Quantitative Inorganic Analysis Laboratory
Formal Report
Date Performed: 28
August 2015
Date Submitted: 22
September 2015
Department of Mining,
Metallurgical and
Materials Engineering
College of Engineering
Instructor: Searle
Aichelle Duay
Gravimetric Determination of Moisture and Phosphorus in Fertilizer Samples
Gravimetric Determination of Moisture and
Phosphorus in Fertilizer Samples
D.A. Mercado
In a fertilizer sample, the two determinants of its purity is the amount of
phosphorus and moisture content. Using the different processes of gravimetric
determination, the purity of the fertilizer was determined. The moisture content was
calculated using the wet and dry weights of the sample, which were obtained using
the heating and cooling process, and was found to be 0.4312% 0.0001. The
phosphorus content on the other hand was obtained using the precipitation
gravimetric process by allowing the sample to precipitate with MgSO47H2O and
NH3. With the use of the gravimetric factors, the %P was obtained at
11.99% 0.0002 for the wet and 12.04% 0.0002 for the dry basis. The % P 2O5
at a wet and dry basis were also found to be 27.47% 0.0005 and 27.59% 0.0005,
respectively. It is given that the amount of phosphorus in the form of P 2O5 is 20%
which gives a percent difference of 37.35% and 37.95% respectively for the wet and
dry basis.
Mercado, 2015| 1
Introduction
The main components of fertilizers are nitrogen,
phosphorus and potassium which aids in the growth of
plants by providing the nutrients that it needs. [1]
Phosphorus is an important nutrient which plays a large
role in the plants growth as it helps utilize the starch
and sugars and can help with the photosynthesis
process. The phosphorus deficiency in plants can be
remedied with the use of phosphate fertilizers which is
why it is important to determine the phosphorus content
in the sample to test its purity. [2] Another important
factor in the fertilizer samples purity is its moisture
content. This determines the quality, grade and storage
life of the fertilizer. [2]
The technique used to determine the phosphorus and
moisture content was the gravimetric method of
analysis. This type of analysis is centered on the
measurement of the mass using the analytical balance.
Gravimetric analysis is a very accurate and precise
method of determining the amounts of different
components in the fertilizer sample. The precipitation
gravimetry, which was used to determine the
phosphorus content, is done by converting the analyte
into a sparingly soluble precipitate that can be weighed.
[3]
The goal of the experiment is to quantitatively
determine the moisture content through constant
weighing and the phosphorous content through
precipitation gravimetry. The gravimetric process must
be properly done to achieve a pure precipitate that can
be weighed.
Materials and Methods
The crucible was prepared by thoroughly washing one
crucible and its cover. Both parts are then labeled properly
using a pencil. The crucible, along with its cover, was
then placed in the oven with the temperature on 110C
until the next laboratory session. Using a pair of crucible
tongs, the hot crucible and cover were then transferred
into a desiccator. The desiccator was then moved to the
balance room and was left to cool for 15 minutes. After
cooling the crucible, the weight was then taken. After it
was weighed, the crucible was the transferred back into
the oven, with its cover slightly ajar, to let it dry for 30
minutes (with the temperature still at 110C). The heating
and cooling process was done continuously until the
differences of the consecutive weights were only 0.0002
to 0.0003 g apart from each other or in other words, the
constant weight was obtained.
After the constant weight of the crucible and the cover
were obtained, 3.0 g of fertilizer sample (to the nearest 0.1
mg) were then weighed into the constantly weighed
Gravimetric Determination of Moisture and Phosphorus in Fertilizer Samples
crucible. The crucible with the fertilizer sample was then
placed in to the oven with the cover slightly ajar to dry for
1 hour at 110C. At the one hour mark the crucible was
then transferred into the desiccator. The desiccator was
then transferred back into the balance room and the
crucible was left to cool for 15 minutes. The weights of
the crucible, cover, and fertilizer were then taken, taking
note not to open the crucible during the process. The
crucible was then returned into the oven and was left to
dry for 30 minutes. The heating and cooling was
repeatedly done until the constant weight was obtained.
The weight of a filter paper was taken and then placed
in the desiccator while not in use. The dried fertilizer
sample was then transferred into a 250-mL beaker along
with 40 mL of distilled water. This was ten stirred to
dissolve the solid sample. Since the fertilizer sample did
not dissolve completely, it was then filtered, using a filter
paper that has not been weighed. After filtering, 45 mL of
10% MgSO47H2O solution was then added into the
filtrate of the fertilizer sample and distilled water mixture.
150 mL of NH3 was then added into this mixture while
constantly stirring, wherein the first 50 mL was added
dropwise and the rest was slowly added. The mixture was
then allowed to rest at room temperature for 15 minutes.
Then this was filtered using the pre-weighed filter paper.
The precipitate was also washed with two portions of 5
mL distilled water and two portions of 10 mL 95%
ethanol. The filter paper was then spread on a filter paper
and was left in the locker to dry until the next laboratory
session. After drying, the filter paper was transferred into
a beaker and was placed in the oven for 1 hour at 110C.
This was then placed in a desiccator and cooled for 15
minutes. After cooling, the filter paper was taken out of
the beaker and was weighed.
Results and Discussion
Gravimetric methods are a mass measurement based
analysis. The mass of a pure compound that is related to
the analyte is quantitatively determined. [3] In order to
achieve accurate and precise data, the constant weighing
process was done for this experiment. This process is
significant in the gravimetric method since it eliminates
any errors in the measurements of the weights such as
change in moisture content every time the crucible is
exposed to air. In obtaining the constant weight, the last
two consecutive weights should have a difference of
0.0002 to 0.0003 g. The tolerance of the analytical
balance used was at 0.0002 g which means that the
values of the weights only vary slightly and are in the
range of the uncertainty of equipment used, giving a more
precise value. As seen in Table I, the constant weight
obtained varied from the first weighing done by 0.0007 g
which proves that it is important to use the constant
weighing process in order to obtain more accurate and
precise results.
Mercado, 2015 | 2

Table I. Constant Weighing of Crucibles with Covers
Weighing No. Weight [g]
1 37.0100 0.0002
2 37.0107 0.0002
3 37.0107 0.0002
Constant Weight 37.0107 0.0002
The moisture of the fertilizer was then obtained in
order to determine the purity of the sample. Moisture
determination is important since it accurately determines
the percent mineral content in the fertilizer. [4] The
fertilizer was ground up to small powder-like particles
before it was weighed and oven dried in order to speed up
the drying process since the surface area of the sample has
been increased. The ground fertilizer sample was then
obtained using weighing by difference giving a weight of
2.9916 0.0002 g. It is better to use weighing by
difference than direct weighing since the sample is placed
directly into the glassware being used for the experiment,
as opposed to a secondary weighing vessel such as a
watch glass or filter paper. This method eliminates any
loss of sample since this can be easily seen if the
weighing device is very precise. The method gives a
more accurate and precise amount of the sample that is to
be used.
The crucible was repeatedly heated, cooled and
weighed in order to obtain the constant weight. After
heating, the crucibles were cooled to room temperature
before they were weighed. This step is important since the
hot air is rising and being replaced by the cold air in the
room thus creating air currents. These air currents can
greatly affect the reading in the analytical balance if the
crucible was weighed while it was still hot. [5] After the
constant weighing of the fertilizer sample in the crucible,
the net weight of the dried sample was obtained to be
2.9787 0.0002 g. This was calculated by subtracting
the constant weight obtained of the crucible with the
sample with the constant weight of the empty crucible.
The difference of the wet and dry sample weights gives
the mass of water in the fertilizer sample. The percent
moisture was then calculated to be 0.4312% 0.0001.
The gravimetric analysis of the amount of phosphorus
in the fertilizer sample was then done using precipitation
gravimetry. The dried fertilizer sample previously used
was dissolved in distilled water and was made to react
with MgSO47H2O and NH3 thus creating a magnesium
ammonium phosphate hexahydrate precipitate.
Gravimetric Determination of Moisture and Phosphorus in Fertilizer Samples
The Ammonia was added dropwise and slowly in order
to regulate and control the acidity of the solution. If a
basic solution was created then PO43- would have been
formed instead of HPO42 ions. The hydroxide ions will
then precipitate with Mg2+ forming magnesium hydroxide.
If the solution is too acidic on the other hand, then H 2PO4-
will be formed instead of a precipitate. In order to avoid
this and properly form the magnesium ammonium
phosphate hexahydrate precipitate, the ammonium should
be added very slowly and dropwise. After the addition of
the ammonia, the solution was left to stand and digest for
15 minutes in order to complete the precipitation reaction.
Here, the precipitate is left to stand in the mother liquid
before it is filtered. A coaulated colloid would be easily
filtered if it is allowed to digest since the weakly bound
water particles are removed from the precipitates creating
a denser crystal.[3] The precipitate was then obtained by
filtration and was then washed with distilled water
followed by 95% ethanol in order to dry the precipitate
much faster. The precipitate was then oven dried and
weighed. The weight of the precipitate allowed for the
calculation of the %P and %P2O5 as seen in Table II.
Table II. Amount of Phosphorus in the Fertilizer
Sample
Fertilizer Component Percentage
%P (wet basis) 11.99% 0.0002
%P (dry basis) 12.04% 0.0002
% P2O5 (wet basis) 27.47% 0.0005
% P2O5 (dry basis) 27.59% 0.0005
Given that the theoretical percentage of Phosphorus in
the form of P2O5 was 20%, the percent difference of the
wet and dry basis were 37.35% and 37.95% respectively.
The results obtained vary greatly from those obtained by
the other groups since the percent difference is large.
There is also a great range of values from the different
groups, 14.10%-28.05% for the wet and 14.79%-27.84%
for the dry, due to the large percent differences. The
percent difference of the other groups ranged from 3.25%-
39.2% for the dry and 3.45%-40.25% for the wet.
The possible sources of error in the experiment could
come from the mishandling of the crucible. This could
lead to added moisture content, loss of sample or even the
change of the weight of the crucible if it has been dropped
leading to its chipping or breaking. If the cooling time for
the crucible was consistently varied then this may also
lead to inaccurate results. The loss of the sample can lead
to a lower moisture and phosphorus content which can
give a very high percent error. If the solution was not left
to digest long enough, a larger percentage of phosphorus
may be collected due to the impurities of the precipitate
leading again to a high percent error.
Mercado, 2015 | 3
Conclusions and Recommendations
The moisture content of the fertilizer sample was
calculated as 0.4312% 0.0001, which gives a very low
percentage. This shows that the fertilizer is of high purity
as it has very little amounts of water in its composition
and has more of its main nutrients. The amount of
phosphorus on the other hand was seen to be 27.47 %
0.0005 for the wet basis and 27.59% 0.0005 for the
dry basis in the form of P2O5. Given that the theoretical
amount of P2O5 has been determined to be 20%, this gives
a percent difference of 37.35% and 37.95% respectively
for the wet and dry basis. The deviation from the
theoretical amount could have risen from errors in the
experiment proper such as the loss of the precipitate in the
filtration process or the incomplete precipitation of the
phosphorus in the fertilizer. Another method that could be
used other than Thermo gravimetry is the Karl Fischer
method. This method has the same benefits as the
gravimetric method but also has a direct water
measurement and can be used for many different kinds of
samples. It allows for the analysis of volatile materials but
is more complex than the other methods

References

[1]North Carolina Department of Agriculture and

Consumer Services. http://www.ncagr.gov/CYBER/
kidswrld/plant/nutrient.htm#Primary
%20Nutrients(accessed September 10, 2015).

[2] Plants and Soil Science eLibrary. http://passel.unl.

edu/pages/informationmodule.php?
idinformationmodule=1130447043&topicorder=2
(accessed September 19, 2015).

[3] Skoog, D.; West, D.; Holler, F.J.; Crouch, S.

Fundamentals of Analytical Chemistry,9th ed.; Cengage
Learning Asia Pte Ltd: Pasig, 2014; pp 274-280.

[4] University of Massachusetts Amherts. http://people.

umass.edu/~mcclemen/581Moisture.html (accessed
September 19, 2015).

[5] California State University Dominguez Hills. http://

www.csudh.edu/oliver/demos/heatcruc/heatcruc.htm
(accessed September 19, 2015).

[6] Morse, D.; Baer, D. Laboratory Balances: How They

Work, Checking Their Accuracy. ASCP Journals
[Online] 2013: 10.1309/QYR5UV73FRY2Y BMJl.
abmed.ascpjournals.org/content/35/1/48.full. pdf
(accessed September 19, 2015).

Gravimetric Determination of Moisture and Phosphorus in Fertilizer Samples Mercado, 2015 | 4

 Appendix I

Table I. Constant Weighing of Crucibles and Fertilizer Sample (with Cover)

Weighing No. Weight [g]

1 39.9680 0.0002
2 39.9895 0.0002
3 39.9894 0.0002
Constant Weight of Crucible + Sample 39.9894 0.0002
Constant Weight of Empty Crucible 37.0107 0.0002
Mass of Water 0.0129 0.0003
% Moisture 0.4312% 0.0001

Table II. Obtained Weights in the Determination of Phosphorus in Fertilizer Samples

Object Weighed Weight [g]

Sample Weight 2.9916 0.0002
Net Weight of Dried Sample 2.9787 0.0002
Weight of Filter Paper 0.9155 0.0002
Weight of air-dried Filter Paper with Precipitate 2.5056 0.0002
Net Weight of Dried Precipitate 1.5901 0.0003

Calculations
Mass of Water = Sample Weight Dried Weight r = (0.0002) 2 (0.0002) 2 = 0.0003
= 2.9916 2.9787 = 0.0129 g
2 2
0.0129
% Moisture = x100 0.4313% r = (0.004312) 0.0003 0.0002 0.0001
2.9916 0.0129 2.9916
Weight Dried Precipitate = 2.6056 0.9155 = 1.6901g r = (0.0002) 2 (0.0002) 2 = 0.0003

1.5901 30.97
0.0003
2
0.0002
2

%Pwet = 137.31 x100 11 .99% r = (0.1199) 0.0002

1 .5901 2.9916
2.9916
1.5901 30.97 0.0003
2
0.0002
2

%Pdry = 137.31 x100 12.04% r = (0.1204) 0.0002

1.5901 2.9787
2.9787
1.5901 1mol 141.94 0.0003
2
0.0002
2

%P2O5,wet = 2mol 137.31 x100 27.47% r = ( 0 .747) 0.0005

1.5901 2.9916
2.9916
1mol 141.94
1.5901 0.0003
2
0.0002
2

%P2O5,dry = 2 mol 137. 31 x100 27.59% r = ( 0 . 2759 ) 0.0005

1.5901 2.9787
2.9787

Appendix II
Answers to Questions:
Gravimetric Determination of Moisture and Phosphorus in Fertilizer Samples Mercado, 2015 | 5
1. Discuss the principles of operation of mechanical and electronic balance.
A mechanical balance is used by placing an object with an unknown mass on one end and an object with a known
mass on the other. The lever opposes the torque exerted by the mass of the unknown object as the object of the
known mass is moved. Once the lever is balanced, the distances of the two objects can be used to determine the
force of the unknown object and therefore its mass as well. An electronic balance on the other hand works on the
concept of magnetic force restoration. The force of the object being weighed is simultaneously being lifted by an
electromagnet. The opposing forces are then measured which then gives the mass of the object being weighed. [6]
2. Discuss the possibility of using NH4Cl instead of NH3 to precipitate the phosphorus in the fertilizer sample.
NH4Cl cannot be used instead of NH 3 since MgCl2 will be formed which means that the ammonium phosphate
hexahydrate precipitate will not be formed and consequently the phosphorus content cannot be measured or
determined.

Gravimetric Determination of Moisture and Phosphorus in Fertilizer Samples Mercado, 2015 | 6