GRAVIMETRIC DETERMINATION OF MOISTURE AND

PHOSPHORUS IN FERTILIZER SAMPLE

A.L. BULIGAN
1
INSTITUTE OF CHEMISTRY, COLLEGE OF SCIENCE
2
DEPARTMENT OF FOOD SCIENCE AND TECHNOLOGY, COLLEGE OF HOME ECONOMICS
UNIVERSITY OF THE PHILIPPINES, DILIMAN, QUEZON CITY, PHILIPINES
DATE PERFORMED: AUG. 27, 2014
INSTRUCTORS NAME: COLLEEN ROSALES


ABSTRACT
Determination of %moisture, %phosphorus and %phosphorus pentoxide content of a fertilizer
sample is the main goal of the study. The experiment uses the principle of gravimetric analysis. The
sample undergoes repeated heating and cooling process in an oven at constant temperature at 110
O
C
and a desiccator respectively. A precipitation of MgNH4PO4*6H2O was also observed to determine the
final weight of the sample. A % moisture of 2.62500.01% was obtained which is within range of the
accepted value in the market. An approximate of 10% and 24% of %P and % P2O5 respectively was
also obtained in this experiment which is also within the range of the accepted value in the fertilizer
market.



INTRODUCTION
Gravimetric analysis is a quantitative
analysis in which it can determine the
amount of species in a material by converting
it to a product that we can isolate and weigh
completely
[1]
. This can be classified into two
types: precipitation and volatilization. Under
precipitation method, you will separate the
specie thru precipitation reaction, filtering,
washing the precipitate and conversion to a
product of known composition. In
volatilization method, the specie that is being
studied is volatilize at a suitable temperature,
collected then weighed.
Fertilizers contain essential nutrients
that are necessary for plant growth such as
phosphorus, nitrogen and potassium. In
particular, phosphorus when applied to soil
helps promote root growth, winter hardiness,
stimulates tillering, and often hastens
maturity and it also and aids in
photosynthesis under Calvin Cycle
[2]
.
In this experiment, the moisture
content of the fertilizer sample was
determine by oven drying the sample to a
constant temperature at 110
O
C. Also in this
experiment, the phosphorus content of the
fertilizer was measure by precipitating the
fertilizer sample as magnesium ammonium
phosphate hexahydrate, MgNH4PO4*6H2O.
The chemical reaction is given as follows:
(1)

METHODOLOGY
A. Preparation and Constant Weighing of
Crucibles
Crucible with cover was thoroughly
wash and clean. This was place in the oven at
110
O
C with the cover slightly ajar and was
kept until the next period. The crucible was
handle using crucible tongs and a watch glass
throughout the experiment. The crucible was
transfer to a desiccator and was allow to cool
for 15minutes. The weight was then obtained
using an analytical balance. After weighing,
the crucible with cover was transfer back to
the oven at 110
O
C for 30mins to dry. The
cover was left ajar. The cooling and heating
process was repeat until a constant weight
was obtained.
B. Moisture Analysis
The fertilizer was weigh up to 3.0g to
the nearest 0.1mg into the constantly weigh
crucible using the technique weighing by
difference. This was then placed back to the
oven at 110
O
C for 1 hour with the cover
slightly ajar. The crucible was then
transferred to the desiccator and was allow to
cool for 15mins. The crucible with the
fertilizer was weigh. After weighing, it was
transfer back to the oven with the same
temperature for 30mins. This process of
cooling and heating was repeat until a
constant weigh was obtained.
C. Preparation of Solutions
A 500ml of 10% (w/v) MgSO4*7H2O
solution was prepare and three 500ml of
2M NH3 solution.
D. Precipitation of MgNH4PO4*6H2O
A fluted filter paper was prepare and
was weigh. The dried sample was place in a
clean and dry beaker. This was dissolve with
40ml of distilled water. The resulting solution
was filter afterwards using a different filter
paper which is not weighed. Discard the filter
residue. After filtration, 45ml of 10% MgSO4
7H2O was added to the filtrate. 150ml of 2M
NH3 was added slowly while stirring. The
solution was covered with a watch glass and
was allowed to precipitate for 15mins in the
fume hood. The solution was filter using the
pre-weighed filter paper. The filter paper was
wash with 5ml distilled water twice and was
wash again with 5ml of 95% ethanol. The
filter paper with the fertilizer sample was
place in a beaker and was to the oven at
110
O
C for 1 hour. It was then transferred to
the desiccator for 15mins. This was weigh
using an analytical balance and the weigh was
recorded.
RESULTS AND DISCUSSION
The whole experiment consists of two
parts; the first one is to measure the moisture
content of the sample and the second one is
to obtain the phosphorus content of the
sample. This goal was achieve using
gravimetric analysis. The first step of the
experiment was done by taking the constant
weight of the crucible. This was place in the
oven at 110
O
C for 30mins to dry then cooled
for 15mins in the desiccator. The cooling of
the crucible is crucial to avoid errors caused
by air currents. A buoyant effect on the pan
and the object was exert by convection
currents within the balance. Warm air inside
the crucible is lighter compare to the same
volume at a lower temperature [3]. Using
crucible tongs is also important in this
experiment because handling the crucibles
with our bare hands may affect the result of
the data. Our skin contains moisture that will
adhere to the crucible itself. After the initial
weigh in, the whole heating-cooling-weighing
is repeated until a constant weight was
observed. A constant weight will be obtain if
the next weight is within the range of 0.0003
from the previous recorded weight. This
implies that no more moisture can be remove
from the crucible. This assumption is based
on the uncertainty of the analytical balance:
(1)

Table 1. Constant Weighing of the Crucible
Weighing # Weight (g)
Weighing 1 32.48200. 0002
Weighing 2 32.48130. 0002
Weighing 3 32.48130. 0002
Constant weight 32.48130. 0002

After getting the constant weight of
the crucible, 3.0171grams of the fertilizer
sample was obtained using the technique
weighing by difference. This technique is
done by noting the initial mass of the
container holding the fertilizer sample then
noting the mass again after transferring the
sample to the constant weighed crucible. The
mass decrease of the container is then
recorded as the mass of the sample obtained.
This technique also prolongs the lifetime of
the analytical balance by weighing light vials
instead of heavy Erlenmeyer flasks since the
balance can only hold up to 200 g. This was
use instead of the direct method because of
the amount of the sample might not be
transferred completely due to intermediate
objects like watch glass. The crucible was
then heated in the oven 110
O
C for an hour
with the cover slightly ajar. The cover was
place slightly ajar so that the moisture in the
sample can evaporate. It was then transferred
to the desiccator for 15mins to cool. After
cooling, the crucible was weigh.
Table 2. Constant Weighing of Crucible with
Sample
Weight
Weighing 1 35.50110.0002
Weighing 2 35.46750.0002
Weighing 3 35.46650.0002
Weighing 4 35.41920.0002
Constant weight of
crucible + sample
35.41920.0002
Net weight of dried
sample
2.93790.0002

The mass of water which is
0.0792000.0003 was also obtained by
subtracting the initial amount of the sample
to the net weight of the dried sample. The
percent moisture can be calculated using the
formula:
%moisture
=

A % moisture of 2.6250 0.01 was
obtain using the formula above.
Aside from the oven drying method of
determining the moisture, there is also a
different method which is the direct method
of moisture determination. The direct method
may use a moisture balance, which is faster
and more accurate, compared to an oven
drying, which takes many hours to complete.
A moisture balance also weighs and heats a
sample simultaneously, reducing errors
caused by moisture evaporation during
transport and weighing.
The second part of the experiment
took place after obtaining the %moisture of
the sample. A fluted filter paper was made
because the filtrate is much more important
than the residue. After dissolving the sample
using distilled water, it was then filtered.
45ml of 10% MgSO47H2O was added to the
filtrate. 150 mL of 2M NH3 solution was then
added slowly while stirring. This now is the
precipitation part of the gravimetric analysis.
Slowly addition of NH3 avoids the
supersaturation which is a requirement in
lowering the Von Weimarn ratio.
Supersaturation varies inversely with the
particle size
[4]
. It means that a small
magnitude of supersaturation means having a
smaller magnitude for the Von Weimarn
Equation:

where:
Q = concentration of reactants before
precipitation.
S = solubility of precipitate in the medium
from which it is being precipitated.

Thus resulting to a larger particle size
of the precipitate. A small magnitude for R is
required so that a larger precipitate will form.
NH4Cl was not used instead of NH3 because
the digestion process requires a basic
substance wherein NH4Cl is acidic. The
beaker was placed under a fume hood for
about 15mins. This part of the experiment is
called digestion. It promotes slow
recrystallization of the precipitate. Digestion
of crystalline precipitates for some time after
formation frequently yields a purer, more
filterable product
[4]
. This was then filtered
using the fluted filter paper and was wash
twice using distilled water and 95% ethanol.
Ethanol was used because the precipitate
formed is insoluble to ethanol which is a non-
polar substance. Ethanol also displaces water
and helps to promote the drying of
precipitate since it can easily evaporate.
The filter paper was place in a beaker
and was put inside the oven at 110
O
C for 1
hour. This was done so that the filter paper
together with the sample will dry completely.
It was allow to cool inside the desiccator for
15mins. This was then weighed and recorded.
Table 3. Sample Size / Weight of Filter Paper /
Weight of Precipitate
Weight (g)
Sample weight (as
received)
2.93790.0002
Sample weight (dried) 3.01710.0002
Weight of filter paper 0.74260.0002
Weight of filter paper +
precipitate
3.22240.0002
Net weight of dried
precipitate
2.47980.0002

After obtaining these data,
%phosphorus (%P) and %phosphorus
pentoxide (%P2O5) in a dry and wet basis
using the following formulas:











Using the formula above, the
following data were obtained:
Table 4. Reported Values
%P (wet) 10.6530.006
%P (dry) 10.3740.06
%P2O5 (dry) 24.4110.006
%P2O5 (wet) 23.7710.06

By law, fertilizer sold in the market
should have a label guaranteeing the
percentage of nutrients. Three combinations
(fertilizer grade or analysis) on the product
identify percentages of nitrogen (N),
phosphate (P2O5), and potash (K2O),
respectively
[5]
. For example, a 20-10-5
fertilizer contains 20% nitrogen, 10%
phosphate, and 5% potash. With the data
obtain in the experiment; it can be identify
what is the ratio of the nutrient inside the
fertilizer.
CONCLUSION AND RECOMMENDATION
Determination of %moisture, %P,
%P2O5 was carried out properly in the whole
experiment. % moisture of 2.6250% + 0.01 is
within the accepted value of 1-10%. In this
experiment, a value of %P which is 10% and a
value of 23-23% for %P2O5 were obtained.
Since there is no accepted value of %P and %
P2O5 that is being used by fertilizer
manufacturers and the amount that is being
used depends on the amount of the other
nutrients
[6]
. Sources of error in this
experiment would be incorrect weighing
technique since theres a possibility that the
sample might get spill during the transferring
from the desiccator to the oven and analytical
balance. The temperature of the surrounding
may not be optimal. One source of error could
also be the time used for the precipitate to
form. The 15mins allotted might not be
enough for the large precipitate to form since
it could still be seen that some smaller
precipitate passed through the filter paper. It
could be recommended that the direct
method which is faster and more accurate
could be used instead of oven-heating method
to determine the moisture content of the
sample. This would have a lesser error
propagation.
REFERENCES
[1] Ebbing, Darrell ; Gammon, Steven, General
Chemistry, Enhanced Edition , 2011
[2] Soils - Part 6: Phosphorus and Potassium
in the Soil. Plant and Soil Sciences eLibrary
[3] Harris, D. (2007). Quantitative Chemical
Analysis. (8
th
ed.).New York:W.H. Freeman
and Company
[4] Skoog, D., West, D., Holler, F. J., & Crouch,
S. (2004).Fundamentals of analytical
chemistry. (8
th
ed.). Canada: Brooks/Cole-
Thomson Learning.
[5] Understanding Fertilizers. Colorado State
University.
http://www.ext.colostate.edu/mg/gardennot
es/232.html
[6] The Basics of Fertilizer Calculations for
Greenhouse Crops. Virginia Cooperative
Extension.
http://pubs.ext.vt.edu/430/430-100/430-
100.html