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Aim :

Experiment No
To determine the sulphate content of the given water sample

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.

Apparatus:

1) Magnetic stirrer
2) Klett summerson colorimeter or spectro photometer
3) Measuring spoon

Reagent:
a) Conditioning reagent Mix 50 ml glycerol with a solution containing 30 ml
conc. HCL, 300 ml distilled water, 100 ml 95% ethyl alcohol and 75 gm
sodium chloride.
b) Barium chloride crystals AR grade.
c) Standard Sulphate solution Prepare by diluting 10.41 ml of the standard 0.02
NH2SO4

to 100 ml with distilled water.

Procedure:
a) Formation of barium sulphate turbidity Measure 100ml

sample or a suitable

aliquot made up to 100ml into a 250ml Erlenmeyer flask. Add exactly 5 ml


conditioning reagent and

mix in the stirring apparatus. While the solution is

being stirred add a spoon full of barium chloride crystals stir


b) Measurements of barium sulphate turbidity Immediately after the stirring period
is over, pour some of the solution into the absorption cell of the photometer and
measure the absorption at fifth minute. Maximum turbidity is usually achieved
within 2 min. and the reading remains constant there after for 3-10 min.
c) Read mg SO4 present in the sample on the calibration curve prepared by standard
solutions,

Calculation:

mg / l SO42- = mg SO42- x 1000 / ml sample


Conditioning
2-

Reaction - SO4 + BaCl2

BaSO4
SO4Solution

Result :

Experiment No
Aim

: To determine the chloride content (Avgentometric method) in the given


water samples.
: Chloride in the form of chloride Cl ions, is one of the major inorganic

Theory :

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.

Reagents

: i) Chloride free water: Demonized water


ii) K2CrO4 indicator: Dissolve 50 gm in distilled water. Add AgNO3
solution till a definite red precipitation is formed. Allow to stand for 12
hours filter. Dilute the filtrate to 1 liter D.W.
iii) Standard AgNO3 (0.0141 N): Dissolve 2.395 gm in distilled water and
dilute to 1 Liter. 1ml of standard silver nitrate (0.0141 N) is equivalent to
500g Cliv) Standard NaCl (0.0141 N): Dissolve 824.1 mg water and dilute to 1 lit.
1ml of this solution is equivalent to 500g Cl-.

Procedure:

: i) Use 100ml or a suitable aliquot diluted to 100ml with distilled water.


ii) If the sample is colored, add 3ml Al(OH)3 wash combines the filtrate
and washing.
iii) Check the pH and adjust it to near neutrality.
iv) If sulphide, sulphite or thiosulphate is present, make the water alkaline
to Phenolphthalein with NaOH. Add 1ml H2O2, stir, neutralize with
H2SO4.
v) Titrate the sample with AgNO3 after adding 1ml K2CrO4 to the sample
till orange red color appears.
vi) Run the blank taking distilled water as the sample.

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 500g Cl- or 0.5mg Cl-

Formula :
(A-B) x 0.5 x1000
-

Mg/l Cl =
ml of sample

Where

Reaction:

A = ml titrant of sample
B = ml titrant for blankV
Cl- + AgNO3 -- AgCl+ NO3
K2CrO4 + 2AgNO3 -- Ag2CrO4 + 2KNO3

If pH> 8.3 - Ag (OH) 2, is precipitated,


If pH < 7 Cr2 O7, is precipitated.
Ksp AgCl = 3 x 10-10, Ksp Ag2CrO4 = 5x 10-12

Observation Table :
S.N

(A-B) x 0.5 x1000

Type of sample
-

Mg/l Cl =
ml of sample

Result:
Conclusion :

Experiment No

Aim

: To determine Biochemical oxygen demand ( B.O.D.)of given


water samples

Theory

: BOD is the amount of O2 required by microorganism for stabilizing


biologically decomposable organic matter in water sample under
aerobic condition. It is mainly used to determine pollution load of
the waste water, degree of pollution in lake or stream and the
efficiency of waste water treatment system.

Principle :

: The method consist of airtight bottle of specified size overflowing


with sample and incubating at specified temperature for five days.
Dissolved oxygen ( D.O.)of blank and sample is measured and BOD is
calculated using the formula. It is necessary to provide standard
condition such as nutrients, pH, temp and mixed group of organism is
seed for determination of BOD. Temperature is controlled at 20O C. The
test is conducted for 5 days as 70 to 80 % is stabilized during the period.

Apparatus

Specially prepared BOD glass bottles provided with exactly fitting


ground glass stoppers and surrounding well to accommodate 5 ml of
water so as to exclude exchange of gases. BOD incubator working at
200C.

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 solution22.5gm 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.

Calculations

5- BOD mg/l = Initial DO (mg/l) 5 day DO (mg/l)

Reaction

CnHaObNc + (n+a/4 b/2 3/4C)O2 - CO2 + (a/2 3/2C) H2O +


NH3

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