Chapter 3

Methodology
3.1 Study area:

The study area is located at the bank of Tapi River between Adajan to Galteshwer in
Surat, Gujarat. This river is situated at 72º 38' to 78º 17' E longitudes and 20º 5' to 22º 3' N
latitudes. The Tapi river’s total length is about 724 km and drains an area of 25,200 square
miles (65,300 square km). The Tapi river is situated at the north part of the Deccan plateau and
south part of Maharashtra. The Tapi River flows along with its tributaries - the Purna Girna
and Panjhra which flows from the south in Maharashtra state.

3.2 Sample collection:

The sampling site was Adajan to Galteshwar at the Tapi river bank in Surat, Gujarat,
which was 47 km long. Approximately two samples were collected in between 1 km area. Total
100 samples were collected for the soil testing. The samples were collected mostly from the
outer surface of the river bank. The depth was (0-10) cm to study the anthropogenic sources
for different types of pollution as industrial pollution normally contaminate the upper layer of
the soil i.e. 0 - 40 cm.

A plastic spatula was used for the sample collection. The samples were collected in self
lock polythene bags with packing in double plastic bags. All the samples were collected in
December 2018 in 15 days. The collected soil samples were air dried for 5 days at room
temperature and then crushed with a wooden material crusher. After that it was sieved (2mm)
for analysis.
3.3 Method for physical parameter

3.3.1 Soil colour:

Requirement:

 Munsell’s soil colour chart

 Cardboard
 Soil sample

Procedure:

Soil color is usally expressed in terms of sybols as given in the munsell’s soil colour
chart. Spread the soil saple uniformly over acardboard sheet. And then compare the particles
of soil with munsell’s standard colour chart.the chip with which the soil colour matches is taken
out and the symbols indicated on the chart is noted which givens the colour of soil.

3.3.2 Soil pH:

Requirement

 Buffer tablet 4.0 pH

 Buffer tablet 7.0 pH
 Buffer tablet 9.2 pH
 Saturated potassium chloride

Procedure:

Calibrate the pH meter with Buffer solution. Take 10gm soil sample + 20 ml distilled
water after stirring half an hour check the pH of the reading on pH meter

3.3.3 Soil EC (Electrical Conductivity)

Requirement:

 Calcium sulphate anhydrous (Gypsum) (saturated solution)

 Potassium chloride (0.01N)
Make Reagent

 Calcium sulphate anhydrous (CaSo4):

5gm Caso4 + distilled water make final volume/litre then check the conductivity 2.2 ml
mohs/cm at 25° C.

 Potassium chloride (0.01N):

0.7456gm KCl + distilled water make final volume/litre then check the conductivity
1.14 ml mohs/cm at 25°C.

Procedure:

Calibrate the conductivity meter with CaSo4 solution or KCl solution 10gm soil sample
+ 20 ml distilled water after stirring half an hour then check the electrical conductivity of the
reading on conductivity meter.

3.4 Method for Chemical Parameter

3.4.1 Chloride

Requirements:

 Conical flask
 Pipettes
 Burettes
 Shaking machine
 Soil sample
Reagent:
 Potassium dichromate K2SO4
 Silver Nitrate

Procedure:

Take 10gm soil + add 100ml distilled water and dissolved. Filter and take 50 ml
suspension in the flask + add 2-drop K2SO4. Titrate with AgNO3 till red or pinkish yellow
coloured appear. Chloride is completely precipitated as AgCl and the first faint tinge of red
Ag2Cr persists.

% of Chloride =

3.4.2 Soil mineral:

Methods: EDTA titration method

Requirements:

 Soil sample
 Conical flask
 Burette
 Pipette

Reagents:

 Buffer (Ammonia buffer) solution =pH-10

 EBT indicator
 Murexide indicator
 2 N NaoH
 Std. EDTA

Procedure:

Take 50 ml sample + add 2 drops of buffer solution + 2 drops of indicator EBT + titrate
with EDTA solution till colour change from wine red to blue and stop titration when blue colour
produced.

3.4.3 Total organic carbon

Method: Walkley and Black rapid titration method

Requirement:

 Soil sample
 Sieves
 Pipettes
 Flask
 Reagent
 1 N-K2Cr2O7
 Phosphoric acid:85%
 Sulphuric acid
 Diphenylamine
 1 N-FeSO4

Procedure:

Take 1-2 gm a well ground soil sample in a 500 ml flask + add 10ml K2Cr2O7 + add
slowly 20 ml cons. H2SO4 and swirl the flask for 1 minute and keep I for about 30 minute for
digestion to take place + add 200ml D/W + 10ml of 85% H3PO4+ 1ml diphenylamine indicator
and titrate by FeSO4 from the burette until the solution is purple or blue + add FeSO4 slowly
in drops until the colour to bright green + add 0.5 ml of 1 N-K2Cr2O7 to restore an excess of
dichromate and complete the titration by adding FeSO4 drop by drop until the last trace of blue
colour disappears.

% of Organic Carbon =

Where,
A= Volume of K2Cr2O7 in ml
B= Volume of FeSO4 in ml
W=Weight of soil taken

3.4.4 Sulphate

Method: Gravimetric method with drying of residue

Requirement:

 Conical flask
 Pipettes
 Filter paper
 Weight balance
 Hot air oven

Reagent:

 HCL solution (1:1 dilution)

 Barium chloride solution (BaCl2)

Procedure:

Take water sample 50ml and heat the sample till boiling then start to boil, add 1ml HCL
in it + add warm BaCl2 solution until precipitates appear to be computed and then add about 2
ml BaCl2 solution excess and then filter the ppt with membrane filter paper and put the filter
paper in to the oven at 105° C and then find out the weight of ppt.

Sulphate =

Where,
W1= Pre weight of filter paper (g)
W2 = Post weight of filter paper (g)
411.6 = BaSO4/ SO4-2 Equaivalent

3.4.5 Calcium carbonate / Bicarbonate

Method: titration method

Requirement:

 Flask
 Pipettes
 Rotary shaker
 Funnel
 Filter paper

Reagent:

 Phenolphthalein indicator solution:

0.25% Phenolphthalein in 60% ethyl alcohol
 Methyl red / methyl orange:
Dissolve 0.5 g methyl red / methyl orange in 100 l of D/W
 Sulphuric / hydrochloric acid:
Dissolve 83 ml HCL and make up 1000 ml with D/W

Procedure:

Take 100 ml of the soil extract + add 2-3 drops of phenolphthalein indicator solution.
A red colour indicates the presence of carbonates. And titrate with 0.1 N HCL acid until the
colour just disappears. Now add 2 drops of methyl red/methyl orange indicator and continue
the titration until the colour just change, denoting the complete neutralization of the
bicarbonates present.

% of CO3-2= V1 × 0.030
% of HCO3-2= (V2-V1) × 0.0305
Where,
V1= Volume in ml of 0.1 N HCl acid used to neutralize 100 ml of the soil extract to the
phenolphthalein end point.
V2= Volume in ml of 0.1 N HCl for methyl red/ methyl orange end point.

3.4.6 Inorganic phosphorus

Method: Spectrophotometrically

Requirement:

 Funnel
 Filter pepper
 Evaporate plate
 Spectrophotometer
 Balance
 Soil sample
Reagent:

 Standard phosphate solution:

Dissolve 219.5 mg of potassium hydrogen phosphate (K2HPO4) in water and make up

the final volume to 1 litre with D\W.

 Vanadomolybdophoshoric acid reagent:

(1) 25g (NH4)2 MoO4 in 300ml D/W
(2) 1.25g NH4VO3 by heating to boiling 300 l water + 330 l conc. HCL cool the
solution
(3) Mixed (1) and (2) solution and make it up to 1000ml.

Digestion of sample:

Take 100 ml sample & digested with 2ml concentrated sulphuric acid & 5ml
concentrate nitric acid. Evaporate gently until white dense fumes are observed. If the solution
is coloured or turbid repeat addition of concentrate sulphuric acid & concentrate nitric acid till
it is colourless. Cool the solution & filtered, dilute to 1000 ml.

Procedure:

Prepare a series of standard ranging from 0.05 to 1.0 mg of phosphate by taking the
appropriate volumes of standard phosphate solution in a 100 ml S.M.F then add 10 ml of
Vanadomolybdophoshoric acid reagent and dilute to 100 ml. Allow to stand for 10 minutes for
full colour development and read the absorbance at 400-490 nm and draw a calibration curve
by plotting absorbance v/s mg of phosphate.

3.4.7 Organic nitrogen

Method: Kjedahl distillation titration method

Requirement:

 Kjeldahl distillation assembly

 Beaker
 Measuring cylinder
Reagent:

 Sodium tetra borate

 Sodium thiosulfate
 Ethyl alcohol
 Boric acid
 Sodium carbonate
 Sodium hydroxide
 Methyl blue
 Methyl red indicator
 Cupric sulphate
 Potassium sulphate
 H2SO4

Procedure

50ml sample + 50 ml digestion reagent. When observe white fumes. And then add to
300 l of D/W +add 50 ml NaOH-Na2S2O3 5H2O solution. Joint the round bottom flask with
distillation assembly. Take 50 ml of Mixed-Boric indicator in 100 ml beaker. Collect the
distillate till the mark of beaker to 100 l mark. Titrate with 0.02 N H2SO4 till the colour change
green to original colour of mixed-boric indicator.

N mg/L =

Where,
T1= Volume of H2SO4 titrant used against sample (ml)
T2= Volume of H2SO4 titrant used against distilled water Blank (ml)