Quantitative Inorganic Analysis Laboratory

Formal Report
Date Performed: 18
August 2015
Date Submitted: 24
September
2015
Institution/Department:
Department of
Mining, Metallurgical and
Materials Engineering
College: Engineering
Instructor: Searle
Aichelle Duay

Gravimetric Determination of Moisture and

Phosphorus in Fertilizer Samples
Z. C. Hachero
The purpose of the experiment was to do a quantitative determination of percent
moisture and phosphorus in fertilizer samples using gravimetric method of analysis. A
fertilizer sample placed in a crucible was dried in an oven and was weighed until a
constant weight was obtained. Phosphorus in the fertilizer was precipitated as
magnesium ammonium phosphate hexahydrate to calculate the percentage
phosphorus and percentage diphosphorus pentoxide. The calculated %moisture of the
fertilizer sample was 1.69 0.01%. The obtained %P and %P2O5 in dry basis were
4.707% 0.001% and 10.786% 0.003 % respectively. The obtained values of %P2O5 was less than the theoretical value of 20%, yielding a 47.13% error. The values
obtained were within the range of accepted values in the market so we can say that
the method used was effective in determining the amounts of different species in a
substance.

Gravimetric Determination of Moisture and Phosphorus in Fertilizer Samples

Hachero, 2015 | 1

Introduction
Fertilizer quality is notified in terms of physical and
chemical characteristics. The physical parameters
include moisture content and particle size while the
chemical parameters refer to the amount and form of
nutrients. The main objective in analysing fertilizers is
to assess their quality. The quality of fertilizers is stated
by the manufacturers and, in most countries, it is
statutorily notified. Content determination is necessary
for quality issues and control, as well as legal and
labeling requirements.
Gravimetry includes all methods wherein the use of
mass or a change in mass is used to analyze
species.There are two types of gravimetric analysis. One
is the direct method where the analyte is directly
weighed. The other is indirect analysis where the
analyte is removed and the change in mass of the whole
thing is used to analyze the analyte. For the first part of
this experiment, we are going to use an indirect method
of gravimetric analysis.
Since fertilizers are soluble in water making it easy for
plants to absorb nutrients through their roots a
precipitant is to be used to precipitate phosphorus, P, in
the form of magnesium ammonium phosphate
hexahydrate, MgNHPO6HO, as shown in the
chemical equation
5H2O(l) + HPO42-(aq) + NH4+(aq) +
Mg2+(aq)+OH-(aq) MgNH4PO46H2O(s)

(1)

understand the principles and importance of constant

weighing along with the relation of the experiment to
analyte separation by precipitation.

Materials and Methods

The experiment had three main parts: the constant
weighing of the crucible, the analysis of moisture in the
fertilizer sample, and the determination of phosphorus
content.
For the first part of the experiment, a crucible with
its cover was prepared and heated by placing it in an
oven set at 110C. The crucible was then transferred
into a desiccator and was allowed to cool for fifteen
minutes. It was then weighed in an analytical balance
through weighing by difference. After weighing, the
crucible was transferred back to the same oven and
heated for 30 minutes and after, again underwent the
cooling process by being transferred into the dessicator.
It was then weighed, and the process of heating and
cooling was repeated until a constant weight was
obtained.
The second part of the experiment was for the
determination of moisture content in the fertilizer
sample. A sample of the fertilizer was then transferred
into the constantly weighed crucible until the net weight
of the sample has reached 3 g. The crucible along with
the sample is heated in an oven at 110 C for one hour.
The cover of the crucible was slightly ajar to allow the
escape of vapor. The same cycle of heating and cooling
was used until a constant weight was obtained.

The phosphorus content in the fertilizer sample was

determined quantitatively using gravimetric methods. A
filter paper was prepared and weighed, then kept in the
desiccator while not in use. The dried fertilizer sample
was quantitatively transferred in a 250-mL beaker and
40 mL of distilled water was added to dissolve the
FW P
weig h t ppt
sample. The mixture was filtered using a different filter
FW MgNH 4 PO 4 6 H 2 O
P=
100 paper than that of previously weighed, until a clear filter
weig h t sample
was obtained. To the filtrate , 45 mL of 10% MgSO 47
(2)
H2O was added and then 150 mL of 2 M NH 3 was
;and,
slowly added, with the 1 st 50 mL being added dropwise,
while stirring. The mixture was allowed to stand at
FW P2 O5
weig h t ppt
FW MgNH 4 PO 4 6 H 2 O room temperature for 15 minutes to complete the
precipitation process. The precipitate was transferred to
P 2 O 5=
100
weig h t sample
the pre-weighed filter paper and was washed with two 5
(3)
mL portions of distilled water and then with two 10 mL
portions of 95% ethanol. The filter paper with the
The objective of the experiment is to quantitatively precipitate was placed on a watch glass and stored in the
determine the percent moisture and in fertilizer locker. In the next laboratory period, the filter paper
samples through constant weighing using gravimetric with the precipitate was placed in an oven set at 110C
method of analysis. Also, this experiment is done to
Then, from the weight of the precipitate, which is
MgNHPO6HO, the percentage or phosphorus, P,
and phosphorus pentoxide, P2O5, can be calculated by
using the equation:

Organic Chemistry Laboratory

Formal Report

for 1 hour. Then it was cooled for 15 minutes inside a

desiccator and was weighed.

Results and Discussion

The objective of the experiment was to do a
quantitative determination of moisture and phosphorus
content in fertilizer samples through the use of
gravimetric methods of analysis.
In the first part of the experiment, a crucible with
cover was oven dried and weighed repeatedly until a
constant weight was obtained to ensure that water
present in the crucible will all evaporate as it may affect
the weight of the sample later on the experiment. The
crucible had a constant weight of 35.5007 0.0002 g. A
constant weight was obtained when the difference
between two consecutive weights are between 0.0002 to
0.0003 g. A difference of 0.0003 g between weights is
considered constant based on the calculation of
uncertainties and error propagation of the analytical
balance. Shown below is the calculation:
2

0.0002
0.000 2 2+ = 0.0003 g

(4)

In the process of constant weighing, the crucibles

and samples were cooled to room temperature before
weighing as not to create convection currents that give
false weight. [3] It was also cooled in a desiccator which
maintained the moisture content in the samples.
A fertilizer sample weighing 3.0059 0.0002 g was
placed in the constantly weighed crucible. The sample
was grounded into fine powder to increase the surface
area, which will allow more moisture particles to escape
from the sample and to hasten the drying process.
The constant weight of the crucible with sample is
38.4476 0.0002 g. Moisture determination in fertilizer
samples is important, and a low percentage of moisture
content is ideal because excess moisture in fertilizer will
result in clumping.
The cycle of heating, cooling and weighing,
increases the accuracy of the measurement and
decreases the chances of errors due to the presence of
moisture in the sample. Samples usually often contain

Chem 31.1 Section, Room No., Time

water that is in equilibrium with the atmosphere and

therefore the composition of the sample is dependent on
the relative humidity and ambient temperature at the
time and place of the analysis or measurement, thus
increasing its weight. [2] The values obtained for
moisture determination are listed in Table 1.
Table I. Reported Values for Moisture Determination
Constant Weight of
38.4476 0.0002 g
Crucible+Sample
Constant Weight of
35.5007 0.0002 g
Empty Crucible
Net Weight of Dried
2.9496 0.0003 g
Sample
Weight of Wet Sample
3.0059 0.0002 g
Mass of Water
0.0590 0.0004 g
% Moisture
1.96 % 0.01%
The net weight of dried sample and the mass of
water in the sample were 2.9496 0.0003 g and 0.1423
0.0004 g, respectively. The calculated % moisture in
the fertilizer sample was determined to be 4.74%
0.01%. Different methods for moisture determination
besides oven drying include the direct method of
moisture determination and Karl Fischer titration
method. The direct method uses the moisture balance
and provides faster and more accurate measurement of
moisture using loss on drying method while the Karl
Fischer titration method uses a chemical reaction in
determining the moisture and water content of the
sample. [1]
In the third part of the experiment, the phosphorus
content in the fertilizer sample was determined
quantitatively using gravimetric methods. In this
experiment, the phosphorus in the fertilizer sample was
separated by precipitating it as MgNH4PO46H2O, a
white and stable insoluble compound. The precipitate
forms only upon the slow neutralization of the solution
with NH3. To make sure that the formed precipitate will
be easier to filter, digestion was done. This allowed the
fine particles of the precipitate to settle at the bottom of
the beaker and form particles which are slightly larger,
due to the adsorption of a particle with the other
particles, for easier filtration. In an acid solution the
phosphate ions react with hydronium ions to form
monohydrogen phosphate ions. The net effect of this is
to reduce the concentration of the phosphate ions (PO43-)
and prevent the formation of MgNH4PO46H2O. The
hydroxide ions necessary for the neutralization must be
supplied by a weak base such as ammonium. A strong
base, like NaOH, would cause the precipitation of

Authors Surname, 2015| Page Number

Mg(OH)2 instead of the double salt magnesium

ammonium phosphate hexahydrate. The hydroxide ions
necessary for the neutralization must be supplied by a
weak base such as ammonium hydroxide. A strong base,
like NaOH, would cause the precipitation of Mg(OH)2
instead of the double salt magnesium ammonium
phosphate hexahydrate. NH4Cl was not used because it
can interfere with the production of phosphorus since
Cl- might react with Mg2+ which will form MgCl 2 and
may produce a different precipitate.
To satisfy the precipitate requirement for gravimetry,
which is to have bigger particles for easier precipitation,
the NH3 was added slowly while the solution is
continuously stirred allowing particle growth to be
favoured rather than nucleation as pointed out by the
Von Weimarns Relative Supersaturation Ratio.
The precipitate was washed with water and 95%
ethanol, which is sufficiently volatile to be easily
removed when being dried and to remove all residual
traces of inert ions included in the supernatant, without
dissolving any of the precipitate. The ethanol is
dissolved when the precipitate is placed in the oven.
The net weight of dried precipitate was 0.8187 0.0003
g. From the wet and dry weight of the fertililzer sample,
the %P and % P2O5 can be calculated The values
obtained were tabulated in Table II.
Table II. Reported Values for Phosphorus Content
Determination
%P (wet basis)
3.444% 0.001%
%P (dry basis)
3.612% 0.001%
%P2O5 (wet basis)
7.891% 0.003 %
%P2O5 (dry basis)
8.276% 0.003%
Possible sources of error for the experiment include
the rate of addition of NH 3, if the NH3 was added faster,
the rate of nucleation will also increase and thus more
particles will be produced, but smaller. Some of these
particles might pass through the filter and result in
decreased phosphorus content. If the temperature when
the experiment was done was too low, the rate of
particle growth will increase and will also result in less
phosphorus content.
Human error like touching the
crucible or the filter paper, can also alter the results of
the experiment.
Conclusions and Recommendations
The percent moisture that was calculated is
1.9600% which was within the range of accepted values
in the market. The theoretical value of %P2O5 is 20% of
the fertilizer sample, which is significantly different

from the experimental value of 10.574%. The

experiment yielded a 47.13% error for the %P 2O5. This
is a high value for an error and thus, theoretically, the
experiment is an error, but compared to the data of the
other groups, the %P and %P 2O5 values are close to
each other yielding a standard deviation of 2.638865.
This data suggests that the actual values are close to the
data recorded and that the experiment is a success. The
range of the accepted values for the phosphorus and
phosphate content is very large since the amount of
phosphorus and phosphate in the fertilizer will highly
depend on the other chemicals found in the fertilizer and
on the type of plants that the fertilizer will be put to.
The method was carried out properly and all sources of
errors were minimized as much as possible. No gross
errors were committed. It is recommended that other
ways of moisture determination be used, and compared
to the oven drying method, to know which method is
much more efficient.

References
[1] International Fertilizer Industry Association.
Determination of Moisture of Fertilizers. 2014
http://fertilizer.org/ (accessed Sept. 20, 2015)

[2] Caro, J., & Hill, W. (1956). Fertilizer Characteristics,

Characteristics and Fertilizer Value of Phosphate
Rock from Different Fields. Journal of Agricultural
and Food Chemistry, 684-687.
[3] Skoog, D., West, D., Holler, F.J., Crouch, S., Chen,
S. Introduction to Analytical Chemistry 8th ed.
Cengage Learning, Singapore. 2012.
[4] Harris, D. Quantitative Chemical Analysis 8th ed.
W.H. Freeman and Company, New York. 2010.
[5] Higson, S. (2004). Analytical chemistry. Oxford:
Oxford University Press.
[6] Morse, D., & Baer, D. (2004). Laboratory Balances:
How
They
Work,
Checking
Their
Accuracy. Laboratory Medicine, 48-51

Organic Chemistry Laboratory

Formal Report

Chem 31.1 Section, Room No., Time

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