UNIVERSITY DISTRITAL FRANCISCO JOSE OF CALDAS

FACULTY OF SCIENCES AND EDUCATION

MASTER IN CHEMISTRY

2013

AUTORS: Diana Roa García* Jesenia Rodríguez 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 Kjeldahl method comprises three

main phases:
The nitrogen can reach the ground from
organic inputs and bacterial * Digestion of the sample: The sample
attachment, once you set the ground is is subjected to digestion by heating with
used by plants, animals and sulfuric acid and a mixture of salts
microorganisms that incorporate it into which accelerate and facilitate the
their tissues. The cycle is completed oxidation of organic matter and the
once these organisms die, so the conversion of all forms of nitrogen in N3
nitrogen re-enters the soil, this process +, which in acid medium radical are as
always begins with simple organic ammonium (NH4 +) thus leading to
compounds (NH4 +, NO2-, NO3-, N2, organic forms of nitrogen mineral forms.
NH3) and ends with complex organic
compounds; after returning * Distillation: Once it has all the nitrogen
decomposition stage simple (NH4 +) the sample is exposed to a
compounds. strong base of sodium hydroxide to
form ammonium hydroxide, which when
If there is lack of nitrogen in the soil, subjected to heat decomposes into
microorganisms will strongly affected ammonia (NH3) and water.
growth and on the contrary there is
abundant levels of the same, * Rating: The ammonia released by the
accelerated bacterial growth and decay, reaction is collected in a known volume
increasing ammonia production of boric acid is titrated with hydrochloric
problems and usable nitrogen escaping acid or sodium hydroxide as the case
into the atmosphere; most soils the and by comparison with a white
relationship between C and N is close determines the amount of acid that
to 10:1 maintaining balance, normal reacted with NH3.
nitrogen content varies from 0.05 to 2% MATERIAL AND EQUIPMENT
in its various forms.
* Soil sample dried and ground with a For samples that containing nitrates.
mortar. Add 5 mL of concentrated sulfuric acid,
2 g of K2SO4 and 0.1 g CuSO4. Stir
* Analytical balance. gently to mix thoroughly. And we
proceed to have the pipe in the digester
* Kjeldahl flasks.
until the solution clarifies (digestion end
* Beakers. when the sample color is blue-green
light, the process will take
* Specimens. 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
* Boiling stones.
prevent loss of this ammonia and a
* Pipette. steam trap so that the tip of the
condenser is immersed in an
* Burette. Erlenmeyer flask containing 25 ml of
boric acid solution to 4 % w / v, 2-3
* Universal support clip.
drops of methyl red to 0.2% w / v.
SOLUTIONS AND REAGENTS
Are added pumice granules to prevent
*Mp=0,2 g bumping, leans the ball and add 20 mL
of sodium hydroxide solution 35% w / v,
*H2SO4= 5 ml concentrated or enough to make alkaline medium
and check that all joints are well done.
*K2SO4= 2 g
The digested mixture will become dark
*CuSO4= 0,1 g (blue-gray or dark brown). If it changes
color add more NaOH.
*NaOH= 20 ml 35%
Then heated until all the distilled
*H3BO3= 25 ml 4% ammonia (150 mL of distillate
minimum) to the flask containing boric
PROCEDURE acid and tested with litmus paper pink
Determination of nitrogen by the until ammonium negative result. With
Kjeldahl method drawing the distillate outlet tube, rinsing
the exterior of the tube in the distillate
Digestion to prevent entrainment of steam.

Weigh soil sample of 0.2 g, previously Titration_ Degree

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.
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 sodium hydroxide as the reaction
by X milliequivalents of base 14 (the that occurs is related to the titration
equivalent weight of N). of the excess boric acid as set forth
ANALYSIS AND RESULTS the following equations:

Assessing the distillate with HCl until H3BO3 =H+ + H2BO3 (1)
the color shift. Given that Mol of HCl =
Mol of NH3 = Mol of N in the sample H2BO3=H+ + HBO3 (2)
Mol of H2SO4 = NH3 = 2Mol, 2Mols of
N in the sample. HBO3-= H+ + BO3 (3)

Table No. 1. data Hydroxide holder is shifting the

equilibrium equation 2, where as if
Prueb volumen hydrochloric acid is titrated with the
a equilibrium shifts according to
Vol1 0,2 ml equation 1, it is advisable to perform
acid titration as the dissociation
Vol2 0,1 ml
constant for this equilibrium is
Vol3 0,2 ml greater than in Equation 2 and incur
fewer errors.
X 0,166 ml
Tabla 4.9 Criteria for assessing soil based on its
Note: the acid titrant dilution was total nitrogen content
performed, so that the final (Moreno, 1978).
concentration is 0.037 N.

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)
El porcentaje de nitrógeno
V = volume of acid consumed (ml) contenido en la muestra de suelo se
calcula a partir de la siguiente
14 = Atomic weight of nitrogen. expresión:
0.037 Nx0, values approaching 166
mlx14

mg N = 0.1036 mg

Assessing the sample may be

Where:
performed with hydrochloric acid or
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.