Gravimetric Determination of Phosphorus in Fertilizer Samples

Medrano,, J.M. Pasco

E.M.M. Medrano
Department of Mining, Metallurgical and Materials Engineering, College of Engineering
University of the Philippines, Diliman, Quezon City, Philippines
Date Due: 7 January 2014
Date Submitted: 7 January 2014

Abstract

Concepts in precipitation gravimetry were applied in this experiment.

Phosphorus from fertilizer samples was dissolved in water, ammonia and
magnesium sulfate heptahydrate solution. A white precipitate, magnesium
ammonium phosphate hexahydrate, was formed. The solid contained the
phosphorus from the fertilizer sample. It was weighed and then results
compared to the amount of phosphorus indicated in the package. The
outcome showed that fertilizers actually have lower phosphorus content than
indicated in the package.

Keywords: gravimetric analysis, digestion, phosphorus, precipitate, ethanol, stirring

INTRODUCTION dissolved in 40 mL water. A different filter paper

Phosphorus is one of the main components in
fertilizers. To determine how much phosphorus is
present in a fertilizer sample, gravimetric analysis
through precipitation of magnesium ammonium
phosphate hexahydrate, MgNH4PO4 • 6H2O, was
used.
Gravimetric analysis through precipitation
works with soluble analyte.[1] In this experiment,
soluble phosphorus was the analyte which was
precipitated and measured.
This experiment aimed to demonstrate proper
gravimetric steps in order to quantitatively
determine the amount of phosphorus in fertilizers.
METHODOLOGY
Filter paper was weighed then kept in the
desiccator prior to use in the latter part of the
experiment.
Powdered fertilizer weighing 3.0056 grams
when wet and 2.9159 grams after drying was
was used to filter the mixture. 45 mL of 10%
MgSO4 • 7H2O was then added to the filtrate.
Then, 150 mL of 2M NH3 was slowly added while
stirring. White precipitate was formed.
The mixture was then allowed to stand at
room temperature for 15 minutes. The precipitate
was then quantitatively transferred to the
pre-weighed filter paper then washed with two (2)
5 mL portions of distilled water. Two (2) 10 mL
portions of 95% ethanol was used to wash the
precipitate. The filter paper was then spread on a
watch glass and stored in the locker until the next
laboratory period.
The filter paper with precipitate was then
dried in the oven at 100°C for 1 hour. It was then
cooled for 15 minutes and then weighed. Results
were tabulated.
RESULTS AND DISCUSSION
The amount of phosphorus was quantitatively
determined. The results pooled from 10 trials were
as follows:
 amount of phosphorus in fertilizers especially
Table 3.1 %P and %P2O5 because phosphorus is one of the main
%P 4.5455% ± 0.0226% components of fertilizers.
%P2O5 10.3918% ± 0.05167%
Through gravimetric analysis, the percent
The phosphorus content of fertilizers is phosphate was determined and compared against
expressed in percent phosphate. The sample used the amount indicated on the package. The
has 20% P2O5. Compared to the results, there is a experiment was able to fully use the concepts in
relative error of 48%. This error may be attributed precipitation gravimetry.
to several factors like the forming of MgOH2 or
magnesium hydroxide. The formation of MgOH2 REFERENCES
will cause less precipitate to be formed. The
constant stirring and slow addition of ammonia [1-2] Crouch, S.; Holler, F.; Skoog, D.; West, D.
aimed to lower the formation of magnesium Fundamentals of Analytic Chemistry, 8th
hydroxide. Another one is the acidity of the ed.; Harris: Canada, 2004; p. 336
solution. Since a change in acidity will affect the
amount of HPO42− , a solution that is too basic or [3] Crouch, S.; Holler, F.; Skoog, D.; West, D.
Fundamentals of Analytic Chemistry, 8th ed.;
too acidic will cause less precipitate to be formed.
Harris: Canada, 2004; p. 341
In precipitation gravimetric analysis, the first
APPENDIX
step is to convert the analyte into a sparingly
soluble precipitate. [2] The phosphorus in the
1.1 Data
sample was precipitated using water, ammonia
and magnesium ions as shown in the reaction
Trial 1 2 3 4 5
below:
Sample weight 3.0 3.1 3.0 2.9
3
2− +
(as received), g* 29 625 001 958
2+ -
5H 2O + HPO + NH 4 4 + Mg + OH --> Sample weight 3.0 2.9 2.9 2.8 2.9
MgNH 4 PO4 • 6 H 2O (s) (1) (dried), g* 188 434 434 905 025
Weight of filter 1.4 2.9 1.2 1.0 1.1
paper, g 251 187 653 64 661
Ammonium chloride, NH4Cl, may not be Weight of
used in place of ammonia, NH3, because it will air-dried filter 2.6 3.2 2.4 1.9 2.2
cause the formation of MgCl2 and the precipitate paper with 14 666 236 515 265
will not be formed. precipitate, g
Net weight of
1.1 0.3 1.1 0.8 1.0
For 15 minutes, the solution was left to digest. dried
889 479 583 875 604
This step helped to improve the purity and precipitate, g
filterability of the precipitate. [3] Trial 6 7 8 9 10
Sample weight 3.0 3.0 3.0 3.0 3.0
The precipitate was then washed with ethanol (as received), g* 063 771 056 001 781
which was polar in nature so that any polar Sample weight 2.9 2.9 2.9 2.9 2.9
impurities would dissolve and be removed from (dried), g* 087 961 159 074 93
the precipitate. Weight of filter 1.1 0.9 0.9 1.11 1.1
paper, g 554 315 424 37 312
Weight of
CONCLUSION
air-dried filter 2.2 2.1 2.1 2.4 2.3
paper with 705 411 326 369 737
The experiment showed that the actual precipitate, g
amount of phosphorus in fertilizers is lower than Net weight of
the amount indicated in the package. This 1.11 1.2 1.1 1.3 1.2
dried
illustrates how important it is to determine the 51 096 902 232 425
precipitate, g
 1 FM P2O5
1.2 %P m ppt × ×
2 FM MgNH 4 PO4 •6 H 2O
× 100% (4)
%P was calculated in excel using the following mwetfert
formulas:
FM P The results were as follows:
m ppt ×
FM MgNH 4 PO4 •6 H 2O
%P (dry)= × 100% (2) Trial 1 2 3 4 5
mdryfert
%P2O5 11.3 3.18 11.1 8.55 10.2
FM P (wet basis) 5127 1429 6601 5215 3659
m ppt ×
FM MgNH 4 PO4 •6 H 2O %P2O5 (dry 11.3 3.41 11.3 8.87 10.5
%P(wet)= × 100% (3) basis) 8962 8247 8073 9606 6564
mwetfert 11.3 3.29 11.2 8.71 10.4
Average
The results were as follows: 7044 9838 7337 741 0111
Standard 0.02 0.16 0.15 0.22 0.23
Trial 1 2 3 4 5 Deviation 712 7456 1827 9379 2675
%P (wet 4.96 1.39 4.88 3.74 4.47 Trial 6 7 8 9 10
basis) 5198 16 4165 2167 7622 %P2O5 10.7 11.3 11.4 12.7 11.6
%P (dry 4.98 1.49 4.97 3.88 4.62 (wet basis) 2704 6838 5215 5522 7379
basis) 1975 5188 8085 406 1554 %P2O5 (dry 11.0 11.6 11.8 13.1 12.0
4.97 1.44 4.93 3.81 4.54 basis) 8698 7572 0445 6191 0571
Average
3586 3394 1125 3113 9588 10.9 11.5 11.6 12.9 11.8
Average
Standard 0.01 0.07 0.06 0.10 0.10 0701 2205 283 5857 3975
Deviation 1863 3247 6411 0333 1775 Standard 0.25 0.21 0.24 0.28 0.23
Trial 6 7 8 9 10 Deviation 4516 7326 911 7573 4704
%P (wet 4.69 4.97 5.00 5.57 5.10
basis) 2151 2682 9326 9307 6275
%P (dry 4.84 5.10 5.16 5.75 5.25
basis) 9594 7119 3425 7199 1462
4.77 5.03 5.08 5.66 5.17
Average
0873 9901 6375 8253 8868
Standard 0.111 0.09 0.10 0.12 0.10
Deviation 329 5061 8964 5788 2663

1.3 %P2O5

%P 2O5was calculated in excel using the following

formulas:

%P2O5(dry)=

1 FM P2O5
m ppt × ×
2 FM MgNH 4 PO4 •6 H 2O
× 100% (4)
mdryfert
%P2O5(wet)=