Gravimetric Determination of Phosphorus in Fertilizer Samples

E.M.M. Medrano
Medrano,, J.M. Pasco
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
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

dissolved in 40 mL water. A different filter paper

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 100C 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

because phosphorus is one of the main
components of fertilizers.

Table 3.1 %P and %P2O5

4.5455% 0.0226%
%P
10.3918% 0.05167%
%P2O5
The phosphorus content of fertilizers is
expressed in percent phosphate. The sample used
has 20% P2O5. Compared to the results, there is a
relative error of 48%. This error may be attributed
to several factors like the forming of MgOH2 or
magnesium hydroxide. The formation of MgOH2
will cause less precipitate to be formed. The
constant stirring and slow addition of ammonia
aimed to lower the formation of magnesium
hydroxide. Another one is the acidity of the
solution. Since a change in acidity will affect the
amount of HPO42 , a solution that is too basic or
too acidic will cause less precipitate to be formed.
In precipitation gravimetric analysis, the first
step is to convert the analyte into a sparingly
soluble precipitate. [2] The phosphorus in the
sample was precipitated using water, ammonia
and magnesium ions as shown in the reaction
below:
2
4

5H 2O + HPO + NH
MgNH 4 PO4 6 H 2O (s)

+
4

2+

+ Mg + OH -->
(1)

Ammonium chloride, NH4Cl, may not be

used in place of ammonia, NH3, because it will
cause the formation of MgCl2 and the precipitate
will not be formed.
For 15 minutes, the solution was left to digest.
This step helped to improve the purity and
filterability of the precipitate. [3]
The precipitate was then washed with ethanol
which was polar in nature so that any polar
impurities would dissolve and be removed from
the precipitate.
CONCLUSION
The experiment showed that the actual
amount of phosphorus in fertilizers is lower than
the amount indicated in the package. This
illustrates how important it is to determine the

Through gravimetric analysis, the percent

phosphate was determined and compared against
the amount indicated on the package. The
experiment was able to fully use the concepts in
precipitation gravimetry.
REFERENCES
[1-2] Crouch, S.; Holler, F.; Skoog, D.; West, D.
Fundamentals of Analytic Chemistry, 8th
ed.; Harris: Canada, 2004; p. 336
[3] Crouch, S.; Holler, F.; Skoog, D.; West, D.
Fundamentals of Analytic Chemistry, 8th ed.;
Harris: Canada, 2004; p. 341
APPENDIX
1.1 Data
Trial
Sample weight
(as received), g*
Sample weight
(dried), g*
Weight of filter
paper, g
Weight of
air-dried filter
paper with
precipitate, g
Net weight of
dried
precipitate, g
Trial
Sample weight
(as received), g*
Sample weight
(dried), g*
Weight of filter
paper, g
Weight of
air-dried filter
paper with
precipitate, g
Net weight of
dried
precipitate, g

1
3.0
29
3.0
188
1.4
251

2
3.1
625
2.9
434
2.9
187

2.6
14

2.9
434
1.2
653

4
3.0
001
2.8
905
1.0
64

5
2.9
958
2.9
025
1.1
661

3.2
666

2.4
236

1.9
515

2.2
265

1.1
889

0.3
479

1.1
583

0.8
875

1.0
604

6
3.0
063
2.9
087
1.1
554

7
3.0
771
2.9
961
0.9
315

8
3.0
056
2.9
159
0.9
424

9
3.0
001
2.9
074
1.11
37

10
3.0
781
2.9
93
1.1
312

2.2
705

2.1
411

2.1
326

2.4
369

2.3
737

1.11
51

1.2
096

1.1
902

1.3
232

1.2
425

FM P2O5
1
m ppt
2 FM MgNH 4 PO4 6 H 2O

1.2 %P

mwetfert

%P was calculated in excel using the following

formulas:

m ppt
%P (dry)=

%P(wet)=

FM P

The results were as follows:

FM MgNH 4 PO4 6 H 2O

mdryfert
FM P
m ppt
FM MgNH 4 PO4 6 H 2O
mwetfert

100% (2)

100%

(3)

1
4.96
5198
4.98
1975
4.97
3586
0.01
1863
6
4.69
2151
4.84
9594
4.77
0873
0.111
329

Average
Standard
Deviation
Trial
%P (wet
basis)
%P (dry
basis)
Average
Standard
Deviation

2
1.39
16
1.49
5188
1.44
3394
0.07
3247
7
4.97
2682
5.10
7119
5.03
9901
0.09
5061

3
4.88
4165
4.97
8085
4.93
1125
0.06
6411
8
5.00
9326
5.16
3425
5.08
6375
0.10
8964

4
3.74
2167
3.88
406
3.81
3113
0.10
0333
9
5.57
9307
5.75
7199
5.66
8253
0.12
5788

5
4.47
7622
4.62
1554
4.54
9588
0.10
1775
10
5.10
6275
5.25
1462
5.17
8868
0.10
2663

1.3 %P2O5
%P 2O5was calculated in excel using the following
formulas:
%P2O5(dry)=

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

Trial
%P2O5
(wet basis)
%P2O5 (dry
basis)
Average

The results were as follows:

Trial
%P (wet
basis)
%P (dry
basis)

100% (4)

100% (4)

Standard
Deviation
Trial
%P2O5
(wet basis)
%P2O5 (dry
basis)
Average
Standard
Deviation

1
11.3
5127
11.3
8962
11.3
7044
0.02
712
6
10.7
2704
11.0
8698
10.9
0701
0.25
4516

2
3.18
1429
3.41
8247
3.29
9838
0.16
7456
7
11.3
6838
11.6
7572
11.5
2205
0.21
7326

3
11.1
6601
11.3
8073
11.2
7337
0.15
1827
8
11.4
5215
11.8
0445
11.6
283
0.24
911

4
8.55
5215
8.87
9606
8.71
741
0.22
9379
9
12.7
5522
13.1
6191
12.9
5857
0.28
7573

5
10.2
3659
10.5
6564
10.4
0111
0.23
2675
10
11.6
7379
12.0
0571
11.8
3975
0.23
4704