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Kjeldahl procedure involves digestion and distillation. When soil is heated with sulfuric acid and catalyst mixture, organic N is digested to Ammonium-N. Then the concentration of ammonia is measured by volumetric titration in the presence of an indicator after steam distillation under the alkaline condition.
Kjeldahl
procedure involves digestion and distillation. When soil is heated with
sulfuric acid and catalyst mixture, organic N is digested to Ammonium-N. Then
the concentration of ammonia is measured by volumetric titration in the
presence of an indicator after steam distillation under the alkaline condition.
Apparatus
and reagents
·
Kjeldhal distillation assembly
·
Titration Apparatus
·
Distilled water
·
Beaker
·
Conical flask
·
Burette and pipette
·
Graduated cylinders
·
Catalyst mixture
·
Sulphuric acid (concentrated)
·
Sodium hydroxide solution (40%)
·
Zink granules.
·
Boric acid cum indicator solution-
·
Hydrochloric acid (0.1N)
Procedure
·
Weigh 10 gm of air-dry soil/sediment in a
300 ml round bottom flask
·
Add 20 gm of catalyst mixture and 35 ml of
sulphuric acid.
·
Heat the contents from bottom of the flask
for about 2 hours.
·
Cool the contents (digest) and add about
100 ml of distilled water,
·
Wait for about 5 minutes, and deliver the
supernatant into 1liter distillation flask A of Kjeldhal distillation assembly.
·
Wash the residue with a little of
distilled water several times and transfer the supernatant each time to the
same distillation flask.
·
Add 100 ml of sodium hydroxide solution
and a few granules of zinc.
·
Take 25 ml of boric acid cum indicator
solution in a 500 ml Erlenmeyer flask B and place it below distillation
assembly so that the lower open ends of the condenser are dipped in solution.
·
Heat the distillation flask on a hot plate
and collect about 150 ml of distillate in flask B.
·
Remove the flask with distillate and
titrate the distillate (which has turned blue due to dissolution of ammonia)
against 0.1N hydrochloric acid. Turning of blue colour to light brown-pink
indicates the end point.
·
Run distilled water blank in the same
manner.
·
Calculation
% N=[(a-b)/s]*M*1.4*mcf
Where:
a: ml of HCl
required for titration sample
b: ml of
HCl required for titration blank
s: air-dry
sample weight in gram
M: Morality
of HCl
1.4: 14x10-3x100%
(14 atomic weight of Nitrogen)
mcf: moisture correction factor
References
1. George E., Rolf S., John R.; Methods of Soil, plant and water analysis;3rd
ed; p65
2.Sadhan C. Anand Dev G.; Handbook of Water, air and soil analysis; international E publication;2014
3.Haluschak P. Laboratory
Methods of Soil Analysis Canada-Manitoba Soil Survey,
April 2006