University Francisco Jose de Calda

DETERMINATION OF NITROGEN, FERTILIZER phosphorus and potassium in INORGANIC

Maria Fernanda lasso 20162150305, Cristian Delgado 20171150034
Inorganic Analysis - Professor Alvaro Jimenez

SUMMARY
The following report the results of the analysis of the sample is presented in this case this is
an inorganic fertilizer of unknown origin, to determine what type of fertilizer will be
compared with tables of percentages obtained and different analytical tests as performed
Kjeldahl method (for nitrogen) and atomic absorption analysis (potassium) and finally
volumetric analysis (for phosphorus).
KEYWORDS: Quantitative Determination sample, fertilizers, Kjeldahl nitrogen, atomic
fósforo.absorción, volumetry.

INTRODUCTION: mineral fertilizer or chemicals are

● fertilizers
A fertilizer is a type of substance or
nutrient call also in soluble and
assimilable by plant roots chemical
forms, to maintain and / or increase the
content of these elements in the soil.
Plants do not need complex compounds
of vitamins or amino acids essential to
human nutrition, and synthesizing all they
need. They only require tens of chemical
elements which must be in a form that the
plant can absorb, these elements are
(PO5), (S-SO4), (CaO), (PO5) (N (HN4))
(N) free .
1. Classification:
1. organic fertilizers and minerals:
organic fertilizers are products derived
from plants or animals that meet the
minimum characteristics required.
products obtained by chemical processes
developed on an industrial scale. Usually
it is obtained by synthesis inorganics.
2. simple and compound fertilizers:
fertilizers may contain one or more of the
primary nutrients (N, P, K). Fertilizers
according to the reference element
containing nitrogen fertilizers as (N),
phosphate (P) or potassium (K) becomes.
Compound fertilizers when they are
obtained by simple mixing roughly made
of simple components. When it develops
products with more than one chemical
combination of nutrients but using several
main products often called complex
fertilizers. In any case can be
distinguished within complex, or
compound fertilizers or binary or ternary
fertilizers according which contain two or
three of the above, independent of any
other nutritional elements could element.
3. solid fertilizers: these may be
powdered, crystallized, (product obtained
by solidification of very fine droplets
which are sprayed from the top of a tower An "incomplete" would label as fertilizer
of "granules") granulate or pearlescent. (0-0-60) and (0-46-0) since it would only
be one of the three main nutrients.
4. Liquid fertilizers: is more or less
Another example would be incomplete
concentrated solutions which may contain
fertilizer (0-20-20) as one of the three
one or more nutritional elements such as
nutrients missing.
fertilizer. The most common are ternary
compound fertilizers are suspensions and Fertilizers also have "relationships"
solutions nitrogen liquid. indicating the relative amounts of
nutrients together. For example, a
For this research you may possibly have 4
fertilizer (10-10 - 10) is a ratio of 1.1 - 1,
types of cover fertilizers in the following
and a fertilizer (20-10 - 5) is the ratio (4-
table:
2-1.) Relationships may be useful in
ANASAC fertilizer - triple 15 finding the "perfect mix" for a particular
type of plant or situation. For example,
Compocion fertilizer ANASAC Compocion
percentages orchards with a ratio of (1-2-1), which
ANASAC would result in a fertilizer (5.10 - 5) or
total nitrogen (N) 15.0% (20/10/10). Most trees with a ratio of (2-
Ammoniacal Nitrogen (N) 9.0%
1-1), which would be a fertilizer or as a
(05.05.10 20.10.10) product. Lawns
NITRIC (N) 6.0%
preferred ratio fertilizer (3-1-2), so that a
Comparable phosphorus 15.0% fertilizer product with (10/20/30) on the
(PO5)
label would be a good value.
water soluble potassium 15.0%
(K2O) High analysis fertilizers (those with a
total calcium (CaO) 2.20% higher number on the label) would apply
total sulfur (S-SO4) 1,70%
to a lower rate for the same results. In
other words, 5lb fertilizer (20-20 - 20)
produce the same amount of actual
nutrients as 10 pounds of fertilizer (10-10
- 10.)
2. ID:
● Kjeldahl method
All fertilizers have three numbers on the
label indicating the fertilizer analysis, or In analytical chemistry, the Kjeldahl
"weight percent" of nitrogen, phosphorus method is a method for quantitative
and potassium, in that order. determination of nitrogen content in
organic substances more nitrogen
Therefore, a bag of 50 kg of fertilizer 20- compounds contained in inorganic
10 - 5 labeling containing 20% nitrogen (. ammonia and ammonium (NH3 / NH4 +).
10 lbs), 10% of available phosphate (5
pounds), and 5% soluble potassium (2.5 1. Part Two: Degradation
lbs ). In addition, this product is This method comprises preparing the
considered a "complete" fertilizer, since sample using sulfuric acid (H2SO4),
all three nutrients are present. some catalyst (selenium (Se), copper (Cu)
or mercury (Hg)) and a neutral salt
(Potassium sulfate (K2SO4)), the use of
acid is due to organic compounds in the
sample to produce ammonium sulfate
decomposes, the use of a catalyst is due
to its ability to reduce and use of the
neutral salt the increased boiling point of
the medium (337 ° C to 373 ° C).
Soil Sample+ H 2 S O4 →…
… ( N H 4 ) 2 S O4(aq )+ C O2 (g )+ S O2 (g) + H 2 O (g )
Figure 1 shows degradation
2. Part Two: Distillation
After the process of decomposition of the
sample, a small amount of sodium
hydroxide (NaOH) is added to obtain,
finally, the ammonia contained in the
reaction product in the first part.
( N H 4 ) 2 S O4 (aq )+ 2 NaOH → …
… N a2 S O 4(aq) +2 H 2 O ( l) +2 NH 3( g)
3. Part: Capture ammonia
After addition of the addition of sodium
hydroxide (NaOH) ammonia (NH3) is
drawn into the receiving vessel by a
stream of water vapor.
The receiver for the distillate container is
filled with an absorbent solution to
capture the ammonia gas dissolved, the
most common solution used absorbent is
boric acid (B (OH) 3) in an aqueous
solution of 2% - 4% concentration.
( OH )
−¿¿
B (OH )3 + H 2 O+ N H 3 → N H +¿+B 4 ¿
4
For this part can also be used sulfuric acid
(H2SO4) in place of boric acid (B (OH)
3).
+¿¿
H 2 SO 4 (TOTAL) +2 N H 3 → S O 2−¿+2 NH 4 ¿
4
Figure 2 Distillation and capture of ammonia (NH3)
4. Part: Qualification
4.1 Direct titration:
When boric acid (B (OH) 3) is used as the
absorbing solution, an assessment is
carried out using a standard sulfuric acid
(H2SO4) or hydrochloric acid (HCl) and
various indicators solution, the range of
concentrations the solution is 0.01 N to
0.5 N based on the amount of ammonia
(NH3).
−¿+ HX → X +B ( OH ) + H2 O ¿
B (OH )4

−¿; etc¿
HX = strong acid (X =)Cl−¿; S O 4 ¿
4.2 Back - Titration:
When sulfuric acid (H2SO4) is used as
the absorbing solution, the residual
sulfuric acid (H2SO4) (excess does not
react with ammonia (NH3)) is titrated
with a standard solution of sodium
hydroxide (NaOH) and the amount
ammonia (NH3) is calculated by
difference.
+ ¿+2 H 2 O ¿
H 2 SO4 ( RESIDUAL) +2 NaOH → S O2−¿+2 Na
4 For determination of phosphorus:
5. Part: Calculation of grams
nitrogen obtained.
Here to this part, we can calculate this in
two ways:
5.1 Using the concentration of titrant acid
and the volume is used to find the
equivalent-gram of sample:
V HCl∗[ HCl N ] =Eq−g of N H 3
5.2 Using this equation to calculate the
milligrams of nitrogen:
mg of N=V HCl∗[ HCL N ]∗14 g N
6 Part: Calculation of the percentage
of nitrogen
For this part, the calculation of nitrogen
in the soil sample which can be done in
two ways:
1. With equivalent-grams in grams
H ∗14 gN
gN 3
17 gN H 3
%N= ∗100∗6.25
g of sample
2. With milligrams nitrogen (N)
mg of N
%N= ∗100 %∗6.25
mgof sample
● volumetric analysis
Volumetric analysis is a quantitative
analytical method widely used. As the
name suggests, this method involves
measuring the volume of a solution of
known concentration is used to determine
the analyte concentration.
¿
of It is to dissolve the sample and precipitate
in an acidic phosphorus as ammonium
phosphomolybdate. The precipitate, after
neutralization, is treated with an excess of
sodium hydroxide solution. Phosphorus
becomes ammonium phosphate and
sodium hydroxide excess (NaOH) is
titrated with acid solution. consumption
of sodium hydroxide is proportional to
the phosphorus content in accordance
with the following reaction:
The spectroscopy atomic absorption
(often called AA or AAS spectroscopy,
by atomic absorption spectroscopy) is an
instrumental method analytic chemistry to
measure specific concentrations of a
material in a mixture and to determine a
variety of elements. This technique is
used to determine the concentration of a
particular element (theanalyte) In a
sample and can be determined over 70
different elements in solution or in solid
samples directly used in pharmacology,
biophysics toxicological research.
MATERIALS:
● Kjeldahl method
For this practice we have used reagents
and equipment found at university, so we
tube for Kjeldahl digestion, Kjeldahl
equipment digestion Erlenmeyer flask,
pipette, burette clamps burette soil
sample, distilled water, sulfuric acid
( H2SO4), potassium sulfate (K2SO4),
copper sulfate (CuSO4), hydrogen
peroxide (H2O2) andmix indicator
● volumetric analysis
hydrochloric acid (HCl), nitric acid
(HNO3), barium chloride (BaCl2),
ammonium hydroxide (NH4OH),
ammonium molybdate ((NH) ₂MoO₄),
distilled water, sodium hydroxide
(NaOH) was used to practice and
phenolphthalein indicator, plate heaters,
beakers, Erlenmeyer flask, volumetric
flask, glass Rod, pipettes, burettes,
Burette Clamp, universal stand, filter
funnel, filter paper and a metal ring.
METHOD:
● Kjeldahl method
1. We begin cleaning the tubes for
Kjeldahl digestion with distilled water
to avoid errors during the process.
2. 1 gram of sample was weighed and
fertilizer inserted into the digestion
tube without touching the walls.
3. 2 grams of potassium sulfate (K2SO4)
are weighed too and are introduced
into the digestion tube without
touching the walls.
4. 0.1 grams of copper sulfate (CuSO4)
too weighed and placed in the
digestion tube without touching the
walls.
5. 5 milliliters of sulfuric acid (H2SO4)
are token and placed in the digestion
tube without touching the walls.
6. A few drops of hydrogen peroxide
(H2O2) are token and placed in the
digestion tube without touching the
walls.
7. After this we introduced the sample
prepared in Kjeldahl digester and wait
until the machine reached 340 ° C.
8. Machine added 15 ml of sodium
hydroxide (NaOH) for ammonia
(NH3).
9. Ammonia (NH3) is distilled with
steam trawls and received in an
Erlenmeyer flask with boric acid (B
(OH) 3) 4%.
10. After this the sample is titrated to find
the equivalent-gram of nitrogen and
then calculate the percentage.
● Volumetric analysis:
1. 1 g of sample in 15 ml of aqua
regia is dissolved and heated for
30 min.
2. It was allowed to cool the sample
to room temperature and excess
 barium chloride added to remove
sulphates present in the sample.
3. The sample was heated for
another 20 min.
4. Precipitated barium sulfate is
filtered to ensure that we have the
sulfate ion.
5. ammonium hydroxide added and
then acidified with nitric acid to
prepare the acidic environment
and favor the reaction with
ammonium molybdate.
6. ammonium molybdate is added
until the reaction stops.
conventional methodology for analysis of
a sample of fertilizer about 5 g of sample
are perfectly homogenates were used, the
extraction of potacion (k) starting
compound for Realizer KCl realize
atomic adsorption the following dilutions
were made:
1) Calculation for utlización for the KCl
in sample
100 mg k∗0,1 ( 7439KClk )∗( 99,5
100 %
%)
=190,6 mg

7. It produces a precipitate which is

then filtered, washed and then
redissolved in water with a little
phenolphthalein.
V 1= ( 50 ml∗100
100 ppm
ppm
)=5 ml
8. Later excess sodium hydroxide to
the color change of Preparation for the solutions in the balls
phenolphthalein was added. 25 ml and were added 10 mL of aqua
9. excess sodium hydroxide is regia to dissolve. The mixture is diluted
titrated with the same with distilled water
concentration HCL.
10.
Dilutions presents on every ball
ATOMIC ABSORPTION
Sample preparation
V 1= ( 25 ml∗10 ppm
100 ppm )
=2,5 ml

one. 5 g were taken fertilizer powder,

calision for 10 min, to remove the sample
from the crucible, put in a dry
enlenmeyer.
V 1= ( 25 ml∗0,2
10 ppm
ppm
)=0,5 ml
two. 10 ml of HCl were added and 10 ml
H2O e3 was boiled for 30 min, until the
V 1= ( 25 ml∗0,4
10 ppm
ppm
)=1 ml
sample is dry and evaporate.
3. Finally the sample was filtered, and the
solution that was saved disolovio in
HNO3
V 1= ( 25 ml∗0,8
10 ppm
ppm
)=2 ml
Finally, aliquots of the balls to take,
analyze with atomic absorption machine,
✔ Grams of NH3
the results are interpreted with the
following equations 17 g N H
[ABS] = K * [C]. + K0
0.2 meq−g N H 3
( 1000 meq−gN H 3
)
=3,4∗10−3 g N H
3

K0 = 0.0000, K1 = 0.2126 ✔ Percentage of N

14 gN

%=
3,4∗10−3 gN H 3 ( 17 gN H 3 )∗100 %∗6.25=1,75 % of N
1 g of Fertilizer
RESULTS:
Then we 2.625% N in 10 ml and 100 ml:
● Nitrogen Determination
After Kjeldahl digestion solution was
100 mL∗ ( 1,7510%mLof N )=17.5 % of N
performed in an Erlenmeyer flask with
100 ml of boric acid (B (OH3)) at 4% ● Using 5.2 Via:
concentration and ammonia (NH3) it was
obtained. ✔ Milligrams nitrogen
m g N =0.1 N HCl∗2 m L HCl∗14 g N =2.8 m g N
After this we titrated 6 aliquots of 10 ml
with hydrochloric acid (HCl) [0.5 N] and ✔ Percentage of Nitrogen
the following results were obtained: 2.8 m g N
%N = ∗100 %∗6.25=1.75 % of N
1000 of Fertilizer
No. ml aliquot ml of HCl
Aliquot Same as the method we 5.1 2.625% N in
10 ml and 100 ml:
one 10 ml 2 ml
two 10 ml 2 ml 100 mL∗ ( 1.7510%mLof N )=17.5 % of N
3 10 ml 2 ml
● Determination of Phosphorus
4 10 ml 2 ml
He added sodium hydroxide 12.6 in the
5 10 ml 2 ml concentration of 0. 34N and subsequently
6 10 ml 2 ml be evaluated retro with hydrochloric acid
of the same concentration namely sodium
Average: 10 ml 2 ml hydroxide in excess, so the milliliters of
Table 2 Quantities of HCl Wasted waste acid are milliliters of sodium
hydroxide excess.
Calculation of the percentage of N:
● Fashion using 5.1:
✔ Milliequivalents of NH3 Then in excess NaOH it is:

0.1 N∗2 m L NaOH =0.2 . meq−g N H 1.8 ml of HCl = 1.8 ml NaOH excess
3
Then the volume of NaOH reacted:
NaOH 12.6 ml Total - 1.8 ml of NaOH
excess = 10.8 ml of NaOH formed Na
(NH4) PO4
g Na (NH4) PO4:
10.8 m L NaOH∗0.34 N NaOH =3.67 meq−g Na ( N H ) HP O 4 4

3.67 meq−g Na ( N H 4 ) HP O 4 ( 10001 eq−g

meq−g )

139.3 g Na ( N H
( 2 eq−g
4 ) HP O4
)=0.253 gNa ( N H 4 ) HP O 4

Burn time samples

g P:

30.97 g P
0.253 g Na ( N H ) HPO
4 4
( 138.3 g Na ( N H ) HP O
4 4
)
=0.057 g P

% D.E.P: Calibration curve for k

0.057 g P ( 1001 g% )=5.7 % P

Absorptions and concentrations in the

calibration curve for the potassium

[ABS] = K * [C]. + K0
K0 = 0.0000, K1 = 0.2126

ATOMIC ABSORPTION potassium concentrations found

[ABS] = K * [C]. + K0
Cleared concentration k ● Determining the amount of potassium
in the sample was not possible
k =¿= [K] / 100 =%
because most are instrumental
methods.
k= ( [ 0,3932[0,0534 ]
] .+ 0,2126 )
= 0.088 k /100 =
CONCLUSIONS:
8.7%
Among all possible fertilizers that we
[0,0520]
k= (
[ 0,3824 ] .+0,2126 )
=0,0873 k / 100 = may have, we conclude that we have
17.5% N% P 5.7% K 8.73 because values
8.7% nearly nitrogen and phosphorus are not
diverted so as the rest of fertilizer found
k= ( [ 0,3878[0,0527]
] .+ 0,2126 )
=0,08777 k / 100 in the tables, but may be a triple
percentages Anasac 15, the method could
= 8.7%
not be as successful, the purity of the
The final concentration of potassium reactants, it is evident in the percentage of
present in the fertilizer, is 8, 73% nitrogen, as the reagents used for this
were of analytical grade.

ANALYSIS OF RESULTS: BIBLIOGRAPHY:

Based on the following table are ● Kjeldahl J. (1883) "Neue Methode

obtained the following percentages
Element % Found in
Fertilizer
N 17.5%
P 5.7%
K 8.73%
● Not have an accurate value in
determining percentage of nitrogen
can be connected directly with a
minimal loss of ammonia at the time
of the distillation of the sample.
● Nor have an accurate value in
determining percentage of phosphorus
it can be related to a loss of sample at
the time of removing filter paper.
zur Bestimmung des organischen
Stickstoffs in Körpern" (New
method for determination of
nitrogen in organic substances),
Zeitschrift für Chemie
analytische, 22 (1): 366-383.
● Julius B. Cohen Practical Organic
Chemistry 1910
● Reagents AppliChem Panreac
ITW. (Sf). Nitrogen determination
by Kjeldahl method. Retrieved
from ITW Reagents:
https://www.itwreagents.com/uplo
ads/20180122/A173_ES.pdf
● University of Valencia. (Sf).
Nitrogen determination by the
method KJELDAHL. Retrieved
from
https://www.uv.es/gidprl/practica_
Kjeldahl/index.html
● Vazquez, MV (June 19, 2015).
Learn online now. Obtained
fromhttp://aprendeenlinea.udea.ed
 u.co/lms/ocw/mod/page/view.php
?id=170&inpopup=1
● JP SELECTA SA (October 10,
2012). METHOD Kjeldahl
method / KJELDAHL. Retrieved
from JP Selecta SA - Application
Notes:http://www.grupo-
selecta.com/notasdeaplicaciones/si
n-categoria/metodo-kjeldahl/
● NTC 234: 1996 or fertilizers. Test
method for the quantitative
determination of phosphorus.
● NTC 202: 2001, quantitative
methods for determination of
soluble potassium petticoat in or
fertilizers of materials for their
manufacture.

● Chemical cable. (Sf). Volumetric

analysis. Wired obtained from
Chemical:
http://www.wiredchemist.com/che
mistry/instructional/laboratory-
tutorials/volumetric-analysis