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ENVIRONMENT ENGINEERING-I
PRACTICAL FILE
SESSION 2014
SUBMITTED TO:-
SUBMITTED BY:-
Palak Jain
0101CE111035
CONTENTS
6. Determination
of
BIOLOGICAL
OXYGEN
DEMAND
ACIDITY
OBJECT: To determine the acidity of given sample of water.
SAMPLE DETAILS:
Location:
Time:
Date:
Temperature:
APPARATUS: Burette , Pipette , Conical flask , Glazed tile.
REAGENTS:
a) 0.02 NaOH solution.
b) Methyl orange Indicator solution , and
c) Phenolphthalein indicator solution.
THEORY:
Acidity of a liquid is its capacity to donate H+ ions . It is also defined as
the capacity of a solution to neutralize a std. alkali. The acidity of a water may be
due to the presence of uncombined CO2 , mineral acids and salts of strong acids
and weak bases. Since most of the natural waters and sewages are buffered by
CO2 bicarbonate system, the acidity present due to free CO2 has no significance
from public health viewpoint.
PRINCIPLE :
Titrating or neutralizing samples at pH 4.3 can calc. the mineral acids
present and contributing mineral acidity. The CO2 and bicarbonates (carbonic
acids) present in the sample can be neutralized completely by continuing the
titration to pH 8.3.
INTERFERNCE :
Colour , Turbidity , Iron , Aluminium , and residual chlorine are
prime sources of interference.
PROCEDURE:
(A) Total Acidity
This determination should be made on the spot on a fresh sample
collected in a bottle and stoppered immediately to prevent escape of CO2 .
1) Measure suitable vol. of sample(50 or 100 mL) in 250 mL conical
flask.
2) Add 2-3 drops phenolphthalein indicator and titrate with NaOH till
faintpinkcolour appears indicating pH 8.3.
3) Note down the vol. of NaOH required as A.
(B) Mineral Acidity
1) Measure suitable vol. of sample(50 or 100 mL) in250 mL conical
flask.
2) Add 2-3 drops of methyl orange indicator and titrate with std.
0.02 NaOH till colour changes to faint orange characteristicof pH
4.4 -4.3.
3) Note down the vol. of NaOH required as B.
OBSERVATION:
CALCULATIONS:
RESULTS:
ALKALINITY
OBJECT: To determine the alkalinity of given sample of water.
SAMPLE DETAILS:
Location:
Time:
Date:
Temperature:
APPRATUS: Burette,pipette,conical flask,glazed tiles
REAGENTS:
a)0.02N H2SO4 solution
b)methyl orange indicator solution and
c)phenolphthalein indicator solution
THEORY:
The alkalinity of water is measured by its capacity to neutralize acids. the
alkalinity of natural water is due to presence of salts of carbonates,
bicarbonates,silicates and phosphates along with hydroxyl ions in free
state.however the major portion of alkalinity in natural water is caused by
hydroxide, carbonates,bicarbonates which may be ranked in order of their
association with high pH values.Alkalinity value provide guidance in proper
doses of chemicals in water and waste water treatment process,particularly in
coagulation,softening and operational control of anaerobic digestion.
PRINCIPLE:
Alkalinity of sample can be estimated by titrating with standard sulfuric
acid.titration to pH 8.3 or decolourization of phenolphthalein indicator will show
the complete neutralization of OH and of CO 3 while to pH of 4.5 or sharp
change from yellow to orange of methyl orange will indicate total alkalinity
(complete neutralization of OH,HCO3,CO3)
INTERFERENCES:
Colour,turbidity,iron aluminium and residual chlorine are prime sources of
interference.colour and turbidity can be avoided using potentiometric
titration.residual chlorine can be removed by adding thiosulfate.
PROCEDURE:
a) Take 50 or 100 ml sample in a conical flask and 2-3 drops of
phenolphthalein indicator.
b) If pink colour develops titrate it with 0.02N H2SO4 till the colour disappears
or pH is 8.3.note the vol of H2SO4 required as A.
c) Add 2-3 drops of methyl orange tosame flask, and continue titration till pH
comes down to 4.5.or yellow colour changes to orange.note tho vol. of
H2SO4 as B.
d) If pink colour does not appear after addition of phenolphthalein continue as
in c) above.
e) Calculate total or methyl orange alkalinity (T) or phenolphthalein alkalinity
(P) and express it in mg/l as CaCO3.
OBSERVATIONS:
CALCULATIONS:
P- alkalinity as mg/l in CaCO3=A1000
Vol of sample
T-alkalinity as mg/l in CaCO3=B1000
Vol of sample
Where A=ml of H2SO4 required to bring pH to 8.3
B=ml of H2SO4 required to bring pH to4.5
N=normality of H2SO4 used.
Once the phenolphthalein and total alkalinities are determined then three types of
alkalinities hydroxide,carbonate and bicarbonates can be easily calculated by
following table-
Once carbonate and bicarbonate alkalinities are known then their conversion
milligrams per litre CO3 of HCO3 are possible.
Mg/l CO3= mg/l carbonate alkalinity0.6
Mg/l HCO3=mg/l bicarbonate alkalinity1.22
CHLORIDES
OBJECT: To determine the amount of chlorides in the given sample of water.
SAMPLE DETAILS
Location:
Time:
Date:
Temperature:
APPARATUS:
Burette, Pipette, Conical flask, Glazed tile.
REAGENTS:
a) Silver Nitrate(N/71),
b) Potassium chromate indicator, and
c) Chemicals for pH adjustment.
THEORY:
chloride anion is generally present in natural waters in widely varying
concentration. The presence of chloride in natural water can be attributed to
dissolution of salt deposits, discharges of a effluents from chemical industries, oil
well operations, Sewage discharges, irrigation drainage, contamination from
refuge leachates, and sea water intrusion in coastal areas. Each of these sources
result in local contamination of both surface water and ground water.
The salty taste produced by chlorides depends on the chemical
composition of the water. A concentration of 250mg/l may be detectable in some
water containing sodium ions. On the other hand , the typical salty taste may be
absent in water containing 1000 mg/l chloride, when calcium and magnesium
ions are predominant. A high chloride content also has deleterious effect on
metallic pipes and structures as well as on agricultural plants.
Three methods are suggested for the estimation of chloride, (1)
Involving titration against standard mercuric nitrate solution.(2)An argeniometric
method (Mohrs method), and (3) A determination of chloride is required.
Particularly at low concentrations the potentiometric method is suitable only
when the sample is coloured or turbid, argeniometric is the simplest one and can
PRINCIPLE:
Chloride is determined in a natural or slightly alkaline solution by
titration with standard silver nitrate using potassium chromate as an indicator.
Silver chloride is quantitatively precipitated before red silver chromate is formed.
INTERFERENCES:
Bromide, iodide and cyanide are measured as equivalent of
chloride ions, hence pre-treatment of the sample with the help of special reagents
must be done before titration to remove the interfering substances and colour and
turbidity if present.
If the sample contains sufficient thiosulphate, thiocyanate cyanide,
sulphite and sulphide to interfere seriously with the determination, they may be
oxidised to non-interfering substances as follows.
Measure a suitable quantity of sample into a conical flask and
dilute to 150 ml with water. Add 25 ml H2O2 (3%) and boil for 15 min, then add
further 10 ml H2O2 and boil for 5 min .Repeat the same until the solution is
thiocyanate free.
If the sample is too coloured or turbid to allow the end point to be
readily detected, this interference may be reduced by the following treatment
with a suspension of aluminium hydroxide.
Add 3ml aluminium hydroxide suspension to the measured
quantity of sample. Stir thoroughly, set aside for a few minutes and filter. Wash
the precipitate with distilled water. Collect the washing with the filtrate and
continue as described under procedure.
PROCEDURE :
1) Take 100 ml sample and adjust the pH between 7.0 and 8.0
2) Take 50 ml well mixed sample adjusted to pH between 7.0 and 8.0 and add 1.0
ml potassium chromate k2CRO4.
3) Titrate with standard silver nitrate AGNO3 solution till silver chromate
AG2CRO4 starts precipitating giving res colour. Note the final burette reading.
4) Repeat the above the procedure for distilled water (50 ml) to establish reagent
blank.
OBSERVATIONS:
Initial ph=
RESULTS :
TURBIDITY
OBJECT: To determine the turbidity of a sample by nephlometer
SAMPLE DETAILS:
Location:
Time:
Date:
Temperature:
APPARATUS: Turbidity of Nephlometer, Conical flask etc.
REAGENTS:Turbidity free water, stock turbidity suspension.
THEORY:
Turbidity is a condition of water resulting from the presence of suspended
matters and affects the light condition in the aquatic environment. The turbidity
of natural water may be either due to suspended inorganic substance ,such as silt
and clay or due to palnktonic organism .in fresh waters such as lakes and ponds
the phytoplankton is sometimes sufficiently abundant to produce a notable
reduction in light . Turbidity is an important limiting factor affecting productivity
sample of lakes and ponds and varies greately with the nature of basin degree of
exposure, nature of sediments, rains, floods and other factors
There are various instrument for measurement of turbidity such as the
Jacksons turbid meter ,Hellige turbidmeter and nephlometer and hach turbid
meter .Here we will describe the Nephlometer.
The instrument operates on the principle that light passing through the sample
is scattered by suspended particulate matter.A beam of light is passed through a
cell containing the sample as the beam passes though the suspended particles an
amount of light (directly proportional to turbidity) is scattered at right angles to
the beam and is received by a photo multiplier and amplified .The readings are
obtained in NTU (Nephlometer turbidity Unit).
The digital Turbidmeter is very accurate and stable instrument for measurement
of turbidity up to 1000 NTU (Nephlo Turbidity unit)
PRINCIPLE :The method is based on the comparison of the intensity of light
scattered by the sample under defined condition with the intensity of light
scattered by a standard reference suspension under the same condition .The
higher the scattered light ,the higher the turbidity.
PROCEDURE:
1. Allow sufficient warm up period after switching ON the instrument.
2. Take the test tube containing distilled water or blank solution in the test
tube holder and close the test tube holder cover .make sure that the mark
on test tube coincides with the mark on the panel.
3. Select the required range for measurement.
4. Adjust the display to 000 by adjusting set Zero knob.
5. Remove the test tube containing distilled water and fill another test tube
containing standard solution say 400 NTU as per the expected range of
unknown solution .place it in the tube holder .
6. Take the measurement of the solution suspension and adjust the
calibrate knob so that the display reads the selected standard solution
value.
7. Again check the display zero with the tube containing distilled water.
8. Now the instrument is ready to take measurement of any unknown
suspension.
RESULT & CONCLUSION:
DISSOLVED OXYGEN
Object: - To determine the dissolved oxygen in the given sample of water.
Sample Details:
Location:
Time:
Date:
Temperature:
Apparatus: 300ml ground glass, stoppered bottles, sampling device for
collection of samples, Nesslers tube, tubes, burette, pipette, conical flask, glazed
tile etc.
Reagents: MnSO4 solution, Conc. H2SO4, Alkali Iodide Azide sol., N/40
Na2S2O3 sol., starch indicator
Theory: All living organisms are dependent upon oxygen in one form or the
other to maintain the metabolic process that produce energy for growth and
reproduction. Aerobic processes are the subjects of great interest for their need of
free oxygen. Dissolved oxygen ( DO ) is also important in precipitation and
dissolution of inorganic substances in water.
The solubility of atmospheric oxygen in fresh water ranges from 14.6
mg/L at 0 deg.C to about 7.0 mg/L at 35 deg.C under one atmospheric pressure.
Since it is a poorly soluble gas its solubility directly varies with the atmospheric
pressure at any given temperature.
The water sample is collected under the surface and allowed to flow in to
the sample bottle slowly to prevent mixing in air. Glass stoppered bottles are best
because the stoppers prevent mixing with air.
2. 2Mn(OH)2 + O2 = 2MnO(OH)2
(D.O.) (Brown ppt.)
3. MnO(OH)2 + 2H2SO4 = Mn(SO4)2 +3H20
4. Mn(SO4)2 + 2KI = MnSO4 + K2 SO4 + I2
5. 2Na2S2O3 + I2 = 2NaI + Na2SO4O6
Wrinklers Method with Azide Modification
1. 2NaN3 + 2 H2SO4 = Na2SO4 + 2HN3
(Sodium Azide)
2. 2NaNO2 + H2SO4 = 2HNO2 + Na2SO4
3. NH3 + HNO2 = N2O + N2 +H2O
Procedure:
1. To 300ml shape in BOD bottle, add 2ml Mangnese sulphate solution.
2. Then add 2ml alkali iodide azide solution.
3. Insert the stopper and mix by inverting the bottle 15 times. Precipitate is
allowed to settle leaving a clear supernatant solution.
4. Add 2ml conc, sulphuric acid. Insert the stopper and shake well.
5. From the bottle, 203ml of content is taken out.(this is because 200ml of the
original sampe must be used for titration. As 2ml of eah manganese
sulphate and alkali iodide azide reagents have been addd, the proper
quantity corresponds to 200ml
6. i.e. 200 * 600 = 203 ml
7. (300-4)
8. 1-2 ml of starch solution is addwd which turns its colour to blue.
9. Titrate again till the blue colour just disappears and note the corresponding
reading.
Observation :
Initial pH
S.No. Volume
Sample
1.
2.
3.
Calculations :
1 ml of 0.0025 N Na2S2O3 = 0.2 mg of O2
(.2 * 1000) ml of Thiosulphate (A)
DO in mg/l =
.
200
INTERFERENCES:
Since DO estimation is the basis of BOD test, sources of interferences in the
BOD test are same as that in DO test. In addition, lack of nutrients in dilution
water, lack of an acclimated seed organism, presence of heavy metals and other
toxic materials like residual chlorine are the sources of interferences in this test.
Seed organisms and presence of heavy metal or other toxic material such as
residual chlorine and other sources of interference in this test.
PROCEDURE:
A) Preparation Of Diluted Water
1. Acetate the required volume of distilled water in a container by bubbling
compressed air for 1-2 days to attain DO saturation. Try to maintain the
temperature near 20C
2. Add 1 ml each of phosphate buffer, magnesium sulphite, and Calcium
chloride & ferric chloride solution for each litre of dilution water. Mix
well.
3. In the each case of wastes which are not expected to have sufficient
bacteria population add seed to the dilution water. Generally settled
sewage is considered sufficient for 1000 ml of dilution water
B) Dilution of sample:
1. Neutralize the sample to pH around 7.0 if it is highly alkaline or acidic.
2. The sample should be free from residual chlorine. If it contains residual
chlorine remove it by using Na2SO3 solution as follows. Take 50 ml of
the sample and acidity with addition of 10 ml & 1 ml acetic acid. Add
about 1 g KI. Titrate with sodium sulphite (0.025 N) using starch
indicator. Calculate the volume of sodium sulphite required per ml of the
sample and add accordingly to the sample to be tasted for BOD.
3. Samples having high DO content i.e., DO 9 mg/l due to either algal
growth or some other reason, reduce the DO content by aerating and
agitating the samples.
4. Make several dilution of the pre-treated sample so as to obtain about
50% depletion od Do in dilution water but not less than 2mg and the
residual oxygen after 5 days of incubation should not be less than 1mg/l.
prepare dilution as follows:
5. Siphon out seeded dilution water in a measuring cylinder or volume
flask half the required volume. Add the required of carefully mixed
sample. Dilute to the desired volume by siphoning dilution water and
mix well.
0.1%
1.0%
5.0%
25%
to
to
to
to
S. No.
N/40
Blank
%
Diluted
waste
water
sample
CALCULATION:
O2
consumed=
D.O.
of
blank
D.O.
diluted
sample
RESULTS :