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METHODOLOGY

Preparation of crucibles
One crucible and one cover
were washed, cleaned and labelled
prior to weighing. Masking tape and
paper labels were not used for
labelling as these will easily integrate
inside the oven. To avoid this, the
crucible and cover were marked by a
pencil instead. These were then
placed inside the oven set at 110C
for one week with the cover slightly
ajar.

Constant weighing of crucibles


The crucible and cover were
transferred into a desiccator using a
pair of tongs. After cooling for 15
minutes, the crucible with cover was
weighed in an analytical balance. It
was noted to always use the crucible
tongs when handling the crucible and
the cover. The use of bare hands will
just add moisture to the container
that may cause certain errors in the
constant weighing process. The
crucible with its cover slightly ajar
was returned to the oven set at 110C
for 30 minutes to dry. Weighing was
done again after cooling the crucible
and cover for 15 minutes in a
desiccator. These heating and cooling
processes were repeated until a
constant weight, two successive
weighings with a difference of 0.0002
g to 0.0003 g, was obtained.

Moisture analysis
About 3.0 g (to the nearest 0.1
mg) of the fertilizer sample was
weighed into the constantly weighed
crucible and cover through weighing
by difference. After recording the
weight reading, the crucible with
sample and cover (slightly ajar) was
placed in the oven set at 110C to dry
for 1 hour. It was then transferred to a
desiccator to cool for 15 minutes. It
was noted that the cooling time used
in obtaining the constant weight of
the empty crucible, which is 15
minutes, should be the same with the
cooling time in obtaining the constant
weight of the crucible with sample.
The weight of crucible with cover and
sample was taken and recorded. It
was then returned to the oven set at
110C to heat for 30 minutes. These
heating and cooling processes were
repeated until a constant weight was
obtained.

Preparation of solutions
Prior to the experiment proper,
500 mL of 10% (w/v) MgSO 47H2O
solution and three 500 mL of 2 M
NH3 solution was prepared.

Precipitation of MgNH4PO46H2O
After recording the wet and dry
weights of the fertilizer sample used
for moisture determination, the dried
sample was quantitatively transferred
into a clean and dry 250-mL beaker.
40 mL of distilled water was added
and the resulting mixture was

constantly stirred to dissolve the


sample. If the sample does not
dissolve completely, the mixture
should be filtered such that a clear
filtrate will be obtained. 45 mL of 10%
MgSO47H2O solution was added to
the filtrate. While stirring, 150 mL of
2 M NH3 was slowly added. The
mixture was allowed to stand at room
temperature for 15 minutes to
complete the precipitation process.
The
precipitate
was
then

quantitatively transferred to the preweighed filter paper and washed with


two 5 mL portions of distilled water
followed by two 10 mL portions of
95% ethanol. The filter paper was
spread on a watch glass and stored in
the locker for two nights. After air
drying,
the
filter
paper
with
precipitate was placed in the oven set
at 110C for 1 hour. It was then
cooled inside a desiccator for 15
minutes and weighed afterwards.

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