Determination of Total

EXPERIMENT 4 DETERMINATION OF Available Nitrogen in a

Soil Sample
TOTAL AVAILABLE
NITROGEN IN A SOIL
SAMPLE

Structure
1. Introduction
Objectives
2. Principle
3. Requirements
4. Solutions Provided
5. Procedure
6. Observations and Calculations
7. Results

4.1 INTRODUCTION
In the previous experiment you learnt how percent organic matter in the soil can be
determined by wet oxidation method. The present and next three experiments are
related to the analysis of soil for some of its nutrient elements. In Unit 3 of Block 1
you read about various macro and micronutrients present in soil and the
dependence of soil productivity on these. It is important to analyse nutrients present
in a soil sample so as to gauge its productivity level and recommend suitable
remedial measures in case of any imbalance of these nutrients. In this experiment
you would learn and perform the determination of nitrogen.

Nitrogen, an important plant nutrient is present in the soil in both organic as well as
inorganic forms. The organic component of the soil nitrogen is present primarily as
plant, animal and microbial remains and as such is unavailable to plants. It
becomes available through mineralisation and organic matter decomposition
processes. In fact, the organic form of nitrogen in the soil can be visualised as a
reservoir of nitrogen and reflects the nitrogen supplying capacity of the soil. Only a
minute fraction say about two percent gets mineralised due to microbial activity in
the growing season.
The
plantsinorganic
in (NH component of the
) - N and (NO 
) -soil nitrogen
N forms andisreflects
presentthe
in extent
the form
of of ammonium
mineralisation.
(NH ), nitrate 4 (NO ) and nitrite3 (NO ) ions. Of these, nitrogen is taken up by
The amount
4 of nitrogen in3these forms is an indicator
2 of the nitrogen
availability for the current crop and in turn determines the immediate requirements
of N- fertilizer.

Determination of nitrogen in the soil is done in a number of ways depending on

whether the objective is to determine total nitrogen content or individual
components
like, organic nitrogen or (NH  ), - N, (NO  ) - N or (NO  ) - N or their
combinations.
4 3
2
In this experiment you will learn to determine total available ( or mineralisable)
nitrogen from the organic matter using alkaline potassium permanganate method.
As mentioned above, it is a measure of nitrogen reservoir or the nitrogen supplying
Objectives
capacity of the soil.
After studying and performing this experiment, you should be able 29
to:
Experiments  explain different types of nitrogen availability in the soil,
 explain the principle and procedure involved in the potassium
permanganate method of total available N determination, and
 interpret the nitrogen value in terms of nitrogen supplying capacity of the
soil .
4.2 PRINCIPLE
The easily hydrolysable and oxidisable fractions of organic nitrogen present in a soil
sample can be extracted out using alkaline KMnO4 - a mild oxidising agent. For this
purpose a known amount of soil sample is boiled with a measured quantity of alkaline
KMnO4. It leads to evolution of ammonia which is absorbed in a known volume of standard
sulphuric acid. A part of the acid is neutralised by ammonia and the excess is titrated
with a standard solution of alkali using methyl red as indicator.
This method gives the amount of available nitrogen content as the percent of the soil.
This value is also expressed in terms of Kg/ha. For this purpose it is assumed that 1
ha of furrow slice (0-15cm) of the soil weighs 2.24 million kg. If the amount of
available nitrogen is found to be less than 272 kg/ha. the sample is rated low, if it is
272-
544 kg/ha, it is rated medium and if the available nitrogen content is more than
544 kg/ha it is rated as high.

4.3 REQUIREMENTS
Apparatus Chemicals
1. Kjeldahl flask (800 cm )
3
1. Potassium permanganate
2. Distillation apparatus 2. Sodium hydroxide
3. Measuring cylinder 3. Sulphuric acid
4. Pipette 4. Methyl red indicator
5. Burette
6. Conical flas k

4.4 SOLUTIONS PROVIDED

You will be provided with these solutions. However, if required these can be
prepared by the following procedures:

1. 0.32% KMnO4 : Weigh 3.2 g KMnO4 and transfer it to a 1 dm3 or 1000 cm3
volumetric flask. Add some distilled water to the flask and dissolve it by
gently swirling the flask. Carefully make up the volume to 1 dm3.

2. 2.5% NaOH : Weigh 25 g of NaOH pellets and transfer to a 1 dm3 graduated

beaker or measuring cylinder. Dissolve it in distilled water and carefully make up
the volume to 1 dm3.

3. 0.02 M NaOH: Dissolve about 1.0 g of NaOH pallets in water in a standard

flask or a measuring cylinder. Standardise by titrating against 0.01 M oxalic acid
using methyl red indicator. Adjust the strength to 0.02 M.

4. 0.01 M H2SO4 : Carefully add 0.6 cm3 of concentrated H2SO4 (sp. gr. 1.84) to one
dm3 of distilled water. Standardise by titrating against a standard alkali solution
using methyl red indicator. Adjust the strength to 0.01 M.

5. 0.15% methyl red indicator : Dissolve 0.15 g of methyl red powder in 50 cm3 of
ethyl alcohol and make up the volume to 100 cm3 with water.

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 Determination of Total
4.5 PROCEDURE Available Nitrogen in a
Soil Sample
Perform the following steps to determine total available ( mineralisable) nitrogen in
a soil sample.
1. Set up the distillation apparatus with the help of your counsellor.
2. Weigh 20 g of given soil sample and transfer it carefully into Kjeldahl distillation
flask.
3. Moisten the sample with about 10 cm3 of distilled water. Wash down the soil
adhering to the neck of the flask.
4. Add 100 cm3 of 0.32% KMnO4 solution and 100 cm3 of 2.5% NaOH solution
and a few glass beads or broken pieces of glass rod to avoid bumping to the
above sample and immediately stopper the flask.
5. Take 25 cm3 of 0.01 M H2SO4 in a 150 cm3 conical flask and add 3-4 drops of
methyl red to it. Dip the end of the delivery tube of the distillation apparatus
into it.
6. Heat the distillation flask steadily to distill 100 cm3 of liquid ammonia in about
30 minutes time.
7. Titrate the excess of standard H2SO4 left in the conical flas k with 0.02 M NaOH
and note the volume used (X cm3 ) in the observation table.

4.6 OBSERVATIONS AND CALCULATIONS

Observation Table

Weight of soil taken = 20 g

25 cm3
Volume of 0.01 M H2SO4 =

Volume of 0.02 M NaOH required for back ---------------- cm3

titration = X cm3

Volume of 0.01 M H2SO4 used by NH3 evolved ---------------- cm3

= (25  X) cm3

Calculations
3
1 cm of 0.01 M H2SO4 = 0.00028 g of nitrogen
Amount of nitrogen in 20 g of soil = (25 X) 0.00028 g = Z g
% available nitrogen ( per 100 g of soil) = Z  100/20 % = Z’
% Available nitrogen in ppm = Z’  10,000
Available nitrogen in Kg/ha = Z’  22400

4.7 RESULTS
The amount of available nitrogen in the given sample of soil =
……… Kg/ha

The soil sample on the basis of its available nitrogen value is rated

as: low / medium / high. ( Tick the appropriate option)

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