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Principle : Sulphate ions ( SO4-2 ) is precipitate in an acelic acid medium with barium
chloride ( BaCl2) so as to form barium sulphate (BaSO4) crystals of uniform size. Light
absorption of the BaSO4 suspension is measured by photometer and the sulphate
concentration is determined by comparison of reading with standard curve.
Result :
Experiment No
Theory : : Chloride in the form of chloride Cl – ions, is one of the major inorganic
anions in water and waste water. The chloride concentration is higher in
the waste water than the raw water because of sodium chloride ( NaCl) is
a common ingredient of diet and passes unchanged through the
digestive system. At the sea coast, chloride may be present in high
concentration because of leakage of salt water into the sewage system. It
may be also increased by industrial process. High chloride content may
harm metal pipes and structures as well as growing plants.
Principle : In neutral or slightly alkaline solution K2CrO4 indicates the end of silver
chloride gets quantitatively precipitated before red silver chromate is
formed.
Calculation :
1000ml of 1N AgNO3 = 35.45gm Cl-
... 1 ml of 0.0141 AgNO3 = 35.45 x 0.0141mg Cl-
= 0.499mg Cl- or say 500µg Cl- or 0.5mg Cl-
Formula :
Result:
Conclusion :
Experiment No
Reagents :
i) Distilled water of highest purity and thoroughly aerated so as to
saturate with DO at a lowered temp. of 200C.
ii) Phosphate buffer solution – 8.5 gm KH2PO4 , 21.75 gm
K2 HPO4, 33.4 gm Na2 HPO4.
iii) Magnesium sulphate solution–22.5gm MgSO4H2O dissolved in
1-1 of distilled water.
iv) Calcium chloride solution – 27.5 gm anhydrous CaCl2 dissolved
in 1-1 distilled water.
v) Ferric chloride solution – 0.25 gm FeCl3, 6 H2O in 1-1 distilled
water, All other regents are similar to those in Do measurement.
Preparation of dilution water: Place required amount of aerated distilled water at 200C. Add 1
ml each of phosphate buffer, magnesium sulphate, calcium
chloride and ferric chloride per liter of water, Seed the dilution
water, if necessary by adding 1 to 10 ml of settled sewage (24
to 36 hours old) per liter (seed should not exert more then 0.5
mg/l of depletion of DO in the blank). Seeded dilution water
should be used the day it is prepared..
Dilution Of sample : When the BOD value is expected to be more than 5.0 mg/l,
dilution of the sample is necessary neutralized at pH 7.0. the
sample should be free from residual chlorine. If it contain
chlorine then sodium sulphade should be added . Make several
dilutions of the prepared in DO. Depletion in DO should not be
less than than 2 mg/ L and dissolved oxygen should not be less
than 1 mg/L after 5 days. Generally following dilutions are
suggested
0.1 to 1 % for strong trade waste
1 to 5 % for raw and settle waste / sewage
5 to 25 % for oxidized effluent
25 to 100 % for polluted river water
Procedure for BOD set up : Select a definite volume of sample (less than 300 ml), add to
BOD bottle and fill completely with dilution water. All
concentrations should be in duplicate. Keep one bottle of each
concentrate in the BOD incubator for 5 Days at 200C and subject
the duplicate of that concentration to do determination on the
same day. That will be O – Day do. After 5 days do. Similarly put
one or two bottles for finding out the depletion of DO in blank
(Seeded dilution water only). Find out the difference in
between O day Do and 5 day DO values.
Result :
Conclusion :
Experiment No
Aim : To determine the Chemical oxygen demand (COD ) of given sample.
This is determined by refluxing the sample with an excess of potassium
dichromate in a highly acid conditions and estimating by titration the amount of
dichromate used. With a reducing agent like ferrous ammonium sulphate.
Theory : The COD is used to measure of oxygen equivalent of organic matter contain
of sample i.e. susceptible to oxidation by a strong chemical oxidant. For ex.
Specific source. COD can be related empirically to BOD organic carbon or
organic matter. The test is useful for monitoring and controlled after
correlation has been established. The dichromate reflux method is prefer to
procedure using other oxidants because of superior oxidizing ability,
applicability to wide varieties of samples and each of the manipulation
oxidation of most organic compound is 95 to 100 % of the theoretical value.
Principle : Most types of organic matters are oxidized by the biolling mixtures and
chromic and sulphuric acid . A sample is reflux in strong acid solution with
the known excess amount of potassium dichromate. After digestion the
reaming unreduced K2Cr2O7 is treated with ferrous ammonium sulphate
(FAS )to determine the amount of K2Cr2O7 consumed and oxidasible organic
matter is calculated in term of oxygen equivalent . Mercuric sulphate is
added to remove inference of chlorides. Silver sulphate is added as a catalyst
as it catalyst oxidation of long chain alphatic compounds.
Interference: Chlorides – 1mg/l Cl- exerts 0.23 mg/l of COD. There fore correction as mg/l
Cl- x 0.23 should be applied the COD of Cl- from the total COD. Nitrites
exert COD of 1.1 mg/mgN.
Limitations: Amino nitrogen gets converted to ammonia nitrogen. All organic compounds
with few exceptions (e.g. aromatic hydrocarbons, straight aliphatic
compounds and pyridine) are oxidized by this procedure.
Reagents:
i) Standard potassium dichromate 0.25 N
ii) Conc. H2SO4 (A.R. Grade)
iii) Ferroin Indicator – Dissolve 1.485gm 1-10 phenanthroline monohydrate together
with0.695 gm ferrous sulphate (FeSO4, 7H2O) in distilled water and dilute to 100 ml.
iv) Catalyst – Silver Sulphate ( for 8 straight chain sulphatic compds) mercuric sulphate
(for Cl-).
v) Sulphomic acid – Required only if the interference of NO2 is to be eliminated. Add 10
mg sulphamic acid/mg NO2 – N if present, in the refluxing flask. (Do not forget to add
in blank also in this case)
Procedure: Place 50 ml sample or aliquot diluted to 50 ml with distilled water in a 300 ml
round bottom refluxing flask with ground glass joint. Add 25 ml K2Cr2O7 and 75 Conc.
H2SO4 gently shake. Attach refluxing condenser and reflux the mixture for 2 hr. After
refluxing wash the condenser with distilled water. Cool the mixture. Dilute the mixture
with distilled water. Titrate with ferrous ammonium sulphate (0.25 N) with ferroin
indicator till the red colour apprers after the intermediary green colour
Note: -
1. While refluxing if the colour changes to green discard the mixture as
potassium Dichromate is not sufficient to oxidize the solution.
2. For small volumes i.e. 10, 20, 30, 40 ml of samples, proportionate
reduction of potassium Dichromate & sulphuric acid may done)
Calculation:
COD mg/l = (A-B) N x 8000 / V
Where A = Volume in ml. Ferrous ammonium sulphate for blank
B = Volume in ml. Ferrous ammonium sulphate for Sample
V = Volume of sample
N = Normality of ferrous ammonium sulphate
Experiment No
Aim To prepare filter sand from the stock sand and determine effective size and
uniformity coefficient
Theory Natural run –of – bank sand may be too coarse or too fine for a projected filter.
Within economical limits, specified sizing and uniforming can be obtained by
screening out coarse grains and washing out fines. To get the purified water , the
sand shoud have specific properties i.e. D10 , D60.
Formula :
Pusable = 2 ( P60.- P10 )
Ptoo fine = {P10 – 0.2 (P60.- P10 ) }
Ptoo coarse = {P10 + 1.8 (P60.- P10 )}
Procedure Wash the sand and then filter the stock sand by arreging the various screens. Shake
the screens for the 20-30 minutes and the measure the wt of sand retained on each
sieve. From the data calculate the % retained on each sieve . Plot the graph by taking
% finer on ‘Y’ axis and diameter of grain size on ‘ X’ axis. From the graph find out
the value of D60 and D10. Assume the value of coefficient of sand ( CU) in the range
of 1.3-1.8. calculate the Pusable, Ptoo fine , Ptoo coarse .
Experiment No
Aim : To determine the Available Chlorine and Residual Chlorine in a Given Water
Sample
Theory :
Chlorine determination includes:
a) Available chlorine in case of chlorine solution, bleaching powder or chlorine tablets.
b) Chlorine demand (assessment of the requirement of the quantity of chlorine to be added).
c) Residual Chlorine- i) Free residual during Break Point chlorination, ii) Total combined during
Break point Chlorination.
Apparatus: Chlorine Determination Kit (Colour Comapatometer)
a) Available Chlorine (Bleaching Powder):
Reagents:
ii) Bleaching powder solution: Make a paste of 1 g. bleaching powder (CaCl, OCL, H2O) in
minimum water and dilute the paste with distilled water to a volume of 100 ml. Take care
to see that the paste is transferred tot eh volumetric flask quantitatively.
iii) 0.025N sodium Thisulphate: 6.25 g. Na2S2O3, 5H2O is dissolved in 1 liter of distilled water.
iv) Glacial acetic acid.
v) Potassium iodide crystals.
vi) 0.1 N potassium iodate solution: 812 mg dissolved in 250 ml. distilled water.
vii) Starch indicator: 5 g soluble starch mixed with little water and ground in a pestle and
mortar so as to prepare a paste. Paste is than transferred quantitatively to 1 liter of boiling
water. Mixture is then allowed to settle overnight and the supernatant is used.
Procedure:
i) Take 10 ml of bleaching powder solution in a conical flask and add to it KI crystals.
Sufficient distilled water and approximately 2 ml of glacial acetic acid mix.
ii) Titrate the sample till dark amber colored solution turns to pale straw color.
iii) Add starch indicator and Mix.
iv) Titrate till the blue colored starch iodide complex becomes colorless.
v) Prepare reagent blank using distilled water. Note the volume of thiosulphate required.
Calculations:
1 ml of 1 N Thio = 35.45 mg Cl2
1 ml of 0.025 N Thio = 35.45 x 0.025
= 0.88625 or Say 0.89
Interference:
Unsaturated organic compounds, Fe2+ Mn2+, NO2, organic nitrogen and NH3 are the main
interfering substances.
These can be eliminated by changing the sequence of regent additions using break point
chlorination.
Apparatus:
Chlorine determination kit (color comparator) to measure residual chlorine.
Reagents:
1. Orthotolidine: Dissolve 1.35 g orthotolidine dihydrochloride in 500 ml distilled water.
Add it to a mixture of 350 ml distilled water + 150 ml Conc. HCl. Store in a colored
bottle.
2. Sod. Arsenite: Dissolve 5 g NaAsO2 and dilute to 1000 ml.
3. Standard chlorine solution: Prepare chlorine solution from bleaching powder and
determine its strength as described in the test for available chlorine. This solution has to
be prepared freshly.
Procedure:
1. Take identical aliquots of 100ml well water in 12 conical flasks or bottles (stoppered).
2. Add chlorine solution in increasing quantity to the bottles or flasks to result in a concentration
in the range of 0.1 to 3.00 gm/l. Mix well.
3. Allow to stand for predetermined contact period usually 30 to 60 min.
4. Determine the residual chlorine present in each bottle by OT test as described.
5. Plot chlorine residual Vs chlorine added and determines chlorine required at breakpoint. This
will give the chlorine demand of that specific water.
6. This can also be determined by measuring free residual chlorine left after contact period. The
dose where 0.2 mg/l free residual chlorine is left out will give the amount of chlorine required
to disinfect the water.
ZONE ZONE ZONE
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5 7.5
CHLORINE DOSE
Zone 1 : Major reaction in between Cl2 & NH4+
Zone 2 : Formation of dichloramine & the further
oxidation of it
Zone 3 : Free residual Cl2
Reaction : Cl OH
| |
i) –C = C – + HOCL - C – C – (unsaturated organic compounds)
| | | |
H H H H
Mg/l ml Ml
I 0.01 0 0.8
II 0.02 0 2.1
IV 0.04 0 4.3
Calculation:
a) Free residual chlorine (as Cl) mg/l = FR-B1
b) Total residual chlorine (as Cl) mg/l = TR-B2
c) Combined residual chlorine (as Cl) mg/l = (TR-B2) - (FR-B1)
Range:
The method is applicable up to 5 mg/l of chlorine.