GRAVIMETRIC DETERMINATION OF MOISTURE AND PHOSPHORUS

IN FERTILIZER SAMPLES

X. E. D. LEWIS
DEPARTMENT OF FOOD SCIENCE AND NUTRITION, COLLEGE HOME ECONOMICS
UNIVERSITY OF THE PHILIPPINES, DILIMAN QUEZON CITY, PHILIPPINES
DATE PERFORMED: FEBRUARY 10-17, 2015
INSTRUCTOR’S NAME:

ABSTRACT

The major component of fertilizer is given by NPK, namely nitrogen, phosphorus and potassium. The
weight declared for phosphorus is 30% in the form of P2O5. The moisture content of a fertilizer determines its
purity. To obtain the moisture and phosphorus content of a sample of fertilizer, gravimetric methods were used.
The moisture content was obtained from the difference of the weight of the wet and the dry sample, and was
found to be 0.7174 0.0003 %. The phosphorus content was determined through precipitation gravimetry
where the sample was reacted with MgSO4•7H2O and NH3 to form a white precipitate, MgNH3PO4•H2O. The
weight of the precipitate obtained was 1.1407 0.0003 g. Using stoichiometric calculations, the % P2O5 and % P
of the sample was calculated to be 22.556 0.0003 % and 14.428 ± 0.0003 % respectively with regards to the
wet sample, and 22.557 0.0003 % and 14.558 ± 0.0003 % respectively with regards to the dry sample.
This resulted to an estimate of 24.81 % difference with the 30% phosphorus claim.

INTRODUCTION measurement is by weight. Gravimetric

Plant foods and fertilizers are
commonly characterized by three letters,
NPK. NPK stands for nitrogen, phosphorus
and potassium respectively, and these are
important elements that support plant
growth. [3] Phosphorus in particular helps in
rapid growth, early maturity and enhances
the quality of vegetative crop growth. [4] The
amount of phosphorus in a fertilizer is
declared as 30 % in the form of P2O5. [3]
Another important factor to fertilizer is its
moisture content. The moisture content of
fertilizer determines its storage and its
purity. [5]
A method to determine the moisture
and phosphorus content of fertilizer is
through gravimetry. Gravimetry includes any
analytical method in which the ultimate
methods provide precise and accurate results
and have found a wide utility in chemical
analysis for many years and are best suited to
the determination of major constituents in
samples. It generally involves a known
solution reaction between analytes and
reagents to give sparingly soluble products
that can be weighed. [1] [2]
In this experiment, the moisture and
phosphorus content of fertilizer samples was
determined through gravimetry.
METHODOLOGY
Constant weighing of crucibles and cover
A crucible with cover was weight after
previously left in the oven at 110°C for two
nights. The crucible and cover was then
returned to the oven at 110 °C for 30 minutes
and then allowed to cool down in a desiccator

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for 15 minutes before it was weighed again.
This process was repeated until a constant
weight, with a minimum difference of 0.0002-
0.0003 g, was obtained from the crucible and
cover.
Gravimetric determination of moisture content
in fertilizer sample
An estimate of 3.0 g fertilizer sample
was weighed into the constantly weighed
crucible and cover. The crucible with the
sample, with the cover slightly ajar, was
placed in the oven at 110 °C for 1 hour. The
crucible was closed and allowed to cool down
in a desiccator for 15 minutes before it was
weighed again. The crucible with the cover
slightly ajar was then returned to the oven at
110 °C for 30 minutes, and then allowed to
cool down in a desiccator with its cover
closed for 15 minutes before it was weighed
again. This process was repeated until a
constant weight, with a minimum difference
of 0.0002-0.0003 g, was obtained from the
crucible and sample.
Determination of phosphorus in fertilizer
sample
The dried fertilizer sample was
dissolved in 40 ml distilled water. The
solution was then filtered using a filter paper.
The filtrate was reacted with 10%
MgSO4•7H2O and 150 ml of 2 M NH3, slowly
added, to form a white precipitate. The
mixture was allowed to stand at room
temperature for 15 minutes to complete
precipitation process. The precipitate was
then quantitatively filtered out using a pre-
weighed filtered paper and washed with 2
portions of 10 ml distilled water followed by
2 portions of 10 ml 95% ethanol. It left to dry
for 2 nights at room temperature and then
placed in an oven at 110 °C for 1 hour. The
filter paper with precipitate was weighed
after a fifteen minute cool down in a
desiccator.
RESULTS AND DISCUSSION
Gravimetry is a method where weight
is the ultimate source of quantitative data.
Thus, it is important to ensure that the
measured weight was from the sample and
not also from other external factors.
The first part of the experiment was
to determine the constant weight of the
crucible by removing the moisture it had
absorbed from the environment. This was
done through repeated oven drying and
weighing until a constant weight was
obtained. Every time the crucible was
removed from the oven, it was placed in a
desiccator. This prevents it from reabsorbing
moisture from the air. It was also weighed
after a fifteen minute cool down, allowing it to
acclimatize to room temperature. This
prevents the effects of dynamic buoyancy
inside the analytical balance when weight
measured. [3]
A constant weight was obtained when
a maximum difference of 0.0003 g was
observed between two successive weighing of
the crucible. This was because the analytical
balance used in the experiment had a
tolerance of 0.0002 g. The calculated
uncertainty reading between successive
measurements on this device was 2.8284 x
10-4 g which is approximately 0.0003 g. The
same analytical balance was used though out
the experiment. The crucible was used in
measuring the weight of the fertilizer sample.
Thus, by obtaining and maintaining the
crucible’s constant weight, its effect on the
measurement of the sample’s weight is
eliminated.
The fertilizer sample was then
dispensed into the crucible. The fertilizer
sample was pound into fine powder
beforehand. This increasing the particle’s
surface area and speeding up the drying
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process and other reactions that the sample
would be subjected to.
The sample’s weight was obtained
using weighing by difference. Weighing by
difference was done by obtaining two
measurements, one was the crucible’s
constant weight and the other was the weight
of the crucible with the sample, and then
subtracting the two weights. This prevents
contact of the sample with laboratory utensils
or weighing paper thus preventing the loss of
a portion of the sample which might adhere
to the utensil or paper. [2] It also limits the
introduction of moisture and into the sample.
The weight of the sample obtained was
3.6274 0.0003 g, which would be referred
to as the wet sample.
The wet sample with crucible was
subjected to repeated oven drying and
weighing until a constant weight was
obtained. The weight obtained was the “dry
weight” of the sample, where the moisture
from the sample would have evaporated. The
difference in the weight of the wet and dry
sample would be the amount of moisture
present in the sample. It was found that the
sample had a % moisture of 0.7471 .0003.
The dry sample was then subjected to
precipitation gravimetry in order to
determine its phosphorus content. It was
dissolved in water and reacted with 10%
magnesium sulfate heptahydrate,
MgSO4•7H2O, and 2 M ammonia, NH3, to form
a white precipitate which is magnesium
ammonium phosphate hexahydrate,
MgNH3PO4•H2O. The net ionic equation of the
reaction reaction is:
() ( ) ( )
(1)
( ) ( )
Ammonia, NH3, was added slowly to
control the acidity of the solution. If the
solution is too basic, PO43¯ will be formed
instead of HPO42ions and hydroxide ions will
precipitate with Mg2+ to form magnesium
hydroxide, Mg(OH)2. However, if the solution
is not basic enough, H2PO4¯ will be formed,
and no precipitate will occur. [3] Slow addition
of NH3 will prevent the co-precipitation of
Mg(OH)2.
The solution was left to stand to
complete the precipitation reaction before
the precipitate was obtained through
filtration. The precipitate was washed with
ethanol to purify the precipitate. It was then
dried and weighed. Using stoichiometric
calculations, the %P2O5 and %P was found to
be 22.556 0.0003 % and 14.428 ± 0.0003 %
respectively with the wet as a basis and 22.557
0.0003 % and 14.558 ± 0.0003 %
respectively with the dry sample as a basis.
This has an approximate percent difference of
24.81% with regards to the 30% phosphorus
claim.
CONCLUSION AND RECOMMENDATION
The calculated moisture content of
the fertilizer sample was 0.7471 .0003 %
which is a very low percentage. This would
mean that the product is pure because most
of the weight would come from the
composition of the fertilizer and not from
moisture.
The % phosphorus was also obtained
to be at about 22.556 0.0003 %. This had a
24.81 % difference. This means that the
phosphorus obtained through gravimetry
was less than the theoretical amount. This
could indicate that the fertilizer had less that
30% phosphorus despite its claim. It could
also indicate that the errors occurred during
the experimentation proper, such as the
incomplete precipitation of phosphorus in the
sample or the loss of precipitate during
filtration. Other methods can be used to
verify the results of this experiment, such as
the Karl Fischer method.
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REFERENCES
[1] Fifield; Kealey. Principles and Practice of
Analystical Chemistry, 5th ed; Blackwell
Science Ltd: London, U.K., 2002
[2] Kenkel, J. Analytical Chemistry for
Technitians, 3rd ed; CRS Press LLC: U.S.A.,
2003
[3] Eastern Michigan University.
https://www.emich.edu/chemistry/genc
hemlab/documents/10-phosphorus.pdf.
(accessed on 2 March 2015)
[4] Alberta Agriculture and Rural
Development
http://www1.agric.gov.ab.ca/$departme
nt/deptdocs.nsf/all/agdex920. (accessed
on 2 March 2015)
[5] Metlo-Toledo International Inc.
http://us.mt.com/us/en/home/applicati
ons/Laboratory_weighing/Moisture_fam_
browse_main.html. (accessed on 2 March
2015)
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 APPENDIX

Table 1. Constant Weighing of Crucible

Weight 1 45. 9581 0.0002 g
Weight 2 45. 9597 0.0002 g
Weight 3 45. 9591 0.0002 g
Constant Weight 45. 9591 0.0002 g

Table 2. Constant Weighing of Crucible and Fertilizer Sample

Weight 1 49. 5597 0.0002 g
Wight 2 49. 5594 0.0002 g
Constant Weight of Crucible + Sample 49. 9591 0.0002 g
Constant Weight of Empty Crucible 49. 9591 0.0002 g
Net Weight of dried sample 3.6003 0.0003 g

Table 3. Determination of the Phosphorus content in fertilizer

Wet weight of sample 3.6274 0.0003 g
Dry weight of sample 3.6003 0.0003 g
% P(wet basis) 22.556 0.0003 %
% P (dry basis) 22.557 0.0003 %
%P2O5 (wet basis) 14.558 0.0003 %
% P2O5 (dry basis) 14.425 0.0003 %

Calculation of the Moisture Content of Fertilizer:

Equation:

( ) ( )

Calculation of the Phosphorus Content in Fertilizer:

Net Ionic Equation:
() ( ) ( ) ( ) ( )

General Equation for % P:

General Equation for %

Percent Error: