Gravimetric Determination of Moisture and Phosphorus

in Fertilizer Samples
Sheenly Anne P. Saavedra1 and Jasper C. Villasis2

National Institute of Physics, College of Science and 2Department of Food Science and Nutrition, College of
Home Economics
University of the Philippines, Diliman, Quezon City
1

ABSTRACT The major component of fertilizer is given by its nutrients: nitrogen, phosphorus
and potassium (NPK) . The weight declared for phosphorus in commercial fertilizers is usually
30% in the form of P2O5 which is the largest percent by weight . Meanwhile, moisture content of
a fertilizer determines its purity . In this experiment, phosphorus content is determined as well
as moisture content of fertilizer using gravimetric method . Gravimetry generally involves a
known solution reaction between analytes and reagents to give sparingly soluble products that
can be weighed; specifically, the precipitation method was used . The moisture content was
obtained from the difference of the weight of the wet and the dry sample, and was found to be
1.2(0.9)% . The phosphorus content was determined through precipitation gravimetry where
the sample was reacted with MgSO4 7H 2O and NH3 to form a white precipitate, MgNH 3PO 4H 2O.
The net weight of the dried precipitate obtained was 1.1407(0 .0003)g. Using stoichiometric
relations and gravimetric factor, %P2 O5 and %P for the dried sample showed to be 8.3(0 .4)%
and 3.6 0.4% respectively . Comparing to theoretical P2O5, which represented 30% P in
fertilizer labels, it resulted to 21 .7% difference and 72 .33% error to the theoretical claim .
INTRODUCTION

Other than carbon, oxygen, and hydrogen,

there are 13 essential elements, called
nutrients, present in soil which is needed in
plants in order for them to grow. The kind
and amounts of nutrients that plants need
have been determined, and among these are
nitrogen, phosphorus and potassium (NPK)
which are present in fertilizers. Fertilizers are
artificial nutrients that keep the soil
productive by replacing those that have been
extracted by plants. They are essential
components in soil to keep cultivated plants
healthy 1 .

Most commercial plant fertilizers supply

these three essential elements as indicated by
the N-P-K numbers in their labels . For
example, an N-P-K rating of 15-30-15 denotes
presence of 15% by weight of nitrogen (N),
30% by weight of diphosphorus pentoxide
(P2O5), and 15% by weight of potassium oxide
(K2O) in the fertilizer .

Another
important
component
in
fertilizers is its moisture content . The
moisture content influences the physical
properties of a substance such as weight,
density, viscosity, refractive index, electrical
conductivity and many more . This component
shows if the fertilizer contains standard
properties such as concentration or purity,
nutritional value, and dry substance content .
Drying techniques are used to determine this
content .
Gravimetric analysis is a technique
through which the amount of the substance
being analyzed can be determined through
the measurement of mass 2 . It is composed of
two types of methods: precipitation and
volatilization .
In
this
experiment,
precipitation gravimetric methods and its
concepts were used to determine the
moisture content and phosphorus content of
fertilizer samples .
For moisture content determination, mass
of sample (as received) and the constant

Saavedra, S.A.P. and Villasis, J.C., 2016 | 1

weight of the sample are compared . The

constant weight of sample is obtained
through drying or ignition . In this experiment,
drying of sample is done at 110C.

A proximate analysis of phosphorus of the

fertilizer sample is done in the experiment
using the precipitation method . This method
is characterized by a substance that is
precipitated out of the solution, and
converted into a weighable form . Principles of
constant weighing are used to determine
weight of crucible and fertilizer sample .
The reaction involved the phosphate
precipitating using precipitating agent
magnesium hexahydrate and a chemical
reaction with NH3. This reaction is given by
the balanced chemical equation:
5H 2O + HPO 42- + NH 4 + + Mg2+ + OH MgNH 4PO 46H2 O(S)

[2]

An important concept for precipitation is

the supersaturation which affects crystal
nucleation and particle growth . This is
represented by the Von-Weimarn ratio, which
shows that initial rate of precipitation is
proportional to the relative supersaturation.
where

[2]

Q = concentration of any
species at any instant
S = equilibrium solubility
A low VWR results in large crystals. This
qualitatively
indicates
that
solute
concentration must be low and solubility
must be high 3.

In
this
experiment,
quantitative
determination of percent moisture is done
through constant weighing and quantitative
determination of phosphorus in fertilizer is
done using gravimetric method of analysis.
MATERIALS AND METHODS

A crucible with cover was dried by leaving it

overnight in an oven set at 110C. From the
oven, it was transferred to a desiccator for
moisture absorption using crucible tongs,
cooled for 15 minutes, and then weighed using

an analytical balance. Heating and cooling

process was repeated until constant weight of
32.3842 grams was obtained.

A glass container containing the sample,

manipulated by paper tongs, is tared then
slowly subtracted its mass by tapping sample
into the crucible. A fertilizer sample of 3.0024
grams was weighed into the crucible with cover
through weighing by difference. It was placed in
an oven with the cover slightly ajar and heated
at 110C for an hour. After, it was transferred to
a desiccator for moisture absorption using
crucible tongs, cooled for 15 minutes, and then
weighed using an analytical balance. Heating
and cooling process was repeated until
constant weight of 35.3514 grams was obtained.
The fertilized sample was dissolved in the
crucible using distilled water before it was
quantitatively transferred to a 250-mL beaker.
Since sample did not dissolve completely, it was
filtered using a filter paper until a clear filtrate
was obtained. About 45 mL 10% (w/v)
MgSO47H2O was added to the filtrate. Then,
150 mL of 2 M NH3 was added slowly, and with
vigorous stirring, a white precipitate was
formed. The solution was left for 15 minutes in
order to undergo digestion. The precipitate was
quantitatively filtered using a pre-weighed
filter paper of mass 0.8698 g. Beaker was
washed with two 5-mL portions distilled water
which was then poured over solid in the filter
paper to wash precipitate. Beaker and
precipitate were washed again using two 10mL portions 95% ethanol. The filter paper with
precipitate was placed in a beaker, making sure
it stood upright. It was then heated overnight in
the oven set at 110C. From the oven, it was
transferred to a desiccator for moisture
absorption using crucible tongs, cooled for 15
minutes, and then weighed using an analytical
balance.
RESULTS AND DISCUSSION

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

Saavedra, S.A.P. and Villasis, J.C., 2016 | 2

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 4.

Crucible obtained a constant weight of

32.3842(0.0002)g. It was determined to be of
constant weight once a maximum difference of
0.0003 g was observed between two successive
weighing of the crucible. This is because the
analytical balance has an error of 0.0002. Once
crucible mass is obtained, it can now be used to
determine weight of sample and weight of
moisture by difference in the next steps.
After, a fertilizer sample of recorded weight
3.0024(0.0002)g was transferred into the
crucible. This would be referred as the wet
sample and was obtained using weighing by
difference. Weighing by difference helps in
preventing sample contact of laboratory
apparatus thus prevents mass loss of sample.
Also, a paper tong was used to hold the glass
container of the sample to minimize contact
and moisture addition. Touching the glass, as
with the crucible, might transfer additional
moisture to the container, lessening the
precision of recorded mass 5.

The second part of the experiment involved

the weighing of the crucibles with fertilizer
until they reached a constant weight of
35.3514(0.0002)g. This would be referred to
as the dry sample. Sample was then dissolved in
distilled water and was filtrated. After the first
filtration, the precipitate was discarded
because it is believed to contain other nutrients
and unnecessary colorants, and the phosphorus
content of the precipitate is believed to have
dissolved in the filtrate.
The clear filtrate was then reacted with 10%
magnesium sulfate heptahydrate, MgSO47H2O,
and 2M ammonia, NH3, to form a white
precipitate which is magnesium ammonium
phosphate hexahydrate, MgNH4PO46H2O.

Ammonia, NH3 , was added slowly to control

the acidity of the solution. If the solution is too
basic, magnesium hydroxide, Mg(OH)2 is
formed due to the dissociation of HPO42- to

PO43 thus having excess hydroxide ions which

will precipitate with Mg2+. However, if the
solution is not basic enough, H2PO4 will be
formed, and no precipitate will occur 6 . Slow
addition of NH3 will prevent the coprecipitation of Mg(OH)2.

The pre-weighed filter paper was kept in the

desiccator to avoid unnecessary moisture
absorption, which may affect the net weight of
the precipitate. The precipitate was left to stand
for 15 minutes to undergo digestion, which is to
stand in contact with the mother liquid. This
aids in lowering the Von Weimarn Ratio,
producing larger precipitates. After, it was then
filtered using the pre-weighed filter paper.
95% ethanol was used after washing the
precipitate with water to remove the water and
facilitate faster drying. Since the precipitate is
soluble in water, the ethanol, a volatile solute,
was also added to reduce peptization.
Table 1 below shows reported values of the
experiment. See Appendix for data sheet
containing raw data (Sample weights, weight
filter paper, weight of precipitate), and sample
calculations.
TABLE 1. Reported Values
Crucible + Fertilizer
Sample
Mass of Water, g
0.0352 0.0003
% Moisture
1.2 0.9
%P (wet basis)
3.6 0.4
%P (dry basis)
3.6 0.4
%P2O5 (wet basis)
8.2 0.4
% P2O5 (dry basis)
8.3 0.4

The possible sources of errors are discussed

in Table 2.
TABLE 2. Possible Sources of Errors and its
Effect on Calculated Parameters
Source of
Parameter and Error
Error
Errors
in Errors in constant weighing
weighing
of crucibles and weighing of
wet sample, precipitate will
lead to less precise results.
Moisture
Weighed mass will not be
absorption of accurate.

Saavedra, S.A.P. and Villasis, J.C., 2016 | 3

apparatus and
of sample
Loss
of
phosphorus
content during
1st filtration

Phosphorus content was

assumed to be fully dissolved
in filtrate. Non totality in
content will result in lower %
P2O5 value
Fast addition of Coprecipitation of Mg(OH)2
NH3
and/or formation of H2PO4
which
results
in
no
precipitate formed. Desired
precipitate formation will not
be precise.
Peptization
Precipitate formed might
lean to being colloids causing
less precipitate to be filtered.
CONCLUSIONS AND RECOMMENDATIONS

The calculated moisture content of the

fertilizer sample was 1.2(0.9) % which is a low
percentage. This indicated that fertilizer sample
has high purity and most of the weight came
from actual nutrients such as NPK. It is also
shown with the difference in wet and dry %P
and %P2O5. Noting that their values are very
close, it verifies that there is little moisture in
the fertilizer sample, thus was of high purity.

However, the calculated %P2O5 was 8.3(0.4)

% for the dry basis, which is very low compared
to the theoretical value of 30% P2O5(from usual
commercial fertilizers). This had a 72.33%
error. This means that the phosphorus obtained
through gravimetry was less than the
theoretical amount and 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 8.

REFERENCES
[1]
[2]
[3]

Shakhashiri.
Agricultural
Fertilizers.
http://scifun.chem.wisc.edu/chemweek/pdf/A
gricultural_Fertilizers.pdf (accessed June 28,
2016).

Skoog D.A., West D.M., Holler J.F. In

Introduction to Analytical Chemistry, 8th ed.;
Cengage Learning: Pasig, 2012; p 195.
Gravimetric
Analysis.
http://web.calstatela.edu/dept/chem/07winte
r/201-lec/201-l-4-gravimetric-analysis.pdf
(accessed June 28, 2016).

[4] Lewis, X. E. D. Gravimetric Determination of

Moisture Content and Phosphorus Content in
Fertilizers.
http://www.academia.edu/12327176/Gravim
etric_Determination_of_Moisture_Content_and_
Phosphorus_Content_in_Fertilizers (accessed
June 28, 2016).
[5]

Weighing
by
Difference.
www.ic.sunysb.edu/Class/che133/techniques/
weighbydiff/wei ghbydiff.pps (accessed June
28, 2016).

[6] Nord, R. S. ANALYSIS OF PHOSPHORUS IN

PLANT.
https://www.emich.edu/chemistry/gencheml
ab/documents/10-phosphorus.pdf (accessed
June 28, 2016)).
[7]
[8]

Harris, D. C. Sample Preparation. In

Quantitative Chemical Analysis, 7th ed.; W. H.
Freeman and Company: New York, 2007; pp 8,
645.
Determination
of
Moisture.
http://www.fertilizer.org/imis20/images/Libr
ary_Downloads/2014_ifa_moisture_determinat
ion.pdf?WebsiteKey=411e9724-4bda-422fabfc8152ed74f306&=404%3bhttp%3a%2f%2fww
w.fertilizer.org%3a80%2fen%2fimages%2fLib
rary_Downloads%2f2014_ifa_moisture_determ
ination.p (accessed June 28, 2016).

Saavedra, S.A.P. and Villasis, J.C., 2016 | 4

APPENDIX
Data Tables
TABLE 1. Constant weighing of crucibles with covers
Crucible w/ covers
Weighing 1
32.3844 0.0002
Weighing 2
32.3842 0.0002
Constant weight
32.3842 0.0002
TABLE 2. Constant weighing of crucibles with covers + fertilizer sample
Crucible + Fertilizer Sample
Weighing 1
35.3515 0.0002
Weighing 2
35.3514 0.0002
Constant weight
35.3514 0.0002
Net weight of dried sample
2.9672 0.0003
TABLE 3. Weight of sample, filter paper and precipitate
Crucible + Fertilizer Sample
Sample weight (as received), g
3.0024 0.0002
Sample weight (dried), g
2.9672 0.0003
Weight of filter paper, g
0.8698 0.0002
Weight of dried filter paper with
1.7195 0.0002
precipitate, g
0.8497 0.0003
Net weight of dried precipitate, g
Working Equations

Important Formulas

Guide Questions
1. What are the other methods used for moisture determination besides oven drying?
Other methods of direct measurement are: iIgnition at 1000C or burning of crucible
with Bunsen burner.
Saavedra, S.A.P. and Villasis, J.C., 2016 | 5

An indirect method of moisture determination is using moisture meters and

hygrometers.
2. What is the significance of grinding the sample before drying?
The samples were ground before oven drying to remove the preliminary forms of
non-essential water that can be removed without oven drying, and to increase the
surface are for easier removal of adsorbed water. The non-essential, adsorbed water
was removed from the surface of the crucible by oven drying at 110. Fertilizer

sample used was already grinded.

3. Discuss the principles of operation of mechanical and electronic balance.
Electronic Analytical Balance - An object is placed on the pan of the balance and the
windows of the balance are closed. This causes the pan and indicator to move
downward, which increases the amount of light striking the null cells photodetector.
A small electric current keeps the balance pan in the null position, and this current
is directly proportional to the mass of the object.
Mechanical Balance - An object is placed on the end of the balance, and standard
masses are placed on the other end. The object remains at one end, and the standard
masses are moved until the beam of the balance is restored to the original position.
The weight reading is taken by adding the intervals at which the standard masses
are situated on the beam.

FIGURE 1. Electronic Analytical Balance

FIGURE 2. Mechanical Balance

4. Is it possible to use NH4Cl instead of NH3 to precipitate phosphorus in fertilizer sample?

Explain your answer.
In the absence of NH3, the acidified form of NH3, NH4Cl, could not have been a
feasible substitute for NH3. This form would have dissociated into the ions NH3, H+ ,
and Cl- , and not have formed a filterable precipitate, which was desired. The acidity
of the solution would have been affected, and the solubility increased.
Saavedra, S.A.P. and Villasis, J.C., 2016 | 6

Calculations

Saavedra, S.A.P. and Villasis, J.C., 2016 | 7