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Gravimetric Determination of Moisture and Phosphorus in Fertilizer Samples
Diego E. Padillaa,*, Hernan Delizob
Institute of Chemistry, University of the Philippines Diliman, Quezon City, Philippines
b
ABSTRACT
In this experiment, the moisture and phosphorus content of the fertilizer are to be determined through the use of gravimetry. This was first done be getting the
constant weight of the crucible and fertilizers. This allowed for a controlled experimentation environment. The fertilizer was then made to be dissolved and
filtered. Afterwards, MgSO47H2O and NH3 were added to the filtrate to make the precipitate occur. The mixture was then filtered once more after it had digested
enough. The results obtained from the experiment show that the percent yield of phosphorus is 0.5940% which is far from the advertised percentage on the
packaging. Because of this, it can be said that the experiment was a failure and that a conclusion cannot be made.
1. Introduction
Gravimetric analysis is a technique used to determine the
mass of a certain substance by using a compound that it can be
derived from. The substance that is being quantified is classified as
the analyte. There are 2 methods of gravimetric analysis. The first
one is called the volatilization method which involves chemically
separating the analyte from the compound thru chemical means. The
second method is the precipitation method which involves turning
the analyte into a precipitate so that it can be filtered.[2]
Fertilizers typically contain moisture and other essential
ingredients needed for plants to grow healthy like nitrogen,
phosphorus and potassium. The percentage amount of these
substances are placed on the packaging to inform the consumer how
much of each ingredient there is. Thus, it is important to make sure
that the labels on these products are accurate. Thru the use of
gravimetry, the percent composition of the moisture and
phosphorus content will be determined.
In this experiment, the precipitation method will be used.
The analyte will be first turned into a precipitate and then filtered
out. From there, the samples will be weighed and the moisture and
phosphorus content will be calculated.
2. Materials and Methods
2.1. Solution Preparation
The first part of the solution preparation was obtaining 500mL of
10% (w/v) MgSO4 H2O. This was done by first weighing the correct
amount of MgSO4 that was needed to be dissolved to achieve the right
molarity. Afterwards, the MgSO4 was dissolved and stored in a
volumetric flask.
Three solutions of 500 mL of 2M NH3 were prepared from a sample
of concentrated NH3. The right volume of NH3 was obtained and
diluted to the right molarity. The prepared NH3 was stored in a high-
density polyethylene volumetric flask until use.
2.2. Obtaining the Constant Weight
A crucible and its cover were first cleaned and labelled
appropriately. It was then placed inside the oven set at 110C for
over a period of 2 days with the cover slightly ajar. Afterwards, the
crucibles were taken out of the oven and placed inside a desiccator
for 15 minutes for it to cool down. The crucibles then had their
weight measure through the use of an analytical balance. After
weighing, the crucibles were placed back inside the oven set at 110 C
for 1 hour. This process was repeated until a constant weight of the
crucible had been achieved. Once constant weight had been achieved,
3.0g of fertilizer was weighed by difference into the crucible. The
crucible with fertilizer was weighed to obtain the wet mass of
fertilizer sample. The crucible with fertilizer was placed inside the
over set at 110C for drying for about 2 days once again. The cycle of
heating for 1 hour, placing it into the desiccator, cooling for 15
minutes and weighing on the analytical balance was repeated until a
constant weight had been achieved. The dried fertilizer was then
transferred to a 250 mL beaker. 40mL of distilled water was added
to the beaker. The mixture was stirred until the fertilizer had
completely dissolved. The mixture was then filtered until a clear
filtrate was obtained. 45mL of 10% MgSO47H2O was added to the
clear filtrate. 150mL of 2M NH3 was added slowly into the solution.
The mixture was made to stand for 15 minutes to allow the
precipitate to settle. The solution was then filtered through a pre-
weighed filter paper. After the filtration, the filter paper was washed
with 95% ethanol and was then allowed to be air dried. The filter
paper was then placed into the oven with a temperature of 110C for
1 hour. The filter paper was taken out after an hour and allowed to
cool for 15 minutes. The fertilizer and filter paper were then weighed.
3. Results and Discussion
In the experiment, a constant weight was needed when
drying both the crucible and the fertilizer to avoid the interference
from moisture in the air. The moisture in the air could interfere with
the weight of the components being measured and the formation of
the precipitate.
Once constant weight had been achieved, the precipitate
was ready to be prepared. MgSO47H2O and NH3 were both used as
precipitating agents to produce MgNH4PO46H2O. They were used
since both have reactive properties with the precipitate allowing the
precipitate to become bigger making it easier for the filter paper to
catch. If done correctly, the precipitate obtained should be pure and
free of contaminants from other ions. Theoretically, this should show
that the moisture and phosphorus content in the fertilizer is of the
same percentage as advertised on the packaging.
Based on the data gathered (see Table 1 Appenidix), the
percentage of both phosphorus and the moisture is lower than what
is said on the packaging. This mismatch could have been possibly
caused by interference of the moisture in the air. When transferring
the crucible from the oven into the desiccator, the crucible was
exposed to air which may have altered the weight by a small chance.
The impurities in the air may have altered the weight of the
precipitates since they may have latched onto the crystalline solids
and added to the weight. Another possible source of error is the
impurities in the filter paper used. The filter paper may have had
impurities while filtering the solution. These impurities could have
also altered the filtration causing the filter paper to filter less of the
analyte being obtained.
4. Conclusion and Recommendations
 P a g e |2

Summary of important results (should answer: so what). Discuss

degree of success or failure of the experiment. If necessary and Appendices
possible, include suggestions for improvement (on the method used,
NOT on the course or how it is being handled). Be direct in stating
conclusion and recommendation (dont include background Table 1. Table of Data
information).
Group
Sample:
Based on the results obtained, the advertised percentage of 1
phosphorus and moisture on the packaging is wrong. However, due
to human error, the results of the experiment have a possibility of Delizo,
being incorrect. Because of these factors, no conclusion can be made
from the experiment and more trials are needed to confirm the Padilla
findings.
Mass of crucible, g 26.5302
When this experiment is being done, it is advised that the crucible
should have as little air exposure possible since a bit of air exposure
can alter its values significantly. It would also be advisable to use Mass of fertilizer as-
more fertilizer samples since the fertilizer samples used were small 3.0015
received, g
and that could have affected the results.

References Mass of fertilizer dried,

2.9696
g
[1] Crouch, S. R.; Holler F. J.; Skoog, D. A.; West, D. M. Fundamentals
of Analytical Chemistry 9E; Brooks/Cole: Belmont, 2014; pp. 280-
283. Mass of filter paper, g 1.2489

Mass of precipitate +
[2]Introduction to gravimetric analysis: 1.3887
Volatilization gravimetry. Khan Academy, filter paper, g
www.khanacademy.org/science/chemistry/chemi
cal-reactions-stoichiome/limiting-reagent-
Mass of precipitate, g 0.1398
stoichiometry/a/gravimetric-analysis. Accessed
5 Sept. 2017.
Mass of H2O, g 0.0319
[3] Wired Chemist. Gravimetric Analysis.
http://www.wiredchemist.com/chemistry/instructional/laborator % Moisture 1.063%
y-tutorials/gravimetric-analysis. Accessed 05 September 2017.
Mass of P, g 0.01764

%P as-received 0.5877

%P dried 0.5940

Mass of P2O5, g 0.04042

%P2O5 as-received 1.347

%P2O5 dried 1.362