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GRAVIMETRIC DETERMINATION OF MOISTURE IN FERTILIZER

SAMPLES & GRAVIMETRIC DETERMINATION OF PHOSPHORUS IN
FERTILIZER SAMPLES



ABSTRACT

Gravimetry is method used to determine composition of a sample quantitatively using constant
weighing processes. In this experiment gravimetric techniques were used to determine the moisture
and phosphorus content of a fertilizer sample through oven drying and precipitation method. The
fertilizer sample was dried and weighed then precipitated and made into a solution ready for
filtration. It was filtrated to isolate the precipitate. The calculated moisture content was 4.74%
0.01%. The %P and %

in both wet and dry samples were calculated in this experiment. It was
calculated that %P and %

in wet sample are 7.38% and 16.927% respectively while 12.62% and
28.919% respectively for dry sample calculation.


INTRODUCTION

Gravimetric analysis is a method of
quantitative chemical analysis which converts
an analyte into a substance that can be
separated from the sample and then weighed.
Gravimetry involves the process of preparing
solutions with the sample of known mass,
separation of desired constituent, weighing
the remaining sample, and computation of
amount of specific composition from the final
weighed constituent.
Gravimetry has different methods. One
method used is the precipitation method
where the analyte becomes a non-soluble
precipitate which will not react to several
reagents added. This precipitate will be
further isolated by means of physical
processes such as removal of impurities and
filtration. Another method is the volatilization
method were the volatile constituents of a
sample are removed by drying which leaves
the desired composition.
Gravimetry is an effective method and is
widely used in the determination of
composition especially quantities of mass
comprising a sample.
To maintain accuracy of measurements and
to lessen possible sources of errors, different
measures and conditions are observed during
gravimetric process. A constant weight must
be observed first before actually weighing the
sample in the container. The drying
temperature is usually 105-110 degrees
Celsius. This is customary to avoid errors due
to the drying temperature.
Gravimetry can be applied in ensuring good
quality fertilizers by knowing the amount of
needed components comprising a sample.
Fertilizers contain soluble constituents like
nitrogen, phosphorus and potassium.
In this experiment the moisture and
phosphorus content of fertilizer samples will
be determined by oven drying to a constant
weight at a constant temperature.

METHODOLOGY

EXP. 2
Preparation of Crucibles

One crucible and one cover were thoroughly
washed and cleaned. The crucible and cover
were labelled and placed in the oven at 110
degrees Celsius for one whole period.

Constant Weighing of Crucibles

Using a pair of crucible tongs, the crucible and
cover were transferred into the desiccator.
2

The desiccator was then allowed to cool for
15 minutes. The weight of the crucible and
cover was then obtained using the analytical
balance. The crucible and cover were
transferred back to the oven at 110 degrees
Celsius for 30 minutes. The cover was slightly
ajar with the crucible. This process was
repeated until a constant weight of the
crucible and cover was obtained. In this case,
the process was repeated four (4) times.

Moisture Analysis

A 3.0 grams of fertilizer sample was weighed
into the crucible with cover. The crucible with
cover containing the sample was transferred
back to the oven at 110 degrees Celsius for
one (1) hour while the cover is slightly ajar.
The crucible was transferred to a desiccator
after one hour in the oven. It was cooled for
15 minutes. The crucible and cover
containing the sample was weighed using the
analytical balance. It was then transferred
back to the oven at 110 degrees Celsius this
time for 30 minutes. These processes were
repeated until a constant weight was
obtained.

EXP. 3
Preparation of Solutions

Solutions of 500 mL 10% (w/v)

and three (3) 500 mL of

2M

solutions were prepared.*

Precipitation of

A 1/3 filter paper was prepared and weighed.
The filter paper was placed in the desiccator
before it was used in the latter part of the
procedure. Dried sample of fertilizer was
transferred to a 250 mL beaker. Distilled
water of volume 40 mL was added to the
sample for it to dissolve. The solution was
then filtered using a filter paper. 45 mL of

was then added to the

filtrate. Slowly, 150 mL 2M

was added
while being stirred. The solution was allowed
to stand for 15 minutes to continue the
precipitation process. The precipitate
collected was transferred to the filter paper
with known weight. It was then washed twice
with 5 mL portions of water. After washing
with water, the precipitate was washed twice
with 10 mL 95% ethanol. The precipitate was
set aside until the next period. The precipitate
was transferred to the oven at 110 degrees
Celsius for 1 hour. It was cooled then for 15
minutes inside the desiccator and then weight
using the analytical balance.

RESULTS AND DISCUSSION

The constant weight measurements gathered
in the experiment are shown in the Table 1.

Table 1. Weight measurement summary
table.

Quantity Measurement (g) Uncertainty
(g)
Constant
weight
Crucible
37.3767 0.0002
Constant
weight
Crucible +
Sample
40.2796 0.0002
Net weight of
sample
3.0474 0.0003
Weight of
Filter Paper
0.9852 0.0002
Weight of
air-dried
filter paper
with ppt
2.7689 0.0002
Weight of
dried ppt
1.7837 0.0003

In each measurement, it can be observed that
after placing the sample in the oven for some
time, the measured weight went down.

Theoretically, the mass loss is accounted to be
the moisture content of the sample which
evaporated through the process of drying. In
this set-up, the measurement cannot be fully
accounted as the moisture content due to
some possible errors in the process. Related
to this, the experiment uses constant
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weighing process and conditions to lessen
possible errors and to account moisture
content more accurately.

From the data in Table 1, it was calculated
that the %Moisture of the sample fertilizer is:

4.74% 0.01%

It is important to determine the moisture
content of fertilizer sample, because moisture
content reflects the mineral content of
fertilizer samples. Mineral content is
important for slow release fertilizers or the
fertilizers which can be activated by
temperature, moisture, or pH. Their reaction
to different conditions depends mostly on the
amount of moisture the fertilizer has.

Aside from oven drying methodwhich was
used in this experimentthere are other
methods which can be used to determine the
moisture content of a fertilizer sample. One
method is the Karl Fischer Method which
uses the Karl Fischer reagent which is a
selective reagent that only reacts selectively
with water to measure moisture content. Karl
Fischer reagent consists of iodine, sulfur
dioxide, a base and solvent such as alcohol.

In the weighing process, the sample was
weighed using the method of weighing by
difference. Weighing by difference has an
advantage compared to normal weighing
such that it minimizes possible sources of
errors. Weighing by difference avoids the
transfer of material to an intermediate object
which avoids incomplete transfer or possible
loss of material.

Every time the crucibles weight was
measured, it was cooled to room temperature
first. The reason for such practice is that to
make a comparative analysis of the mass
which will be measured, the crucibles mass
needs to be measured at a point same as the
condition of the previous measurement or
there should be a basic standard pointin
this case room temperature. Room
temperature is needed to have a comparative
standard point for weighing.

The sample was grinded before oven drying.
This was done to remove the water which
might be occluded in the sample. This
practice also increases the surface area of the
sample which makes it dry faster.

Aside from the mentioned sources of errors,
there are still some possible sources of errors
in this laboratory. Some of these possible
sources: accidentally touching the crucible,
difference in temperature during
measurement, crucible label, vibrations
during weighing and other related cases may
cause even the slightest error in
measurement.

EXP. 3

The fertilizer sample used in experiment 2
contains soluble compounds like nitrogen,
potassium and phosphorus. In the
experiment, the soluble form of phosphorus
in plant food was precipitated as

. The reaction is given by eq

1.

(1)

(B) is the ppt formed in the

process. To compute for the %P and %

in
this ppt gravimetric analysis is needed.

Solution for % P:
GF =






GF =

* 1.7837 g B = 0.2251 g P

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Solution for

:

GF =

GF =

* 1.7837 g B = 0.51583 g

Using gravimetric techniques, the % P and
%

were calculated. The percent

composition were computed in reference to
the dry and wet weights of the fertilizer
sample. In both calculation the percent
composition of both P and

were larger
in the dry sample. This shows that for a given
sample which only contains the specific
constituents needed, the mass corresponds to
the mass of the needed constituents
themselves only and there are less unwanted
constituents like moisture, because they were
already removed.

Gravimetric analysis proceeds with certain
steps to be followed. After the dissolution of
the sample, a solution containing the sample
needs to be prepared. In this step, quantities
such as pH and concentration can be adjusted
for easier computation. The sample will then
be precipitated using a precipitating agent. In
the experiment, the sample was precipitated
using slow addition of

. Precipitation is
done to form a nuclei that in turn will form
the aggregate. Digestion or the Ostwald
ripening happens next. This process is where
the sample is being dried to dissolve small
particles and re-precipitate/ let them be
adsorbed in the larger precipitate. In the
experiment, the digestion process was the
oven drying of the sample. It was observed
that the sample had bigger/ coarse-looking
composition which settled down the
container as an effect of the Ostwald ripening.
The precipitate will be washed and filtered
after that. This is done to isolate the solid
composition of the solution with the liquid
portion. The solid sample was dried for long
period of time at room temperature. After
drying the sample, the sample was washed
with water and ethyl alcohol. The reason is
that because washing the precipitate,
removes some excess ions which is ideal for a
sample to be measured.

In phosphorus determination, there may be
some errors encountered. These errors may
change the results depending on the
parameters used. Example: impurities in the
sample were not removed (mass measured
increases), the precipitation process was not
complete (some ions will still be present in
the sample), not rinsing the ppt before drying
it (the mass measured will increase greatly
because other soluble chemicals may
crystallize in the sample)

In precipitating the fertilizer sample,

was added slowly. The concept behind this
process can be explained by the concept of
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relative supersaturation as shown by eq. 2,
the Von Weimarn ratio.


( )

()

The Vonn Weimarn ratio where Q is the
concentration of reactants before
precipitation and S is the solubility of the
precipitate in a medium. Theoretically, the
relative supersaturation of a sample must be
low. By adding the precipitating agent

slowly, the Q in eq.2, acquires a low value
which makes the relative supersaturation low
in value. There are other measures that
minimize the value of relative
supersaturation like stirring the solution to
avoid build-up of concentration. Precipitation
using dilute solution also lowers the value of
Q. Adjusting pH may increase S but not too
much.

In the experiment, the precipitate was
washed with distilled water and ethanol. In
theory, washing the precipitate with ethanol
will reduce/ remove the excess ions that are
found in the precipitate. This accounts for a
more accurate measurement of the
precipitates weight because the ions which
may have been accounted were removed by
the ethanol wash.

CONCLUSION AND RECOMMENDATION

The moisture and phosphorus composition of
the fertilizer sample were successfully
calculated in the experiment using
gravimetric techniques. It was observed that
percent composition of P and

are higher
in dry sample compared to wet sample. This
is due to the more concentrated composition
of the dry sample which has no or less
moisture unlike the wet sample which still
accounts the mass of the moisture content.
The experiment was able to apply gravimetric
methods in isolating a sample for weighing
and measuring for further computation. It is
recommended that the experiment should be
conducted in a more controlled environment.
Factors such as pressure and temperature
might contribute to the errors in the
experiment. Nevertheless, the experiment
didnt experience much error.
REFERENCES

[1] Wired Chemist.
http://www.wiredchemist.com/chemistry/in
structional/laboratory-tutorials/gravimetric-
analysis (accessed September 20, 2014).

[2] Texas A&M University.
https://www.chem.tamu.edu/class/majors/t
utorialnotefiles/gravimetric.htm (accessed
September 20, 2014).

[3] University of Massachusetts Amherst.
http://www.ecs.umass.edu/cee/reckhow/co
urses/572/572bk15/572BK15.html
(accessed September 20, 2014).

[4] East Stroudsburg University.
http://www.esu.edu/~scady/Experiments/F
ertilizer.pdf (accessed September 20, 2014).