Environmental Lab Manual
Environmental Lab Manual
LABORATORY MANUAL
Expt no Title
1 Measurement of PH of a sample
4 To determine suspended solids, dissolved solid, and total solids of water sample
6 To determine the optimum dose of coagulant in the given sample by jar test.
2. Sanitary Engineering :
Expt no Title
AIM OF THE EXPERIMENT: Determine The PH Of Given Sample Using PH Paper And Digital
PH Meter.
THEORY: PH refers to the hydrogen ion activity. It is expressed as the negative logarithm of the
reciprocal of the hydrogen ion activity in moles per litre. It can be measured by pH paper or
electrometrically by measuring of hydrogen ion by potentiometric measurement using a standard
hydrogen electrode and a reference electrode.
REAGENTS REQUIRED: Standard buffer solution: Standard buffer solution can be prepared freshly by
dissolving the standard buffer tablets or powders (pH 4 and 7.2).
PROCEDURE:
a) Using pH meters:
Note the sample temperature. Rinse the electrode thoroughly with distilled water and carefully wipe
with a tissue paper. Dip the electrode in to the sample solution.
b) Using pH paper:
Dip the pH paper strip in to the solution. Compare the colour given on the wrapper of the PH paper
book.
RESULT:
pH value of sample using pH paper =
pH value of sample using pH meter =
CONCLUSION:
EXPERIMENT NO – 2
AIM OF THE EXPERIMENT: Determine The Turbidity Of The Given Sample Using
Nephelometer In N.T.U.
THEORY:
Turbidity can be measured either by its effects on the transmission of light which is termed as
turbidimetry or its effects on the scattering of light which termed as Nephelometry. Turbidimetry can
be used for sample with moderate turbidity and Nephelometer for sample with low turbidity. Higher the
intensity of scattered light higher the turbidity.
APPARATUS REQUIRED:
1) Nephelometric turbidimeter
2) Cuvettes; it take the samples for measurements
REAGENTS:
• Solution (1) Dissolve 1 g hydrazine sulphate in distilled water and dilute to 100 ml in volumetric
flask
• Solution (2) dissolve 10g hexamine LR grade in distilled water and dilute to 100ml in volumetric
flask
• In 100ml volumetric flask, mix 5 ml solution (1) and 5 ml solution (2) let them stand for 24 hours
and dilute to 100ml of distilled water which has the turbidity of 400 NTU.
• Dilute this solution to 1000ml so that its turbidity becomes 40 NTU.
PROCEDURE:
CALIBRATION:
• Switch on the instrument and keep it on for some time
• Select appropriate range depending upon the expected turbidity of the sample.
• Set zero of the instrument with distilled water and adjust “0” with set zero knob.
• Now in another test tube take standard suspension just prepared of 40 NTU and adjust the reading
in the instrument to 40 NTU.
OBSERVATION :
RESULT:
EXPERIMENT NO 3
AIM OF THE EXPERIMENT: To Determine The Amount Of Total Residual Chlorine Present In The
Given Sample Of Chlorinated Water By Starch Iodide Method.
THEORY: The raw water generally has some amount of bacteria present in it. During the process of
water treatment such as sedimentation and filtration some of it gets removed. The remaining is destroyed
during the process called disinfection. Disinfection is generally achieved by adding chlorine in suitable
form and dose .Therefore it is also known as chlorination. Chlorination is also done in order to arrest any
possible growth of bacteria in the water distribution system. When we add chlorine to the water a part of
it is consumed in destroying the bacteria and some part is available at the consumer end. It is
recommended that an amount of 0.1 to 0.2 ppm of residual chlorine should be available at the consumer
end to achieve the desired purpose.
APPARATUS REQUIRED:
1. Burette
2. Pipette
3. Erlenmeyer flask
REAGENTS:
2. Potassium Iodide
4. Starch solution
PROCEDURE:
3. Add 1gm of potassium iodide and mix thoroughly. Yellow colour is obtained
4. Titrate against standard sodium thiosulphate solution in the burette until a pale yellow colour is
obtained
5. At these stages add 1ml of starch indicator and continue the titration till the blue colour
disappears. Note down the final reading. ( V1)
CALCULATIONS:
V2 = Sample volume
N=Normality of Na2S2O3
Residual Chlorine =
RESULT:
REMARKS:
EXPERIMENT NO 4
INTRODUCTION:
Environmental engineering is concerned with the solid material in a wide range of
natural waters and wastewaters. The usual definition of solids (referred to as "total
solids") is the matter that remains as residue upon evaporation at 103~105°C. The
various components of "total solids" can be simplified as
Total Solids (TS) are the total of all solids in a water sample. They include the total
suspended solids and total dissolved solids. Total Suspended Solids (TSS) is the
amount of filterable solids in a water sample. Samples are filtered through a glass fiber
filter. The filters are dried and weighed to determine the amount of total suspended
solids in mg/l of sample. Total Dissolved Solids (TDS) are those solids that pass
through a filter with a pore size of 2.0 micron (1/1000000th of a meter, Also known as
a Micrometer) or smaller. They are said to be non-filterable. After filtration the filtrate
(liquid) is dried and the remaining residue is weighed and calculated as mg/l of Total
Dissolved Solids.
APPARATUS:
1. Balance
2. Beaker
3. Measuring Cylinder
4. Filter paper
5. Funnel
6. Dropper
PROCEDURE:
(1) Take a clear dry glass beaker (which was kept at 103°C in an oven for 1 hour) of
150ml capacity and put appropriate identification mark on it. Weight the beaker and
note the weight.
(2) Pour 100ml. of the thoroughly mixed sample, measured by the measuring cylinder,
in the beaker.
(3) Place the beaker in an oven maintained at 103°C for 24hours. After 24 hours, cool
the beaker and weight. Find out the weight of solids in the beaker by subtracting the
weight of the clean beaker determined in step (1)
(4) Calculate total solids (TS) as follows:
CALCULATION:
Total Dissolved Solids, TDS (mg/l) =mg of solids in the beaker x1000 /(volume of sample)
THEORY:
Dissolved oxygen (DO) levels in environmental water depend on the physiochemical and biochemical
activities in water body and it is an important useful in pollution and waste treatment process control.
Two methods are commonly used to determine DO concentration:
1. The iodometric method which is a titration-based method and depends on oxidizing property
of DO.
2. The membrane electrode procedure, which works based on the rate of diffusion of molecular
oxygen across a membrane.
Samplers are designed to ensure that air cannot enter into the sample. Most samplers are designed to
retain 3-4 times the volume of samples which is required for analysis purposes. As oxygen values
change with time due to any biological activity, it is important to fix it in field immediately after
collection. This is done using reagents using in DO test and then the titration is done in laboratory.
This method gives low results for samples with high iodine demand and in this case it is better to
preserve sample using 0.7 ml concentrated sulphuric acid and 0.02 g sodium azide. When this is done
it is necessary to add 3 ml of alkali-iodide reagent rather than the usual 2 ml because of the extra acid
the sample contains. Better results are also obtained if the sample is fixed and stored in the dark and
on the ice until the analysis are conducted. The final titration should not be delayed more than 6
hours.
REAGENTS:
1) Manganese sulphate solution: Dissolve 480 g MnSO4.4H2O, 400g MnSO4.2H2O or 364g
MnSO4.H2O in distilled water, filter, and dilute to 1l. The MnSO4 solution should not give a
color with starch when added to an acidified potassium iodide (KI) solution.
2) Alkali-iodide-azide reagent
3) Sulphuric acid: One ml is equivalent to ~ 3ml alkali-iodide-azide reagent.
4) Starch solution: Dissolve 2g laboratory-grade soluble starch and 0.2 g salicyclic acid as
preservative in 100 ml hot distilled water.
5) Standard sodium thiosulphate titrant: Dissolve 6.205 g Na2S2O3.5H2O in distiller water and add
1.5ml 6N NaOH or 0.4 g solid NaOH and dilute to 1000 mL. Standardize with bi-iodate
solution.Standard potassium bi-iodate solution (0.0021M): Dissolve 812.4 mg KH(IO3) in
distilled water and dilute to 1000 ml.
6) Standardization: Dissolve e ~ 2 g KI, free from iodate in an Erlenmeyer flask with 100 to 150
mL distilled water; add 1 mL 6N H2SO4 or a few drops of conc. H2SO4 and 20.00 mL standard
bi- iodate solution. Dilute to 200 mL and titrate librated iodine with thiosulphate titrant, adding
starch toward end of titration, when a pale straw color is reached. When the solution is of equal,
20.00 mL 0.025M Na2S2O3 should be required. If not, adjust the Na2S2O3 solution to 0.025M.
PROCEDURE:
1) Make dilution water by adding 2mL/L of following reagents in distilled water:
a. Phosphate buffer solution
b. Magnesium sulphate solution
c. Calcium chloride solution
d. Ferric chloride solution
e. Sodium Sulphite solution
2) Take 300 mL sample in BOD bottle. Prepare two sets of this sample. Keep one set for DO
analysis for day 0 (i.e., Sample0Day) and another sample in BOD incubator for 5 days at 20°C
(Sample5Day) (this is how 5-day BOD experiment is done). Here you will prepare duplicate
samples and analyze at Day 0 (i.e., Sample0Day_A and Sample0Day
3) For a given sample bottle, add 1 mL of alkali azide and then 1 mL manganeous sulphate
solution. Shake well the bottle and keep it open for 5 minutes to settle the precipitate. Add 2 mL
concentrated H2SO4 and place the cap on the bottle. Shake well the bottle till all the precipitate
is dissolved.
4) Take 203 mL of sample in conical flask and titrate with standard sodium thiosulphate solution
(0.025N) till the colour changes from dark yellow to light yellow. Then add few drops of starch
indicator and continue to titrate till the color of the solution becomes either colorless or changes
to its original sample colour. Note down volume of 0.025N sodium thiosulphate consumed.
5) Calculate the DO Value.
OBSERVATION:
CONCLUSION:
REMARKS
EXPERIMENT NO 6
AIM OF THE EXPERIMENT: Jar Test for Determining Optimum Coagulant Dosage for
clarifying the given sample.
THEORY: Coagulants are used in water treatment plants to remove natural suspended and
colloidal matterter, to remove material which do not settle in plain sedimentation, and to assist
in filtration
Alum [Al2S(SO4)3. 18H2O] is the most widely used coagulant. When alum solution is added
to water, the molecules dissociate to yield SO42- and Al3+. The +ve species combine with
negatively charged colloidal to neutralise part of the charge on the colloidal particle. Thus,
agglomeration takes place. Coagulation is a quite complex phenomenon and the coagulant
should be distributed uniformly through out the solution.
Jar test is simple device used to determine this optimum coagulant dose required. The jar test,
device consists of a number of stirrers (4 to 6) provided with paddles. The paddles can be
rotated with varying speed with the help of a motor and regulator. Samples will be taken in
jars or beakers and varying dose of coagulant will be added simultaneously to all the jars. The
paddles will be rotated at 100 rpm for 1 minute and at 40 rpm for 20 to 30 minutes,
corresponding to the flash mixing and slow mixing in the flocculator of the treatment plant.
After 30 minutes settling, supernatant will be taken carefully from all the jars to measure
turbidity. The dose, which gives the least turbidity, is taken as the optimum coagulant dose.
APPARATUS
REAGENTS:
1) Alum solution (1ml containing 10 mg of alum)
2) Lime
3) Acid/alkali
PROCEDURE :
1) Take 1-litre beakers and fill them with sample up to the mark.
2) Keep each beaker below each paddle and lower the paddles, such that each one is about 1cm
above the bottom.
3) Find the pH of the sample and adjust it to 6 to 8.5.
4) Pipette 1, 2, 3, 4, 5, 6 mL of the alum solution into the test samples.
5) Immediately run the paddles at 100 rpm for 1 minute.
6) Reduce the speed to 30-40 rpm and run at this rate for 30 minutes.
7) Stop the machine, lift out the paddles and allow to settle for 30 minutes.
8) Find the residual turbidity of the supernatant using nephelometer.
9) Plot a graph with alum dosage along x-axis and turbidity along y-axis.
10) The dosage of alum, which represents least turbidity, gives Optimum Coagulant Dosage
(O.C.D.).
11) Repeat steps 1-10 with higher dose of alum, if necessary.
OBSERVATION :
Result:
Optimum coagulant doses =
EXPERIMENT NO 7
AIM OF THE EXPERIMENT: Determine The BOD Value For Determining Biodegradability Of
Solution .
THEORY:
The most widely used test indicating organic pollution of both wastewater and surface water is the 5-
day BOD (BOD5). This determination involves the measurement of the dissolved oxygen used by
microorganisms in the biochemical oxidation of organic matter. BOD5 is the total amount of oxygen
consumed by microorganisms during the first five days of biodegradation. Oxygen demand is
associated with the biodegradation of the carbonaceous portion of wastes and oxidation of nitrogen
compounds such as ammonia. The following equations simplify the process of biodegradation:
APPARATUS REQUIRED:
REAGENTS REQUIRED:
2. Alkali-iodide-azide reagent
4. Starch solution: Dissolve 2 g laboratory-grade soluble starch and 0.2 g salicylic acid as
preservative in 100 mL hot distilled water.
5. Standard sodium thiosulphate titrant: Dissolve 6.205 g Na2S2O3 .5H2O in distiller water and
add1.5 mL 6N NaOH or 0.4 g solid NaOH and dilute to 1000 mL. Standardize with bi-
iodatesolution.
6. Standard potassium bi-iodate solution (0.0021M): Dissolve 812.4 mg KH(IO3) in distilled water
and dilute to 1000 mL.
7. Standardization: Dissolve e ~ 2 g KI, free from iodate in an Erlenmeyer flask with 100 to 150mL
distilled water; add 1 mL 6N H2SO4 or a few drops of conc. H2SO4 and 20.00 mL standard bi-
iodate solution. Dilute to 200 mL and titrate librated iodine with thiosulphate titrant, adding starch
toward end of titration, when a pale straw colour is reached. When the solution is of equal, 20.00 mL
0.025M Na2S2O3 should be required. If not, adjust the Na2S2O3 solution to 0.025M.
PROCEDURE:
DO measurement:
2. For a given sample bottle, add 1 mL of alkaliazide and then 1 mL manganous sulphate solution.
Shake well the bottle and keep it open for 5 minutes to settle the precipitate. Add 2 mL concentrated
H2SO4and place the cap on the bottle. Shake well the bottle till all the precipitate is dissolved.
3. Take 203 mL of sample in conical flask and titrate with standard sodium thiosulphate solution
(0.025N) till the colour changes from dark yellow to light yellow. Then add few drops of starch
indicator and continue to titrate till the colour of the solution becomes either colourless or changes to
its original sample colour. Note down volume of 0.025N sodium thiosulphate consumed.
BOD:
1. Prepare BOD dilutions. Use dilution water (it contains nutrients, the exact Osample in 300 mL BOD
bottle, fill up with dilution water;15 mL sample in 300 mL BOD bottle, fill up with dilutionwater;20
mL sample in 300 mL BOD bottle, fill up with dilution water
2. Take 300 mL sample in BOD bottle. Prepare two sets of this sample. Keep one set for DO analysis
for day 0 (i.e., Sample0Day) and another sample in BOD incubator for 5 days at 20°C
(Sample5Day).
5. Come back in the lab after 5 days and record dissolved oxygen.
CONCLUSION:
REMARKS:
EXPERIMENT NO 8
AIM OF THE EXPERIMENT: Determine COD Value For Determining Organic Strength Of
Solution (Closed Reflux Method)
THEORY:
Chemical oxygen demand (COD) is termed as the amount of a specific oxidizing agent that reacts with
sample under controlled conditions and it is expressed as oxygen equivalence. This parameter indicates
the extent of organic matter contamination of water and is always higher than the biochemical oxygen
demand (BOD). It is used to indicate organic matter contamination and it helps in knowing overall
organic load to the receiving body.
Selection Of Method:
The first method: open reflux method is suitable for a wide range of wastes where large volume of
sample is required (for samples with COD=50 mg O2/L).
In the second method: closed reflux methods, small quantities of metallic salt reagents are required and
small quantities of hazardous waste is produced (for samples with COD= 5 to 50 mgO2/L). In the
closed reflux method, ampules and culture tubes with premeasured reagents are used and then samples
is placed in the tube and COD is determined.
In this experiment, closed reflux method is used and samples with COD < 50 mg O2/L are tested.
Potassium dichromate is a strong oxidizing agent and it can be used to prepare solution of exact
normality.
1. Digestion vessels;
2. block heater;
3. microburette; ampule sealer.
4. Borosilicate culture tubes (16mm*100 mm or 20 mm*150mm) with TFE lined-screw caps
are used.
The block heater is required to operate at 150±2°C with holes to accommodated digestion vessels.
Do not use an oven because of the possibility of leaking samples generating corrosive and explosive
atmosphere.
REAGENTS:
a. Standard potassium dichromate digestion solution, 0.01667M: Add to about 500 mL distilled
water 4.903 g K2Cr2O7, primary standard grade, previously dried at 150°C for 2 h, 167 mL conc.
H2SO4 , and 33.3 g HgSO4. Dissolve, cool to room temperature, and dilute to 1000 mL.
b. Sulfuric acid reagent:
c. Ferroin indicator solution: Dilute it by a factor of 5 as required. This indicator is used to indicate
change in oxidation-reduction potential of the solution.
d. Standard ferrous ammonium sulfate titrant (FAS), approximately 0.10M: Dissolve 39.2 g
Fe(NH4)2(SO4)2.6H2O in distilled water. Add 20 mL conc. H2SO4, cool, and dilute to 1000 mL.
Standardize solution daily against standard K2Cr2O7 digestion solution as follows: Pipet 5.00 mL
digestion solution into a small beaker. Add 10 mL reagent water to substitute for sample. Cool to
room temperature. Add 1 to 2 drops diluted ferroin indicator and titrate with FAS titrant.
Molarity of FAS solution = [VK2Cr2O7 ×0.1] / (VFAS) (3)
Where: VK2Cr2O7= volume of K2Cr2O7 (mL); VFAS = volume of FAS (mL)
e. Sulphamic acid:
PROCEDURE:
1. Wash culture tubes and caps with 20% H2SO4 before using to prevent contamination.
2. Place sample in culture tube or ampule and add digestion solution. Carefully run sulphuric acid
reagent down inside of vessel so an acid layer is formed under the sample-digestion solution layer
and tightly cap tubes or seal ampules, and invert each several times to mix completely.
3. Place tubes or ampules in block digester preheated to 150°C and reflux for 2h behind a protective
shield. CAUTION: These sealed vessels may be under pressure from gases generated during
digestion. Wear face and hand protection when handling and dangerous pressures will be generated
at 150°C.
4. Cool to room temperature and place vessels in test tube rack. Some mercuric sulphate may
precipitate out but this will not affect the analysis.
5. Remove culture tube caps and add small TFE-covered magnetic stirring bar. If ampules are used,
transfer contents to a larger container for titrating.
6. Add 0.05 to 0.10 mL (1 to 2 drops) ferroin indicator and stir rapidly on magnetic stirrer while titrating
with standardized 0.10M FAS. The end point is a sharp colour change from blue-green to reddish brown,
although the blue green may reappear within minutes. In the same manner reflux and titrate a blank
containing the reagents and a volume of distilled water equal to that of the sample.
7. COD is given by
CONCLUSION:
REMARKS:
21 | P a g
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