GRAVIMETRIC DETERMINATION OF MOISTURE AND

PHOSPHORUS CONTENT IN FERTILIZER SAMPLE

A.J.E.TABUSO
DEPARTMENT OF MINING, METALLURGICAL AND MATERIALS ENGINEERING, COLLEGE OF ENGINEERING
UNIVERSITY OF THE PHILIPPINES, DILIMAN QUEZON CITY, PHILIPPINES
DATE PERFORMED: FEB 3, 2015
INSTRUCTORS NAME: ELLA DOLIENTE

ABSTRACT
In the growth of plants, they will need phosphorus to help develop cells and
moisture that brings the phosphorus, with other nutrients, to the plant through the
roots. This experiment was conducted to determine the moisture in a fertilizer
sample by constant weighing and to determine the phosphorus (P) content of the
fertilizer sample using precipitation gravimetry. Precipitation gravimetry is a
method under gravimetric analysis which uses weights of solids to determine the
amount of a sought species or by adding precipitating agent/s to form a precipitate
which was digested, filtrated, heated, cooled, and weighed. In the conducted
experiment, a fertilizer sample weighing 3.0225 grams undergone precipitation
gravimetry and it was determined that 0.625% of it is moisture while 5.006% is
phosphorus. Compared to the theoretical values of %P there is an error of 42.64
which is a high percentage of error but it is relatively same to the data of the other
researchers; therefore, it can be said that the experiment is a success.

INTRODUCTION
Phosphorus is one the essential
needs of plants for their growth. It
helps in cell division and development
of new tissues. Without it, the growth
of a plant and its roots are stunned.
This is the reason why fertilizers
contain phosphorus together with the
other components, and these are
carried by soil water or moisture which
will eventually be absorbed by plants
using their roots [4].
For
this
experiment,
the
moisture and the phosphorus content
of a sample fertilizer is determined by
gravimetric
analysis,
specifically
precipitation gravimetry. Gravimetric
analysis is considered a quantitative

analysis which uses the weights of

solids. It is done to determine the
amount of an analyte, or the sought
species, in a mixture or solution by
adding a precipitating agent, also
referred as the precipitant. Then, a
precipitate will be formed containing
the sought species. The precipitate will
be isolated by filtration and heated,
usually at about 110 C, to expel any
liquid content before measuring its
weight [1].
It also includes a process known
as constant weighing which is done, at
least in this experiment, in weighing
the container of the sample. Constant
weighing is basically heating an
object, in this case the crucible, for
1

some time at about 110C, then

placing it in a desiccator before
weighing it in an analytical balance.
After recording the weight, it will be
heated again and the process is to be
repeated until the obtained mass
reading is relatively constant [3].

weight ppt
P 2 O 5=

FW P2 O5
FW MgNH 4 PO 4 6 H 2 O
100
weight sample

(3)
METHODOLOGY

When
it
comes
to
the
precipitate in precipitation gravimetry,
it must be easy to separate with the
solution by filtration; and to do that,
the precipitate of particles must be big
enough. It must also have low
solubility to prevent it from dissolving
back into the solution. The suspended
particles of the precipitate are also
allowed to settle before filtering, this is
known at digestion [2].

The experiment are mainly

divided into three parts: (A) the
constant weighing of the crucible, (B)
the analysis of moisture in the
fertilizer sample, and (C) the
precipitation of Magnesium
Ammonium Phosphate Hexahydrate
(MgNH3PO46H2O).

Since fertilizers are soluble in

water making it easy for plants to
absorb nutrients through their roots
a precipitant is to be used to
precipitate phosphorus, P, in the form
of magnesium ammonium phosphate
hexahydrate,
MgNHPO6HO,
as
shown in the chemical equation

A slightly ajar crucible was

placed in an oven set at 110C for at
least 24 hours. With the use of
crucible thongs, the crucible was
placed in a desiccator. After 15
minutes, the weight of the crucible
was determined using an analytical
balance. Then, it was placed back to
the oven at 110C for another 30
minutes. This process was repeated
until the crucible weight readings of
the analytical balance remained
constant.

5H2O(l) + HPO42-(aq) + NH4+(aq) +

Mg2+(aq)+OH-(aq) MgNH4PO46H2O(s)
(1)
Then, from the weight of the
precipitate, which is MgNHPO6HO,
the percentage or phosphorus, P, and
phosphorus pentoxide, P2O5, can be
calculated by using the equation:

weight ppt
%P=
(2)
;and,

A. Constant Weighing of the Crucible

B. Moisture Analysis in the Fertilizer

Sample

FW P
With the use of the analytical
FW MgNH 4 PO 4 6 H 2 O
100
balance, roughly 3.0 grams of the
weight sample

fertilizer was placed in the crucible,

which previously went under constant
weighing. The crucible containing the
sample was placed in an oven at
110C with the cover slightly ajar.
After an hour, the crucible was
transferred into a desiccator and was
cooled for 15 minutes. Then, the
2

crucible, with the sample, was

weighed in an analytical balance. After
obtaining its weigh, it was brought
back to the oven at 110C for 30
minutes. This process was repeated
until the analytical balance displayed
constant readings of the weight of the
crucible containing the sample.
C. Precipitation of MgNH3PO46H2O
A filter paper was weighed and
placed in a desiccator. The fertilizer
sample in the crucible was transferred
into a 250-mL beaker. 40 ml of distilled
water was poured into the beaker.
Since not all solids dissolved in the
water, the mixture was filtered
through a filter paper (different from
the weighed filter paper) to obtain a
clear solution. Then, 45 mL of 10%
Magnesium sulfate heptahydrate was
added to the clear filtrate followed by
the slow addition of 150 mL of 2 M
ammonia. The solution was left to
complete its precipitate for 15
minutes. After allowing the complete
precipitation, the mixture was filtered
through the pre-weighed filter paper.
After filtration, the precipitate was
washed with 5 mL of distilled water
twice before washing it with 10 mL of
95% ethanol for two times as well. The
filter paper

RESULTS AND DISCUSSIONS

In
the
beginning
of
the
experiment, constant weighing of the
crucible was done. This process was
necessary for securing that there was
no moisture in the crucible which may
affect its weight since moisture may
be vanished while the experiment was
being conducted. The weight of the
crucible used in this experiment was

44.36995 grams after undergoing

constant weighing (Table 1.1).
After obtaining the fertilizer
sample and its weight, which was
3.0225 grams, the sample was heated
to expel any moisture content in the
fertilizer sample. It was assumed that
the fertilizer to have moisture since
fertilizers needs moisture which will
add up with the soil to dissolve the
nutrients in fertilizers, making it easy
for plants to obtain such nutrient
through their roots [4]. The sample was
grinded before being placed inside the
oven to make sure that the sample is
in fine particle size which will allow
more moisture particles to escape
from the sample. Aside from heating
the sample in an oven, it was also
cooled in a desiccator which absorbed
any moisture left in the sample. After
getting rid of the moisture, the mass
of the sample was decreased to
3.0036 grams (obtained weights
summarized in Table 1.2).
In the experiment, all weighing
processes are done using an analytical
balance and weights are obtained by
difference and not direct weighing
because the analytical balance is very
sensitive that it can be affected with
even the moisture content. By using
the difference of mass readings for
obtaining mass of a species, the setup will be remained unchanged while
the material to be weighed will be the
only one that will cause any change in
the measurement readings [5]. By this
method in weighing, the mass of
moisture in the fertilizer is the
difference of the wet, or initial, mass
of sample and the dry, or heated,
mass of sample
wet sample wt -dried sample wt =
%moisture (4)

which leads to 0.01890.0004 grams

of moisture in the fertilizer sample,
3

and it is equivalent to 0.6250.01% of

the sample.
After determining the moisture
content of the fertilizer sample, it was
dissolved in water to make the sample
aqueous
so
that
precipitation
gravimetry would be possible to apply
on it. The first step in gravimetry is to
add the appropriate precipitant/s to
have a precipitate which contains the
sought species [5]. In the experiment,
the precipitants used are 10%
magnesium sulphate heptahydrate
(MgSO47H2O) and Ammonia (NH3) to
precipitate magnesium ammonium
phosphate
hexahydrate
(MgNH4PO46H2O). To satisfy the
precipitate
requirement
for
gravimetry, which is to have bigger
particles for easier precipitation, the
NH3 was added slowly while the
solution
is
continuously
stirred
allowing
particle growth
to be
favoured rather than nucleation as
pointed out by the Von Weimarns
Relative Supersaturation Ratio:
(Q-S)/S
(5)
by
keeping
Q
(species
concentration) low. Also, stirring the
solution prevents the precipitation of
magnesium hydroxide (Mg(OH)). To
make sure that the formed precipitate
will be easier to filter, digestion was
done. This allowed the fine particles of
the precipitate to settle at the bottom
of the beaker and form particles which
are slightly larger, due to the
adsorption of a particle with the other
particles, for easier filtration [1]. But
this might cause impurities to occur,
which is why the precipitate was
washed with water and 95% ethanol,
which is sufficiently volatile to be
easily removed when being dried.
When the precipitate dried, its weight
was obtained and the percentage of
phosphorus in both wet and dry basis

of the fertilizer sample was calculated

using equation (2). Similarly, the
percentages of phosphorus pentoxide
in wet and dry basis were computed
with equation (3) to get the data in
Table 1.3.
Table 1.3 Percentage Values
of P and P2O5 in Fertilizer Sample
Species
P in wet basis
P in dry basis
P2O5 in wet basis
P2O5 in dry basis

Percentage
5.0060.001
5.0370.001
11.4700.002
11.5430.003

Meanwhile,
the
theoretical
percentage of P2O5 is 20%. This will
make the theoretical percentage of
phosphorus in the fertilizer sample to
be 8.727%. As compared to the data
in Table 1.3, there are differences in
the final data implying that errors
were made during the experiment
which affected the data.
The experiment was sensitive
due to the fact that there are a lot of
possible errors that the researchers
might have done which will affect the
data. One of which is the possibility
that the crucible or weight filter paper
was accidentally touched. The body
fluids, like sweat or oil can add
moisture to the set-up and affect the
weights, due to the sensitivity of the
analytical balance. Another is when
the crucible broke in the middle of the
experiment. This basically means that
the experiment must be started all
over again. Also, carelessness in
transporting the crucible, or filter
paper, or even just in drying processes
may have caused some solids to be
blown away, which will reduce the
accuracy of the weight.
CONCLUSION
RECOMMENDATION

AND

In this experiment, the set-up

has a high risk of damage which can
reflect to the data and results.
Considering that the theoretical value
of %P2O5 is 20% of the sample, while
for %P, the theoretical value is
8.727%. Comparing these values to
the data in Table 1.3, there is a big
difference. Expressing these into
percent errors, there will be an
average of 42.47 % error. This might
be a high percent and it is enough to
say that the experiment is a failure r
error but compared to the data of the
others, the %P and %P2O5 values are
close to each other. This might
suggest that the actual values are
close to the data recorded and that it
is actually a success.
The data might have been
better
if
the
experiment
was
conducted with more caution. An
example is in transferring of crucible.
By accidentally holding the crucible
with bare hands or breaking the
crucibles, the experiment must be
repeated from the very beginning for
accuracy. Also, when moving with the
filter paper containing the precipitate,
the paper must not be touched with
bare hands, and movements should
not be too sudden, to prevent spilling
and generally loosing precipitate
particles which will affect the accuracy
of the experiment.

REFERENCES
[1] Rattenbury, E.M. Introduction to
Titrimetric and Gravimetric Analysis.
Pergamon Press Ltd., London. 1966.
[2] Treadwell, F.P. Analytical Chemistry
vol. 1. Braunworth & Co., Brooklyn.
1916
[3] Khopkar, S.M. Basic Concepts of
Analytical
Chemistry.
New
Age
International Ltd. 1998
[4] Plant and Soil Sciences eLibrary.
Soils-Part 6:Phosphorus and Potassium
in
Soil.
http://passel.unl.edu/pages/informatio
nmodule.php?
idinformationmodule=1130447043&to
picorder=2 (accessed Feb 24, 2015).
[5]
UC
Davis
ChemWiki.
8B:Pecipitation
Gravimetry.http://chemwiki.ucdavis.ed
u/Analytical_Chemistry/Analytical_Che
mistry_2.0/08%3A_Gravimetric_Metho
ds/8B%3A_Precipitation_Gravimetry
(accessed Feb 23, 2015).

APPENDIX
Table 1.1 Constant Weighing
Material
Crucible Weight 1
Crucible Weight 2
Average

Crucible with Sample

Weight 1
Crucible with Sample
Weight 2
Average

Weight (g)
44.36980.000
2
44.37010.000
2
44.369950.00
03
47.37350.000
2
47.37350.000
2
47.37350.000
3

Table 1.2 Determination of Moisture

Weight of Empty
Crucible
Weight of Crucible
with Sample
Weight of Wet
Sample
Weight of Dried
Sample
Weight of Moisture
Percentage Moisture
Sample Calculations:

Mass of water=3.0225 g3.0036 g

moisture=

0.0189
100
3.0225
30.97 g
245.44 g
100
3.0225 g

1.199 g
%P(wet )=

44.369950.0
003 g
47.37350.00
03 g
3.02250.000
2g
3.00360.000
4g
0.01890.000
4g
0.630.01%

30.97 g
245.44 g
100
3.0036 g

1.199 g
%P( dry)=

141.99 g
245.44 g
100
3.0225 g

1.199 g
P2 O5 (wet )=

141.99 g
245.44 g
100
3.0036 g

1.199 g
P2 O5 (dry )=