GRAVIMETRIC

DETERMINATION OF MOISTURE
PHOSPHORUS CONTENT IN FERTILIZER SAMPLES

AND

C.F. BATIFORRA, A.M.F.C. TRINIDAD AND J.P.Q. ILAGAN

DEPARTMENT OF CHEMICAL ENGINEERING, COLLEGE OF ENGINEERING
UNIVERSITY OF THE PHILIPPINES, DILIMAN QUEZON CITY, PHILIPPINES
DATE PERFORMED: 04, 06, FEBRUARY
INSTRUCTORS NAME: MARIEL CLORES

2015

ABSTRACT
The amount of substances that make up fertilizers have a big effect on its
economic value and overall quality. To maintain the quality of market-value
fertilizers, their components are consistently measured through the use of different
methods. The main goal of this experiment is to determine the moisture and
phosphorus content of a fertilizer sample using gravimetric analysis. The computed
moisture content was at 0.7729% 0.0001%. The phosphorus content was at
approx. 4.6% and the phosphate content was at 10.5%. The values obtained were
within the range of accepted values in the market so we can say that the method
used was effective in determining the amounts of different species in a substance.

INTRODUCTION
Gravimetry includes all methods
wherein the use of mass or a change
in mass is used to analyze species.
There
are
two
types
of
gravimetric analysis. One is the direct
method where the analyte is directly
weighed. The other is indirect analysis
where the analyte is removed and the
change in mass of the whole thing is
used to analyze the analyte. For the
first part of this experiment, we are
going to use an indirect method of
gravimetric analysis.
In some cases, the analyte is in
its aqueous form. In order to weigh it,
we need to convert it into solid form
by using a precipitating agent to
precpitate it out of the solution. The
three
fundamental
steps
in

precipitation are precipitation, drying

and then weighing.
In precipitation, we need to
know the concept of nucleation and
particle growth. Nucleation is the
formation of nuclei from the reaction.
Particle growth is when these nuclei
start to grow in size. In an ideal
precipitation, we want large crystals
with high purity in order for us to
easily filter them out. Precpitation will
be demonstrated in the second part of
the experiment.
METHODOLOGY
The experiment was done in
two parts. The first part is the
determination of moisture content of
the sample and the second part is the
determination of the phosphorus
content.

A. Constant Weighing of the Crucibles

For the first part of the
experiment, one crucible with cover
was prepared by air-drying it in an
oven set at 110 C and kept there for
one hour. After this, the crucible and
cover were only handled using a pair
of crucible tongs. The crucible and
cover was then put in a dessicator and
allowed to cool in the balance room for
15 minutes. The crucible and cover is
then weighed on an analytical balance
and the weight is recorded.
The
crucible and cover is again air-dried
but now for only 30 minutes. They are
again cooled and weighed using the
same method. After recording a
difference of 0.0001g between the 1st
and 2nd weighings, the last recorded
weighing is recorded as the constant
weight.
B. Moisture Analysis
A sample of the fertilizer is then
transferred slowly into the crucible
until the net weight of the sample has
reached 3 g. The crucible along with
the sample is air-dried in the oven set
to 110 C for one hour. The cover is
slightly opened to allow the escape of
vapor. The same method used in
getting the constant weight of the
empty crucible was also carried out in
getting the constant weight of the
crucible with the sample.
C. Precipitation of MgNH4PO4 6H2O
For the second part of the
experiment, 500mL of 10% (w/v)
MgSO4 7H2O solution and three
500mL of 2M NH3 solution is prepared
for the whole class. A fluted filter
paper is weighed and stored in a
dessicator. The dried sample from the
first part of the experiment is
transferred to a 250-mL beaker. 40mL
of distilled water is added to dissolve

the sample. Any remaining sample in

the crucible is washed out using the
distilled water. The mixture is then
passed through filter paper to remove
the undissolved solids. The filter paper
used here is different from the preweighed filter paper. 45mL of MgSO4
7H2O solution is then added to the
filtrate. Using a dropper, 150mL of 2M
NH3 is added to the filtrate while
continuously stirring. The mixture is
then stored until the next meeting.
The mixture is then passed through
the pre-weighed filter paper. The
beaker is then washed with 2 5mL
portions of distilled water and poured
onto the precipitate to transfer any
remaining precipitate left in the
beaker. The precipitate is then washed
with 2 10mL portions of 95% ethanol.
The filter paper, containing the
precipitate is then placed in the oven
set at 110 for one hour. Afterwards
the filter paper was cooled for 15
minutes inside a dessicator and
weighed. All data was recorded in data
sheet.
RESULTS AND DISCUSSION
A. Moisture Analysis
The constant weight of the
crucible and the cover is measured so
that the weight of the water that will
evaporate from the crucible-sample
setup will all be coming from the
sample only. The difference between
two weighings must be within a
0.0003g range to be considered
constant weight. This value is taken
from the error propagation of an
analytical balance. Multiple weighings
are carried out to ensure all of the
moisture has evaporated. The purpose
of cooling the crucible is to avoid
errors in the measurement due to air
currents caused by the warm air. The
use of crucible tongs is also important

to avoid applying moisture to the

crucible as well as the cover.

This is one possible source of personal

error.

Table 1.1: Constant Weight of

Crucible and cover without sample

The net weight of the dried

sample was computed simply by
subtracting the constant weight of the
empty crucible from the constant
weight of the crucible with sample.
The % moisture is computed by using
the following equations:

Weighing No.
1st weighing
2nd weighing
Constant Weight

Weight (g)
34.8814 0.0002
34.8813 0.0002
34.8813 0.0002

In
obtaining
the
constant
weight, we expected that the weight
of the crucible will slowly decrease
due to the evaporation of moisture.

Mass of water = sample wtwet - sample

wtdry

Mo isture=

mass of water
weight of sample( wet )

100
Table 1.3: Reported Values
Table 1.2: Constant Weight of
Crucibles with dried sample &
Sample Size

Mass Water (g)

% Moisture

Weighing No.
1st weighing
2nd weighing
3rd weighing
4th weighing
5th weighing
Const.
Wt
(w/
sample)
Const. Wt (empty)
Sample Net Wt.
(dry)
Sample Wt. (wet)

We have calculated a really low

percentage of moisture content which
is ideal because excess moisture in
fertilizer will result in clumping.

Weight (g)
38.0090 0.0002
38.0045 0.0002
38.0019 0.0002
38.0010 0.0002
38.0035 0.0002
38.0010 0.0002
34.8813 0.0002
3.1197 0.0003
3.1440 0.0002

From the data above, we can

see that the weight of the crucible has
increased. We assumed that the
crucible has started to absorb
moisture so we recorded the value
from the 4th weighing as the constant
weight. There is a possibilty that the
crucible could have lost more water
before it started absorbing again. We
are not sure if 38.0010 g is the lowest
possible value for the dried sample.

0.0243 0.0004
0.7729%

0.0001%

One disadvantage of using this

indirect method of gravimetry is that
other compounds other than water
may evaporate from the sample if
excess temperatures are used. If other
compounds other than water are
released, the weight of the dried
sample will decrease, calculated mass
of water will increase and we will have
an overall increased moisture content.
This is one possible source of
methodical error for this experiment.
B. Phosphorus Analysis
In the second part of the
experiment, we must determine the
phophorus content of the sample.
Since we are using gravimetry, we
must precipitate out an analyte so that

we can weigh it and use it to

determine the amount of the species
we are looking for. Since we are going
to filter out the precipitate, we want to
have
large
crystals
and
less
aggregates.
There
are
several
methods of achieving this. We must
take note of the Von Weirmann ratio

R=

QS
S

where:
Q = concentration of reactants
before
precipitation
S = solubility of precipitate in
medium
from which it is being
precipitated.
We want this ratio to be as low
as possible so we want to decrease Q
and increase S. In our experiment, the
slow addition of the precipitating
agent contributed to the rate of
particle growth against nucleation. We
also carried out Ostwald ripening, or
digestion,
which
is
letting
the
precipitate stay in it's mother liquid to
enchance the concentration of the
precipitates and contribute to particle
growth.
In the addition of H2O, MgSO4
7H2O and NH3. Three reactions take
place. First the H2O will react with
P2O5.
P2O5(aq) + 3H2O(l) 2H3PO4(aq)
NH3 will simultaneously react
with water to form OH- (and NH4+),
which will react with the formed
H3PO4(aq).
H3PO4(aq) + 2OH-(aq) HPO42- + 2H2O(l)
HPO42-(aq) + NH4+(aq) + Mg2+(aq) + OH-(aq)
+ 5H2O(l) NH4MgPO4 6H2O(s)
The NH4MgPO4 6H2O is the
precipitate that formed and this is the

analyte that we used to compute for

%P and %P2O5. After filtration, the
precipitate is rinsed with ethanol to
remove all residual traces of inert ions
included in the supernatant, without
dissolving any of the precipitate. The
ethanol is dissolved when the
precipitate is placed in the oven.
Table 2.1: Weight of Filter paper
and Weight of ppt
Filter paper wt. (g)

1.1945
0.0002
Filter paper w/ ppt wt. 2.3416
(g)
0.0002
Precipitate net wt. (g) 1.1471
0.0003

We can now compute for %P

and %P2O5 by using the following
equations:
%Pdry =

wt . ppt x

FW P
x 100
FW NH 4 MgPO 4 6 H 2 O
wt . dried sample
%Pwet =

wt . ppt x

FW P
x 100
FW NH 4 MgPO 4 6 H 2 O
wt . sample as received
%P2O5dry =

wt . ppt x

FW P 2 O5
x 100
FW NH 4 MgPO 4 6 H 2 O x 2
wt . dried sample
%P2O5wet =

wt . ppt x

FW P 2 O5
x 100
FW NH 4 MgPO 4 6 H 2 O x 2
wt . sample as received

Table 2.2: Reported Values

%P (wet)
%P (dry)
%P2O5 (wet)
%P2O5 (dry)

4.6050%
4.6409%
10.552%
10.6334%

We can also see that the values

of the dry based phosphorus content
are higher which is valid because the
weight of the dried sample was much
lower.
There
are
many
possible
sources of error in the second part of
the experiment. If the rate of addition
of NH3 was much faster, the rate of
nucleation will also increase. There will
be more particles, but smaller. Some
of these particles might pass through
the filter and result in decreased
phosphorus
content.
If
the
temperature when the experiment was
done was too low, the rate of particle
growth will increase and will also
result in less phosphorus content.
CONCLUSION
RECOMMENDATION

AND

The method was carried out

properly and all sources of errors were
minimized as much as possible. No
gross errors were committed.
The %Moisture that we have
calculated is 0.7729% which was
within the range of accepted values in
the market. The range of the accepted
values for the phosphorus and

phosphate content is very large since

the amount of phosphorus and
phosphate in the fertilizer will highly
depend on the other chemicals found
in the fertilizer and on the type of
plant/s that the fertilizer will be put to.
REFERENCES
[1]
Higson,
S.
(2004). Analytical
chemistry. Oxford: Oxford University
Press.
[2] Morse, D., & Baer, D. (2004).
Laboratory Balances: How They Work,
Checking Their Accuracy. Laboratory
Medicine, 48-51
[3]
Skoog,
D.,
&
West,
D.
(1996).Fundamentals
of
analytical
chemistry (7th
ed.).
Fort
Worth:
Saunders College Pub.
[4] Caro, J., & Hill, W. (1956). Fertilizer
Characteristics, Characteristics and
Fertilizer Value of Phosphate Rock from
Different Fields. Journal of Agricultural
and Food Chemistry, 684-687.

APPENDIX
Answers to Question
Experiment 2

1. The constant weighing process ensures that the sample doesn't have any more
moisture to evaporate.
2. Moisture has a very high effect on the quality of the fertilizer. Too much moisture
in fertilizer will result in clumping and caking.
3A. Other methods include Infrared lamp drying in which the analyte is placed under
an infrared lamp. One advantage of infrared lamp drying is the fast determination
of moisture content using only inexpensive equipment. But it is not officially
recognized as the method is not standardized.
3B. Another method is the Karl-Fischer method. It can be used to determine the
moisture content of fertilizers with very low percent moisture. It is done by reacting
water with sulfure dioxide and iodine to produce sulfuric acid and hydrogen iodide.
Hydrogen iodide is colorless and iodine has a reddish brown color so a color change
will take place. Sulfure dioxide and iodine are gaseuous and will normally be
released. Disadvantages of this method is the use of hazardous chemicals, more
elaborate lab equipment. It also more complex overall.
4. Weighing by difference will have less error of propagation because of the minimal
transfer of the sample. Constant transferring of the sample will leave significant
traces on the surfaces of the containers used.
5. The hot crucibles will create an air current within the analytical balance and
these air current can be detected. They will give the crucible buoyancy, giving a
decreased value.
6. Trapped water molecules between particles will be released. The rate of
evopation will also be faster since surface area has increased.
7. Error propagation of an analytical balance in two weighings is 0.0003. This is
based from the uncertainty of 0.0002.

0.00022+ 0.00022=0.0003

8. Evaporation of volatile substances other than water. (Increased temperature,

Increased measured water mass, %moisture). Not cooling the crucible (decreased
weight). Touching the crucible (increased weight).
9A. A mechanical balance requires the use of weights to counter the force exerted
on one size. The main principle here is to equalize the torques on both sides. The
places of the weights will determine the force of the sample.
9B. An electronic balance uses magnetic force restoration. An object exerts a linear
force while a coil suspended in a magnetic field pushes agsainst it. The position of
the coil, detected by an optical sensor determines the weight of the object.
10.

Appendix
Experiment 3

1. First, the phosphorus needs to be converted into solid form, precipitated out and
filtered. We want large crystals so we need to slowly add the precipitating agent.
Then we let it stay with it's mother liquit to increase it's purity. Then we filter it and
then washed with ethanol to remove traces of ions from the supernatant. Wecan
now weigh the analyte and use it to calculate the amount of phosphorus present in
the sample.
2. Digestion increases the purity of the particles.
3. The temperature when the experiment was done. The rate of addition of NH3
(faster rate, smaller particles, less ppt, smaller phosphorus content). The
concentrations of the reactants (higher concentrations, lower rate of particle
growth, smaller phosphorus content). The solubility of the precipitate (higher
solubility, less ppt, small phoshprous content.
4. The slow addition of NH3 contributes to the rate of particle growth against the
rate of nucleation. The formation of large crystals are critical because otherwise the
particles will be small enough to pass through the filter paper.
5. The ethanol removes traces of ions from the supernatant without dissolving the
precipitate.
6. It will interfere with precipitation of phosphorus as Mg will react with Cl ions to
produce MgCl2.
7.