer
to the filterable residue that passes through a standard filter disk and remain after
evaporation and drying to constant weight at 103- 1050C.
Objective:
To use the principles of gravimetric analysis to characterize the quality, in terms of
solids concentrations, of three types of water, namely: tap water, drinking water, and
secondary effluent.
Materials:
Porcelain dish (100 ml), steam bath, drying oven, muffle furnace, desiccator, Gooch
crucible, analytical balance, glass fiber filter disk, filtration apparatus, pipettes,
measuring cylinders.
Experimental procedure:
a) Total Solids
1. Ignite a clean evaporating dish at 5500C in a muffle furnace for 1 hr.
2. Cool the dish, weigh and keep it in a desiccator.
3. Transfer carefully 50 ml of sample into the dish and evaporate to dryness on a
steam bath.
4. Place the evaporated sample in an oven adjusted at 1030C and dry it for 1 hr.
5. Repeat drying at 1030C till constant weight is obtained.
6. Determine the total solids with the following formula:
3
b) Total suspended solids:
1. Place a filter disk on the bottom of a clean Gooch crucible.
2. Pour 20 ml distilled water and apply vacuum. Repeat the process two more
times.
3. Remove crucible to an oven and dry it for 1 hr at 1030C.
4. After drying, the crucible is kept in a desiccator.
5. Weigh the crucible and place it on a suction unit.
6. Pour 25 ml of sample. Wash pipette with distilled water and pour the washing
also into the crucible.
7. After filtration, dry the crucible at 1030C for 1 hr
8. Weigh till constant weight is obtained.
9. Determine the total suspended solids with the following formula
Report:
In addition to tables showing all experimental results, consider the following points
while preparing your report:
1. Compare the TS, TSS and TDS for the three samples.
2. Describe the results using a mass balance approach.
3. What sources of errors that could affect the accuracy of your results
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Experiment # 2: pH
Aim:
Estimation of the pH value of given water sample
Theory:
The concept of pH was first introduced by Danish chemist Søren Peder Lauritz
Sørensen at the Carlsberg Laboratory in 1909. It is unknown what the exact definition
of p is. Some references suggest the p stands for “Power”, others refer to the
German word “Potenz” (meaning power in German), and still others refer to
“potential”. Jens Norby published a paper in 2000 arguing that p is a constant and
stands for “negative logarithm” which has also been used in other works. H stands
for Hydrogen. Sørensen suggested the notation "PH" for convenience, standing for
"power of hydrogen", using the cologarithm of the concentration of hydrogen ions in
solution, p[H] Although this definition has been superseded p[H] can be measured if
an electrode is calibrated with solution of known hydrogen ion concentration.
Pure water is said to be neutral. The pH for pure water at 25 °C (77 °F) is close to 7.0.
Solutions with a pH less than 7 are said to be acidic and solutions with a pH greater
than 7 are said to be basic or alkaline. pH measurements are important in medicine,
biology, chemistry, food science, environmental science, oceanography and many
other applications.
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Materials:
pH meter, Buffer solutions of known pH, normally 4.0 and 9.2 and glassware
Experimental Procedure:
Result:
Discussion:
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Experiment # 3: Odor (Threshold Odor)
Aim: Determination of threshold odor of given water sample
Theory: Taste and odor in drinking water are two of the most widespread causes of
customer complaints. Although there are no associated health effects, the extensive
public relations difficulties resulting from taste and odor make it important to treat
these problems.
Treatment involves the implementation of a taste and odor control program, which
should be found at every treatment plant. Under some circumstances, this program
may be as simple as routinely monitoring for taste and odor problems and
performing preventive maintenance on the system. In other cases, treatment is
more complex and can involve special equipment to treat the taste and odor
problems.
Taste and odor can enter water in a variety of manners. Surface water sources can
become contaminated through algal blooms or through industrial wastes or domestic
sewage introducing taste- and odor-causing chemicals into the water. Groundwater
supplies can be afflicted with dissolved minerals, such as iron and manganese, which
enter the water when it passes through rocks underground. Tastes and odors can
also enter either type of water in the raw water transmission system and in the
treatment plant due to algal growths, accumulated debris and sludge, or disinfection
byproducts. The distribution system can have many of the same causes of taste and
odor mentioned above, with the addition of problems resulting from cross-
connections and low flow zones.
An integral part of any taste and odor control program is testing the water for taste
and odor problems. The two methods used for these tests - the Threshold Odor Test
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and the Flavor Profile Analysis - are far more subjective than the methods used to
test other water characteristics since both the Threshold Odor Test and the Flavor
Profile Analysis depend on human perception of the taste and odor in the water.
However, despite the difficulty of performing the tests objectively, they still provide
valuable information which can help the operator determine what is causing the taste
or odor problem, how concentrated the problematic chemical is, and how the
problem should be treated.
The Threshold Odor Test is used to determine the amount of odor found in water.
During the procedure, the water being tested is diluted with odor-free water and is
smelled. The dilutions continue until no odor can be discerned. The last dilution at
which odor is detected determines the Threshold Odor Number (TON), which is a
measure of the amount of odor in the water. If several people independently perform
the Threshold Odor Test, the averaged TON can be relatively accurate.
While the Threshold Odor Test is used to determine the concentration of odor-causing
problems in water, the Flavor Profile Analysis can be used to determine which
tastes and odors are present in water. This test uses a panel of trained judges who
taste the water and list which tastes they can detect. Since the tastes present are
described carefully, the Flavor Profile Analysis can be helpful in determining which
chemicals are at the root of the problem.
These tests can be performed to find the source of a particular problem or as part of
routine monitoring. To find the source of a problem, the water should be tested at
various locations, from the source water to the customer's tap. In contrast, routine
monitoring can be less intensive but requires good record-keeping. Past records can
help the operator predict seasonal variations in taste and odor problems so that he
can prevent problems before they reach the customer. Records of past treatment
methods can make it much easier to determine which treatment methods will be
effective during current outbreaks.
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water. Prepare flasks for the final test according to the volume of sample in the jar
that first has a detectable odor.
2.8 mL → Intermediate dilution
12 mL → 12 mL, 8.3 mL, 5.7 mL, 4.0 mL, and 2.8 mL
50 mL → 50 mL, 35 mL, 25 mL, 17 mL, and 12 mL
200 mL → 200 mL, 140 mL, 100 mL, 70 mL, and 50 mL
Add the amounts of sample water indicated to five 500 mL flasks. Next, add odor-free
water to bring each flask to a total volume of 200 mL. Include two blanks (flasks with
200 mL of odor-free water) in the series of samples near the expected threshold for a
total of seven samples. Have a group of testers smell each flask, beginning with the
smallest concentration of sample water. Record the volume of sample water in the
first flask an odor is detected by each tester. Compute the TON using this equation:
Where A = the volume of sample water and B = the volume of odor-free water. Since
A + B is always going to equal 200 mL, the calculation can be restated as:
Usually a number of testers are involved in determining odor for a particular sample
due to the fact that people’s olfactory senses are not uniform. Instead of finding the
arithmetic mean (average) of different TON values, the geometric mean is calculated.
The formula for this process is:
In this formula, each “X” value is a TON and “n” is the total number of TON values.
Model Calculation:
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Results and Calculations:
Conclusions:
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Experiment # 4: Acidity
Theory: The acidity of water is a measure of its capacity to neutralize bases. Acidity
of water may be caused by the presence of uncombined carbon dioxide, mineral
acids and salts of strong acids and weak bases. It is expressed as mg/L in terms of
calcium carbonate. Acidity is nothing but representation of carbon dioxide or
carbonic acids. Carbon dioxide causes corrosion in public water supply systems.
Reagents:
1. Methyl orange indicator
2. Phenolphthalein indicator
3. N/50 Sodium hydroxide solution
Procedure:
1. Place 100 ml of water in a conical flask and add to it one drop of methyl
orange indicator.
2. If it gives an orange red color, mineral acidity is present.
3. Titrate it with N/50 Sodium hydroxide solution to a yellow end point.
4. Note the amount of N/50 Sodium hydroxide solution consumed in ml.
5. In another flask place 100 ml of water and add 0.5 ml of Phenolphthalein
indicator.
6. If it does not give any color, titrate with N/50 Sodium hydroxide solution to
light pink end point.
7. If Phenolphthalein gives a pink color on addition in the sample, acidity is not
available.
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Conclusions:
Experiment # 5: Alkalinity
Aim: To measure the concentration of the various species that
contributes to alkalinity in different types of water.
Materials:
Burette (50 ml), Porcelain dish, Magnetic stirrer and rod, Beaker (150
ml), Pipette, Measuring cylinder (100 ml), pH meter, 0.02N Sulphuric
acid, Methyl Orange indicator, Phenolphthalein indicator.
Experimental procedure:
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For different water samples, the following procedures should be carried
out to determine the total alkalinity and the contributing species.
Indicator Method:
1. Pipette exactly 50 ml of sample into a glass beaker or porcelain
dish and drop in a magnetic rod.
2. Mount a 50 ml burette and fill it to the mark with 0.02N sulphuric
acid solution.
3. Add 5 drops of Phenolphthalein indicator to the sample. If the
solution turns pink, add acid slowly till pink color disappears.
Record the volume of acid in milliliters as P.
4. Add 5 drops of Methyl Orange indicator to the same sample at
the end of the first titration and add 0.02N sulphuric acid slowly
till orange color turns to pinkish yellow. Record this volume as M.
Then, T = P+M.
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Record the titration data in the following table:
Sample
Conclusions:
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Experiment # 6: Hardness
Aim: To determine the total hardness as well as calcium and magnesium of raw
water and treated water samples using EDTA titrimetric method.
Materials:
Burette (50 ml), porcelain dish, magnetic stirrer and rod, pipette, measuring cylinder
(100 ml), ammonia buffer solution, sodium hydroxide solution, Eriochrome black T
indicator, Murexide ( ammonium purpurite), EDTA, raw water sample, treated water
sample.
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Experimental procedure:
For different water samples, the following procedure should be carried out to
determine the total, calcium and magnesium hardness.
1. Pipette exactly 25 ml of raw water sample into a porcelain dish and drop in a
magnetic rod.
2. Mount a 50 ml burette and fill it to the mark with 0.01M EDTA solution.
3. Add 1-2 ml of ammonia buffer, 0.2g Eriochrome Black T indicator.
4. Start adding slowly 0.01M EDTA solution till the color of the solution changes
from wine red to blue. Record the volume of EDTA solution and calculate total
hardness using the following formula:
5. Add 1-2 ml sodium hydroxide buffer and 0.2 g murexide indicator into 25 ml
of raw water sample.
6. Start adding 0.01M EDTA solution slowly till the color of the solution changes
from purple to violet. Record the volume of EDTA used and calculate calcium
hardness using the previous formula.
7. Calculate magnesium hardness (= total hardness - calcium hardness)
8. Repeat titration for the other water samples and calculate the hardness.
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Conclusions
Theory: Oxygen is slightly soluble in water and the dissolved oxygen (DO) does not
react with molecular water. As suggested by Henry's law, the saturation solubility or
maximum possible level of dissolved oxygen is directly proportional to its partial
pressure. This level is influenced by both physical and chemical characteristics of
water like temperature and salinity as well as biochemical activities in the water
body.
The analysis for DO is a key test in water pollution and waste treatment process
control. Presence of high levels of dissolved oxygen in water and wastewater is
desirable because it indicates good quality and as the level drops it could indicate the
presence of potential quality problems. Two standard methods for DO analysis are
available: Winkler (iodometric) method and the electrometric method which uses
membrane electrodes. The iodometric method, which is more accurate and reliable,
is a titrimetric procedure based on the oxidizing property of DO.
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Materials:
300 ml BOD bottles, pipette, burette (50 ml), flasks 250 ml, measuring cylinders,
alkaline-iodide-azide solution, manganous Sulphate solution, concentrated sulfuric
acid, starch indicator, 0.025M sodium thio Sulphate.
Experimental Procedure
1. Prepare aerated water sample by aerating distilled water for several hours.
Also prepare two more water samples containing chemical pollutants.
2. Fill narrow-mouth glass 300 ml BOD bottle with sample water and cap
carefully. Do not agitate the sample.
3. Add 2 ml MnSO4 solution to the bottles immersing the tip of the pipette below
the surface of water.
4. Add 2 ml alkali-iodide-azide solution to the bottles immersing the tip of the
pipette.
5. Cap the bottle tight, invert and mix thoroughly so that dissolved oxygen
present in the bottles is fixed as a brown precipitate (MnO2).
6. When the precipitate settles halfway, add 2 ml concentrated Sulphuric acid to
the bottle and invert it and shake well. The color of the solution turns
orange/yellow due to the oxidation of iodide (I-) to free iodine (I20).
7. Place 203 ml of sample in a flask and place on a magnetic stirrer.
8. Fill a burette with 0.025 M sodium thio Sulphate (Na2S2O3) solution and titrate
the sample till yellow tinge remains.
9. Add 1 to 2 ml starch indicator. Color will become blue then titrate till the
solution becomes colorless. Record the burette readings as mg/l DO.
10. Repeat the analysis for three given samples.
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Conclusions
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suitable for bacterial growth. Complete stabilization of a sample may require a period
of incubation too long for practical purposes; therefore, 5-day period has been
accepted as the standard incubation period.
Materials: BOD bottles, pipette, burette (25 ml), 250 ml flasks, measuring
cylinders, DO meter, incubator, Phosphate buffer, magnesium Sulphate, calcium
chloride, ferric chloride.
Experimental Procedure:
1. Prepare dilution water by aerating distilled water for several hours. Transfer
two liters into an aspirator bottle and add 2 ml each of magnesium Sulphate,
phosphate buffer, calcium chloride, and ferric chloride. Fill two bottles
designated as control with the dilution water (B1 and B2).
2. If seed is required add 0.2% seed material into the dilution water (optional).
3. Add carefully an appropriate volume of the sample, using Table 1 for
guidance, to two bottles and fill them with the dilution water (D1 and D2).
4. Switch and calibrate the dissolved oxygen meter.
5. Measure the initial DO in each BOD bottle (B1 and D1) either using Winkler
method or DO meter.
6. Incubate the bottles B2 and D2 for 5 days. After 5 days measure the final DO
in each bottle by the same procedure.
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I. For diluted sample without seeding
Sample Dissolved Oxygen (DO) mg/l BOD (mg/l)
Initial Final
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Conclusions:
Theory: Similar to BOD, chemical oxygen demand COD is a test used to estimate
the organic strength of wastes. However in this test, the organics are oxidized
chemically not using microorganisms. As a result of this the COD test needs much
less time (say 2 or 3 hours) to be conducted unlike the five days for the standard
BOD test. Also since all organics are oxidized chemically, COD values will be higher
than BOD values especially if biologically resistant organic matter is present in the
waste. It is also possible, for much waste, to generate a correlation between COD, the
quick and easy test, and BOD, the time consuming test. The COD test measures the
oxygen required to oxidize organic matter in water and wastewater samples by the
action of strong oxidizing agent under acidic conditions. Potassium dichromate has
been found to be excellent for this purpose. The test must be performed at an
elevated temperature and in the presence of silver sulfate as catalyst. The principal
reaction using dichromate as the oxidizing agent may be represented by following
equation:
Materials: Digestion vessels, block heater at 150 ± 20C, burette (25 ml), 250 ml
flasks, measuring cylinders, standard potassium dichromate digestion solution,
Sulphuric acid reagent, ferroin indicator solution, standard ferrous ammonium sulfate
titrant (FAS).
Experimental Procedure:
1. Place 2.5 ml sample in tubes and add 1.5 ml digestion solution.
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2. Add 3.5 ml sulfuric acid reagent down inside of vessel so an acid layer is
formed under the sample-digestion solution layer.
3. Tightly cap the tubes invert and shake well.
4. Place tubes in block digester preheated to 150 0C and reflux for 2 hours.
5. Cool to room temperature and place tubes in test tube rack.
6. Transfer contents to a 50ml flask and add 1 to 2 drops of ferroin indicator and
stir rapidly on magnetic stirrer.
7. Start titration against standard 0.1 M FAS until the color changes from blue
green to reddish brown and record the volume used.
8. For blank use same volume of distilled water instead of sample volume.
9. Calculate the COD using the equation below:
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Conclusions:
Experimental procedure:
1. Prepare 500 ml of the following two chlorine solutions: (a)
Approximately 2 mg/l as Cl2 in distilled water (b)
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Approximately 2 mg/l as Cl2 in a 2 mg NH3-N/l solution using bleach
solution (Clorox) as a source of chlorine (concentration about 50 g/l as Cl2)
and distilled water.
2. Place 5 ml phosphate buffer solution and 5 ml DPD indicator solution in a
titration flask and mix.
3. Add 100 ml sample (a) in step 1 and mix.
4. Titrate rapidly with standard ferrous ammonium sulfate (FAS) until the red
color disappears and take FAS volume used as (A), which will be the
concentration of free Cl2.
5. Add a small crystal of KI to the solution from the previous step and mix.
6. Continue titrating with FAS until the red color disappears and take the total
FAS volume used as (B), which will give the concentration of free Cl2 plus
monochloramine.
7. Add about 1 g of KI crystals to the solution from the previous step and mix.
8. Allow to stand for two minutes then continue titrating with FAS until the red
color disappears and take the total FAS volume used as (C), which will give
the concentration of dichloramine.
9. Repeat step 2-8 for sample (b) in step 1.
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Conclusions:
The most widely used measurement unit for turbidity is the FTU (Formazin Turbidity
Unit). ISO refers to its units as FNU (Formazin Nephelometric Units). There are several
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practical ways of checking water quality, the most direct being some measure of
attenuation (that is, reduction in strength) of light as it passes through a sample
column of water. The alternatively used Jackson Candle method (units: Jackson
Turbidity Unit or JTU) is essentially the inverse measure of the length of a column of
water needed to completely obscure a candle flame viewed through it. The more
water needed (the longer the water column), the clearer the water. Of course water
alone produces some attenuation, and any substances dissolved in the water that
produce color can attenuate some wavelengths. Modern instruments do not use
candles, but this approach of attenuation of a light beam through a column of water
should be calibrated and reported in JTUs. A property of the particles — that they will
scatter a light beam focused on them — is considered a more meaningful measure of
turbidity in water. Turbidity measured this way uses an instrument called a
nephelometer with the detector setup to the side of the light beam. More light
reaches the detector if there are lots of small particles scattering the source beam
than if there are few. The units of turbidity from a calibrated nephelometer are called
Nephelometric Turbidity Units (NTU). To some extent, how much light reflects for a
given amount of particulates is dependent upon properties of the particles like their
shape, color, and reflectivity. For this reason (and the reason that heavier particles
settle quickly and do not contribute to a turbidity reading), a correlation between
turbidity and total suspended solids (TSS) is somewhat unique for each location or
situation. Turbidity in lakes, reservoirs, channels, and the ocean can be measured
using a Secchi disk. This black and white disk is lowered into the water until it can no
longer be seen; the depth (Secchi depth) is then recorded as a measure of the
transparency of the water (inversely related to turbidity). The Secchi disk has the
advantages of integrating turbidity over depth (where variable turbidity layers are
present), being quick and easy to use, and inexpensive. It can provide a rough
indication of the depth of the euphotic zone with a 3-fold division of the Secchi depth,
however this cannot be used in shallow waters where the disk can still be seen on the
bottom.
Experimental Procedure:
1. Open the lid of the sample compartment. Insert a test tube filled with distilled
water in to the sample compartment. Close the lid.
2. Push the button SET 0 to get 0 displayed on the readout.
3. Open the lid. Replace the test tube filled with distilled water with a test tube
filled with Formazine standard. Close the lid.
4. Push button SET 100 to get 100 displayed on the readout.
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5. Open the lid. Replace the test tube filled with Formazine standard with a test
tube filled with given water sample. Close the lid.
6. Read the value on the display.
Result:
The turbidity of the given water sample is found to be......................
Conclusions:
1. Sample no. ............, .............., ............ has more turbidity than permissible
limit, so it requires treatment.
2. Sample no. ........., .........., ........... has turbidity within permissible limit, hence
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