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Quantitative Inorganic Analysis Laboratory

Formal Report
Date Performed: 25
August 2015
Date Submitted: 17
September 2015
Institution/Department:
Department of
Chemical Engineering
College: Engineering
Instructor: Cris Angelo
Pagtalunan

Gravimetric
Determinatio

n of Moisture and Phosphorus in Fertilizer


Samples
M. K. Coo
Gravimetric analysis establishes an amount of analyte through measuring
the mass of a pure substance containing the analyte. In this experiment, %P and
%P2O5 were obtained through precipitation gravimetry. The fertilizer sample
undergone drying and cooling processes through the use of crucibles and tongs,
until a constant weight was reached. A %Moisture of 1.4329 was then calculated.
The sample was precipitated as MgNH4PO46H2O and through the use of
gravimetric factors: 5.5% P and 12.5251% P 2O5 were obtained. The experiment
was done to determine the composition and effectiveness of a fertilizer sample.
The fertilizer therefore had low moisture content and a low P and P 2O5 content.

Gravimetric Determination of Moisture and Phosphorus in Fertilizer Samples

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Organic Chemistry Laboratory

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Introduction
Fertilizers are commonly used in
plants and crops to provide nutrients. They
contain compounds of potassium and
phosphorous which are needed by plants to
grow, which may be lacking in the soil where
they are planted. For quality purposes, the
contents of these compounds must be
closely observed and determined to ensure
proper nutrient content. Among other
methods, gravimetry is used because of its
accuracy and low-cost.
Gravimetry is a method in analytical
chemistry used to obtain masses, percent
composition, and other unknown quantities
through the use of an analytical balance, a
device that accurately measures weight.
There are two types of gravimetry, mainly
precipitation gravimetry and
volatilization gravimetry. In precipitation
gravimetry, the analyte is precipitated as a
known compound, filtered, dried, and
weighed to obtain percent compositions of
the constituent elements and compounds in
the analyte. Ideally, the precipitate should
be 1) Easily filterable, 2) of known chemical
composition, and 3) of low solubility to
minimize loss of analyte during filtering and
washing.
In this experiment, a sample of
commercial fertilizer, more specifically the
phosphorous (P2O5) in it, is precipitated as
magnesium ammonium phosphate
hexahydrate (MgNH4PO46H2O) according to
the following reaction:

MgN H 4 P O4 6 H 2 O(s)
2++O H
++ M g
2+ N H 4
5 H 2 O+ HP O4

Eq.1

by addition of MgSO47H2O and NH3. The


precipitate attained is washed, dried, and
weighed.

Chem 31.1 Section, Room No., Time

To determine %P and %P2O5, the


constant weight of the precipitate and
calculations using gravimetric factors will be
used.
This experiment aimed to use
precipitation gravimetry with the use of an
analytical balance to quantitatively
determine the moisture in the crucible and
the content of phosphorus in the sample.

Materials and Methods


A. CONSTANT WEIGHING OF CRUCIBLES
AND
MOISTURE
CONTENT
DETERMINATION
Crucibles were used as containers for the
fertilizer samples. They were thoroughly
washed, dried, and left ajar in the oven
overnight at 110C to allow the excess
moisture to evaporate. After one laboratory
period, they were taken out of the oven and
placed inside a glass desiccator using
crucible tongs. The crucibles were left inside
the desiccator to cool for 15 minutes after
which they were weighed using an analytical
balance. They were then returned to the
oven and left to dry at 110C for 30 minutes
with their lids slightly ajar. After drying, they
were put inside the desiccator to cool for 15
minutes and then weighed again using an
analytical balance. This heating and cooling
process was repeated until a constant
weight was obtained.
A.1 ANALYSIS OF MOISTURE CONTENT
3.0 g of fertilizer was weighed to the
nearest 0.1mg inside the constant weight
crucible. The crucible along with the sample
was then put into the oven to dry at 110C
for 1 hour. The crucibles lid should be
slightly ajar during this initial drying. After
drying, the crucible was transferred into a
glass desiccator to cool for 15 minutes. The
crucible was then weighed using an
analytical balance and placed back into the
oven to dry for 30 minutes. This heating and
cooling process is repeated until a constant

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Organic Chemistry Laboratory

Formal Report

weight of
obtained.

the

crucible

and

sample

is

B. PREPARATION OF SOLUTIONS
500mL of 10%(w/v) MgSO47H2O:
50g of MgSO47H2O crystals (See
Appendix) was dissolved inside a 400mL
beaker. After complete dissolution, it was
quantitatively transferred into a 500mL
volumetric flask, filled to mark, and mixed
thoroughly by inverting the volumetric flask.
The solution was stored inside a clean
reagent bottle and labeled properly.
(3) 500mL solutions of 2M NH3:
67.58mL of 14.8M NH3 (See
Appendix) was pipetted out into a 500mL
volumetric flask already containing about
200mL distilled water. The solution was
diluted to mark and mixed thoroughly by
inverting the volumetric flask. It was then
transferred into a clean reagent bottle and
labeled properly. This was done thrice to
obtain a total of 1500mL of 2M NH3.
C. PRECIPITATION OF MgNH4PO46H2O
A filter paper that was to be used in
the latter part of the experiment was pre
weighed using an analytical balance and
placed inside the dessicator while not in use.
The sample inside the crucible in part A was
quantitatively transferred inside a 250 ml
beaker. 40 ml of distilled water was
measured in a graduated cylinder and added
to the 250 ml beaker to dissolve the sample.
The sample was then filtered in a beaker
using a funnel and a filter paper that was
not pre weighed to remove the impurities
and a clear colored filtrate was obtained. 45
ml of 10% MgSO47H2O was pipetted from
the 500 ml solution in B and this was added
to the filtrate. After the addition of
MgSO47H2O 150 ml of 2M NH3 was
added slowly to prevent nucleation and a
white precipitate was observed. Then, the
mixture was left for 15 minutes to allow it to
cool and precipitate completely at room
temperature. After 15 minutes, the
precipitate was filtered by using the pre
Chem 31.1 Section, Room No., Time

weighed filter paper then it was washed by:


1.) two portions of 5 ml distilled water and
2.) two 10 ml portions of 95% ethanol. The
filter paper was then placed in a watch glass
inside the locker for 1 day to let it dry and
for the ethanol to ignite and react with
excess NH3. On the next day, the filter
paper was heated inside the oven set at
110C for an hour. The filter paper was then
cooled for 15 minutes and then weighed
using an analytical balance.
Filter paper was fitted to a funnel and
weighed using an analytical balance. The
weighed filter paper was then kept inside a
glass desiccator until needed. The
constantly weighed fertilizer sample
obtained in Experiment 2 was then
qualitatively transferred into a 400mL
beaker. About 40mL of distilled water was
then used to dissolve the sample. After
crude dissolution, the solution was filtered
(not with the previously weighed filter
paper) and washed with distilled water until
a clear filtrate was obtained. About 45mL of
prepared 10%(w/v) MgSO47H2O was added
to the clear filtrate. 150mL of 2M NH3 was
then slowly added to the solution while
simultaneously stirring the solution. The
solution was then left to stand for 15
minutes in order for the precipitation
process to complete. The acquired
precipitate was qualitatively transferred to
the previously weighed filter paper. The
precipitate was then washed with two (2)
5mL portions of distilled water, adding the
portions of distilled water to the beaker that
contained the precipitate and then pouring it
onto the precipitate in order to transfer any
remaining precipitate inside the beaker onto
the filter paper. The precipitate was then
further washed with two (2) 10mL portions
of 95% ethanol by the same process. After
all the liquid had passed through the
precipitate, the filter paper was then opened
and spread out onto a watch glass and
allowed to dry inside the locker for one (1)
laboratory period. The filter paper was then
allowed to dry inside the oven at 110C for 1
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hour. After cooling for 15 minutes inside a
glass desiccator, it was then weighed using
an analytical balance.

Results and Discussion


A. Constant Weighing of Crucible and Sample

obtained from the groups are 1.2413%0.01% and


1.2570%0.01% respectively. This means that water
is a little bit greater than 1% of the composition of every
fertilizer sample, which is good for the consumers and
farmers.
B. Precipitation of MgNH4PO46H2O

Oven drying is done to remove moisture from the


crucible and fertilizer sample. Once moisture was
completely removed a constant weight was obtained,
which is needed for calculations. A pair of crucible
tongs was used when handling materials instead of
hands to avoid transfer of moisture from the skin. The
dried materials freshly removed from the oven were
placed in a desiccator. A desiccator contains a drying
agent and is airtight sealed to completely avoid moisture
uptake. The crucible must be first cooled at room
temperature before weighing due to its ceramic
composition. Materials like ceramic are sensitive to
temperature, which could expand or contract when
heated or cooled. All throughout the experiment the
same analytical balance was used to minimize the error
in weighing. To further minimize errors, constant
weighing was a must. This limited successive weights
obtained to agree within 0.3mg before recording final
weight.

The dried fertilizer sample was precipitated by the


addition of distilled water, 10% MgSO47H2O and
2M NH3. The NH3 solution was added slowly while
stirring to have a Q (concentration of species at any
instant) and high solubility. These are desired
conditions to have a lower Von Weimarn ratio. A
low Von Weimarn ratio means larger rate of particle
growth which leads to larger precipitate particles.
Large particle size is desired for easier filtration.
The solution was allowed to stand for ten minutes
for precipitation to complete. This treatment is
called
digestion,
which
promotes
slow
recrystallization and therefore causes larger particle
sizes. The precipitate was washed with distilled
water and ethanol during filtration to remove
impurities sticking with the precipitate. Once again,
the precipitate was oven dried to remove excess
The fertilizer sample was labeled 16N-20P-0K which moisture.
The %P over wet and dried samples and
means that a bag of fertilizer contains 16% nitrogen,
20% phosphate and 0% potash. This sample has enough %P2O5 was solved using the formula:
nutrient to produce MgNH4PO46H2O(s). Before drying
the sample, it was grinded to fine particles to make the
moisture easier to remove.

The %Moisture over wet sample was calculated by


dividing the mass of H2O, which was the moisture
removed from the sample, over the mass of wet sample
or as it was received. The same process is done for
%Moisture over dried samples, however mass of H 2O is
divided by mass of dried sample. The table below shows
the data obtained from all groups.
The data from all the groups both from the
%Moisture over wet and dried samples were suspected
outliers. These could have been caused by accidentally
touching the crucibles and spilling of fertilizer samples
during weighing. However, through the use of the
Grubbs test, all data were retained. The average
moisture over wet and over dried sample of all the data

Chem 31.1 Section, Room No., Time

%P=

mass of precipitateGravimetric factor


weight of wet /dried sample

where Gravimetric factor =


(moles of subtance sought )( AW )
( moles of precipitate ) ( MW )
The suspected values from the compiled
data of all groups were retained using Grubbs test.
However, compared to the theoretical value 20%
P2O5, the deviation of the data obtained is 36%.
This could have been caused by inaccurate
weighing of filter paper, improper addition of NH 3
and excess addition of water. Improper addition of
NH3 would cause production of smaller precipitate
sizes and excess water would cause more
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Organic Chemistry Laboratory

Formal Report
precipitate to form; both affect the weights
References
recorded.
[1] Hage, David S. and Carr, James D. 2011.

Conclusions and Recommendations


The %Moisture obtained from the experiment
and from other groups were all greater than 1%,
therefore enough water is available per fertilizer sample
which is a desirable composition. On the second part the
experiment a large percent error was obtained. Smaller
crucibles, larger tongs and different way of weighing
filter papers are recommended to avoid the occurrence
of a large error.

Chem 31.1 Section, Room No., Time

Analytical chemistry and quantitative analysis.


New Jersey: Pearson Prentice Hall.
[2] Skoog D., West D., Holler F., Crouch S.
Fundamentals of Analytical Chemistry, 9th ed.;
Brooks/Cole, Cengage Learning: CA, 2014,2004.
[3] Harris D. Quantitative Chemical Analysis, 7th Ed.;
WH Freeman and Company, 2007

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