UNIVERSITY DISTRITAL FRANCISCO JOSE OF CALDAS

FACULTY OF SCIENCES AND EDUCATION

MASTER IN CHEMISTRY
2013
AUTORS: Diana Roa Garca* Jesenia Rodrguez Zapata*
DETERMINATION OF NITROGEN IN SOIL SAMPLE
INTRODUCTION
Nitrogen is an essential element in the life processes of many organisms, as it is part of the
main biomolecules of all living things, it is for this reason that it is one of the most abundant
elements on earth and constitutes 78% of the atmosphere, despite these high rates the amount
of nitrogen present in the soil is low because it depends directly on the dynamics and
biogeochemical cycling. This nitrogen can reach the ground thanks to the fixing organic inputs
and bacterial activity from the air, In this experimental practice is to study the level of nitrogen in
a soil sample by the micro method Kjeldahl.

Key words: nitrogen, digestion, distillation, titration.

THEORETICAL FRAME
The nitrogen can reach the ground from
organic
inputs
and
bacterial
attachment, once you set the ground is
used
by
plants,
animals
and
microorganisms that incorporate it into
their tissues. The cycle is completed
once these organisms die, so the
nitrogen re-enters the soil, this process
always begins with simple organic
compounds (NH4 +, NO2-, NO3-, N2,
NH3) and ends with complex organic
compounds;
after
returning
decomposition
stage
simple
compounds.
If there is lack of nitrogen in the soil,
microorganisms will strongly affected
growth and on the contrary there is
abundant
levels
of
the
same,
accelerated bacterial growth and decay,
increasing
ammonia
production
problems and usable nitrogen escaping
into the atmosphere; most soils the
relationship between C and N is close
to 10:1 maintaining balance, normal
nitrogen content varies from 0.05 to 2%
in its various forms.

The Kjeldahl method comprises three

main phases:
* Digestion of the sample: The sample
is subjected to digestion by heating with
sulfuric acid and a mixture of salts
which accelerate and facilitate the
oxidation of organic matter and the
conversion of all forms of nitrogen in N3
+, which in acid medium radical are as
ammonium (NH4 +) thus leading to
organic forms of nitrogen mineral forms.
* Distillation: Once it has all the nitrogen
(NH4 +) the sample is exposed to a
strong base of sodium hydroxide to
form ammonium hydroxide, which when
subjected to heat decomposes into
ammonia (NH3) and water.
* Rating: The ammonia released by the
reaction is collected in a known volume
of boric acid is titrated with hydrochloric
acid or sodium hydroxide as the case
and by comparison with a white
determines the amount of acid that
reacted with NH3.
MATERIAL AND EQUIPMENT

* Soil sample dried and ground with a

mortar.
* Analytical balance.
* Kjeldahl flasks.
* Beakers.
* Specimens.

For samples that containing nitrates.

Add 5 mL of concentrated sulfuric acid,
2 g of K2SO4 and 0.1 g CuSO4. Stir
gently to mix thoroughly. And we
proceed to have the pipe in the digester
until the solution clarifies (digestion end
when the sample color is blue-green
light,
the
process
will
take
approximately 120 minutes).

* Digester.
* 1 L volumetric flask

Distillation

* 1 L Erlenmeyer flask

Kjeldahl flask immediately connect to

the coolant as quickly as possible to
prevent loss of this ammonia and a
steam trap so that the tip of the
condenser
is
immersed
in
an
Erlenmeyer flask containing 25 ml of
boric acid solution to 4 % w / v, 2-3
drops of methyl red to 0.2% w / v.

* Boiling stones.
* Pipette.
* Burette.
* Universal support clip.
SOLUTIONS AND REAGENTS

Are added pumice granules to prevent

bumping, leans the ball and add 20 mL
of sodium hydroxide solution 35% w / v,
or enough to make alkaline medium
and check that all joints are well done.
The digested mixture will become dark
(blue-gray or dark brown). If it changes
color add more NaOH.

*Mp=0,2 g
*H2SO4= 5 ml concentrated
*K2SO4= 2 g
*CuSO4= 0,1 g
*NaOH= 20 ml 35%
*H3BO3= 25 ml 4%
PROCEDURE
Determination of
Kjeldahl method

nitrogen

by

the

Digestion
Weigh soil sample of 0.2 g, previously
spray, place it on a filter paper, fold the
paper being careful not to lose any of
the samples and place it in a dry
Kjeldahl flask, taking care that the
sample does not adhere to walls or
flask neck.

Then heated until all the distilled

ammonia (150 mL of distillate minimum)
to the flask containing boric acid and
tested with litmus paper pink until
ammonium negative result. With
drawing the distillate outlet tube, rinsing
the exterior of the tube in the distillate
to prevent entrainment of steam.
Titration_ Degree
Titration with methyl red indicator.
Distillate is titrated with 1 N HCl
solution, using 2 drops of methyl red as
indicator until the color changes from
yellow to pink each equivalent of NaOH
used corresponds to an equivalent of
NH3 or an equivalent of N in original

sample. The weight in mg of N is given

by X milliequivalents of base 14 (the
equivalent weight of N).

that occurs is related to the titration

of the excess boric acid as set forth
the following equations:

ANALYSIS AND RESULTS

H3BO3 =H+ + H2BO3 (1)

Assessing the distillate with HCl until

the color shift. Given that Mol of HCl =
Mol of NH3 = Mol of N in the sample
Mol of H2SO4 = NH3 = 2Mol, 2Mols of
N in the sample.

H2BO3=H+ + HBO3

(2)

HBO3-= H+ + BO3

(3)

Table No. 1. data

Prueba

volumen

Vol1

0,2 ml

Vol2

0,1 ml

Vol3

0,2 ml

0,166 ml

Note: the acid titrant dilution was

performed,
so
that
the
final
concentration is 0.037 N.

Hydroxide holder is shifting the

equilibrium equation 2, where as if
hydrochloric acid is titrated with the
equilibrium shifts according to
equation 1, it is advisable to perform
acid titration as the dissociation
constant for this equilibrium is
greater than in Equation 2 and incur
fewer errors.
Tabla 4.9 Criteria for assessing soil
based on its total nitrogen content
(Moreno, 1978).

Calculated by the following equation

nitrogen content:

mg N = N x V x 14
where:
N = normality of the acid titration
(1N HCl dilution carried dilution factor
triplicate 0.33 0.037 N)
V = volume of acid consumed (ml)
14 = Atomic weight of nitrogen.

El
porcentaje
de
nitrgeno
contenido en la muestra de suelo se
calcula a partir de la siguiente
expresin:

0.037 Nx0, values approaching 166

mlx14
mg N = 0.1036 mg

Assessing the sample may be

performed with hydrochloric acid or
sodium hydroxide as the reaction

Where:

T = ml of spent clorhidric acid in the

sample.
B = ml of clorhidric acid in the white
worn.
N = exact normality of clorhidric
acid.
S = weight of the soil sample.
Nitrogen=1.162%
CONCLUSIONS
According to the table is reported
that the nitrogen content is
extremely rich as it is greater than
0.221%, however it is not possible to
determine a possible use for this is
unknown ground as the carbon

content and the pH so that it is

recommended for soils which
contain a high content of nitrogen
that
would
accelerate
the
metabolism of many organisms of
great importance in the life cycle of
the system.
It is important to note that in this
case the evaluation was performed
without the determination of the
target, which is why the percentage
of nitrogen is quite high, although
this result the nitrogen content may
be taken as a reference value to
establish useful use of it, such as in
extremely poor soils in nitrogen is
recommended to subject the sample
to new studies, mainly carbon.