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Organic Matter determination (Walkley -Black method)

Method · March 2020

DOI: 10.13140/RG.2.2.22043.00807

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Suraj Poudel
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 Organic Matter determination

(Walkley - Black method)

Written by: Suraj Poudel

BSc. Agriculture
IAAS, Paklihawa Campus
Date: 2020-3-15

Principle:

Oxidiable organic matter in the soil is oxidized by chromic acid in the presence of sulphuric
acid, the reaction being facilitated by the heat of dilution when 2 volumes of concentration
H2SO4 are mixed with 1 volume of K2Cr2O7 solution. The excess chromic acid is determined
by titration with ferrous ammonium sulphate (FAS) solution and the quantity of the substance
oxidized is calculated from the amount of dichromate reduced.

The highest temperature attained by heat of dilution of sulphuric acid is about 120°c, which is
sufficient to oxidized the active forms of soil organic C, but not the more inert forms of C
that may be present. From the experiments, 77 percent carbon were found to be recovered
and same figure was used in calculation. Also, the organic matter is considered to contain 58
percent carbon, and therefore multiplying factor 1.72 was used to convert organic carbon to
organic matter. Since no external heat is being utilized, finer soils passing through 0.2 mm sieve
is taken for the analysis.

This determined is affected by the presence of easily oxidizable substances like chloride, higher
oxidase of manganese and ferrous compounds. Whereas Fe+2 and Cl- give positive or high
value, the oxides of manganese give negative or low value. Soil samples air dried for 1-2 days
contain insignificant amount of soluble ferrous compound and chloride can be easily eliminated
by adding silver sulphate. According to Walkley-Black, normal soil contains invariably small
quantity of reducible oxides of Mn. Only in highly manganiferrous soils, small fraction of all
oxides is present in the active state capable of competing with chromic acid.

Apparatus Required:

1. 50 ml. burette

2. 10 ml. bulb pipette.

3. Measuring cylinder 25 ml or Acid Dispenser or pipette 20 ml capacity.

4. Conical flask 500 ml capacity.

Reagents Required:

1. Sodium fluoride (0.2 g)

2. 1N Potassium dichromate solution: - Dissolve 49.04 g of A.R. Potassium dichromate

(dried at 105°c) in distilled water and dilute to the mark in 1L volumetric flask.

3. 0.5 N Ferrous ammonium sulphate (FAS):- Dissolve 196 g of Fe (NH4)2(SO4) 26(H2O)2

in 800 ml distilled water and 20 ml concentrated sulphuric acid and dilute to 1L.

4. Diphenylamine indicator:- Approximately 0.5 g of reagent grade diphenylamine is

dissolved in 20ml of distilled water, add 100 ml of Conc. H2SO4.

Procedure:

a) Weigh 1gm soil sample, passing through 0.2 mm sieve and add exactly 10 ml of 1N
K2Cr2O7 solution to it, in a 500 ml. conical flask.

b) Add 20ml of concentration sulphuric acid and mix by gentle rotation for 1 minute, to
ensure complete contact of the reagent with the soil, but with care to avoid throwing up
soil to the sides of the flask.

c) The mixture is allowed to stand for 30 minutes.

d) A standardization blank (without soil) is run in the same way.

e) After half an hour, add about 200 ml of distilled water, 30 drops of diphenylamine
indicator and about 0.2 gm. of sodium fluoride.

f) Back titrate the solution with ferrous ammonium sulphate solution. The color is dull
green with chromos ion in the beginning, and then shifts to a turbid blue as the titration
proceeds. At the end point this color sharply shifts to brilliant green.

g) If over 8ml out of 10 ml chromic acid has been consumed during the titration, the
determination is repeated with a small quantity of soil or by adding double or treble
amount of K2CrO7 and H2SO4.

Calculation:

(B-S)*N*3*100*100*100 (B-S)*N
Organic matter % = = *0.67
Weight of soil*1000*77*58 weight of soil
 Where, B = volume of FAS used up for blank titration.

S = Volume of FAS used for sample titration.

N = Normality of FAS from blank titration

Wt = Wt. of soil sample.

Note:

i) Organic matter contains 58 percent carbon.

ii) Recovery factor for this method is 77 percent.

iii) Equivalent weight of carbon = 3.

Some photos captured during soil organic matter determination in Soil Laboratory at
IAAS, Paklihawa Campus

Photo 1: Weighing soil Photo 2: Diphenylamine Photo 3: Preparing

sample indicator dichromate solution
 Diphenylamine indicato

Photo 4: Making arrangement Photo 5: 0.5 N FAS solution Photo 6: Adding 30 drops of
for titration indicator to the sample solution.

Photo 7: End point (brilliant

green color)

Thank You!!!

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