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Lab Book # 28.13

Name: Richelle Lani L. Taruc

Co-Worker: Erma Marie M. Selga

Date Due: August 20, 2002

Date Submitted: August 20, 2002

DETERMINATION OF PHOSPHORUS IN PLANT FOOD AND SIMILAR

SAMPLES Gravimetric Method (MgNH4PO46H2O Precipitation)
Abstract
The experiment was done to determine the phosphorus content of the plant food samples
using the precipitation gravimetric method. Gravimetric analysis involves the separation of the
analyte from the sample to obtain a pure precipitate of MgNH 4PO46H2O, which was of known
composition. The weight of the precipitate was related to the weight of the phosphorus by the
gravimetric factor. The percentage phosphorus was then determined by gravimetric calculations.
The level of phosphorus can be reported as 5.6459% P 0.0008% P and 12.937% P 2O5 0.002%
P2O5, based on the as received weights and 5.9609% P 0.0009% P and 13.659% P 2O5 0.002%
P2O5, based on the dried weights.

Introduction
Plant foods or fertilizers contain nutrients like nitrogen, phosphorus and potassium. They
are essential nutrients that are usually lacking or present in small amounts in soils. The amounts
of these nutrients are expressed in percentages. Nitrogen is expressed as % nitrogen; phosphorus
as % diphosphorus pentoxide (P2O5); and potassium as % potassium oxide (K 2O). The
composition of soil is expressed by a set of three numbers pertaining to % nitrogen, %
phosphorus and % potassium. The plant foods also contain other counter-ions and dyes. It is
important to determine the actual amount of nutrients present in plant foods to ensure good
quality for consumers.
Determination of these nutrients does not require very accurate results, so the fast and
inexpensive gravimetric method can be used. Gravimetric method is based upon determining the
mass of a pure compound to which the analyte is chemically related. In this experiment, only
one of the nutrients was determined, which is phosphorus. The prepared dried sample was
dissolved in water and an insoluble form of phosphorus, magnesium ammonium phosphate
hexahydrate was precipitated by adding ammonia and magnesium sulfate hexahydrate. The
precipitation followed the reaction:
5H2O(l) + HPO42-(aq) + NH4+(aq) + Mg2+(aq) + OH- MgNH4PO46H2O(s)
The white precipitate obtained was washed and air-dried and was then weighed. The weight of
the precipitate can then be related to the weight of P and P2O5 in the sample by a gravimetric
factor. The gravimetric factor is a constant composed of two conversion factors (from weight of
precipitate to number of moles of the precipitate and from the number of moles of precipitate to
the weight of the analyte) and the stoichiometric ratio between the precipitate and the analyte.
The formula for the gravimetric factor is:
GF = a FWsought/analyte
b FWweighed ppt

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Lab Book # 28.13

The percentage phosphorus and percentage diphosphorus pentoxide can be expressed based on
the as received weight and the dry weight. The percentage analyte was computed by:
% analyte = (weight of ppt)(GF) x 100%
weight of sample
The purpose of the experiment was to determine the level of phosphorus in plant food
samples using the gravimetric method.

Data and Results

SAMPLE CALCULATIONS
Net Weight of Dried Precipitate
weight of dried ppt = weight of air-dried filter paper w/ ppt weight of ppt
For Trial 1:
weight of dried ppt = (2.0936 0.0002 g) (0.5038 0.0002 g)
= 1.5898 w
w = (0.0002)2 + (0.0002)2 = 0.0003
weight of dried ppt = 1.5898 0.0003 g
Gravimetric Factors
GF for P = 1
FW of P
1 FW of MgNH4PO46H2O
GF for P2O5 = 1
FW of P2O5
2 FW of MgNH4PO46H2O
Percent Analyte
% analyte = (weight of ppt)(GF) x 100%
weight of sample
For Trial 1:
%Pas received basis = (1.5898 0.0003 g)(1)(30.9738 g/mol) x 100%
(3.5000 0.0002 g)(1)(245.407 g/mol)
= 5.7330% %Pas received basis
%Pas received basis = 5.7330%
0.0003 2 + 0.0002 2 = 0.0011%
1.5898
3.5000
%Pas received basis = 5.7330% 0.0011% P

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%Pdry basis = (1.5898 0.0003 g)(1)(30.9738 g/mol) x 100%
(3.2963 0.0003 g)(1)(245.407 g/mol)
= 6.0873% %Pdry basis
%Pdry basis = 6.0873%
0.0003 2 + 0.0002
1.5898
3.2963

Lab Book # 28.13

= 0.0013%

%Pdry basis = 6.0873% 0.0013% P

%P2O5 as received basis = (1.5898 0.0003 g)(1)(141.9446 g/mol) x 100%
(3.5000 0.0002 g)(2)(245.407 g/mol)
= 13.136% %P2O5 as received basis
%P2O5 as received basis = 13.136%
0.0003 2 + 0.0002 2
1.5898
3.5000

= 0.003%

%P2O5 as received basis = 13.136% 0.003% P2O5

%P2O5 dry basis = (1.5898 0.0003 g)(1)(141.9446 g/mol) x 100%
(3.2963 0.0003 g)(2)(245.407 g/mol)
= 13.948% %P2O5 dry basis
%P2O5 dry basis = 13.948%
0.0003 2 + 0.0003
1.5898
3.2963
%P2O5 dry basis = 13.948% 0.003% P2O5
Average
Average %Pas received basis
X = Xi = (5.7330% 0.0011%) + (5.5588% 0.0011%)
n
2
= 11.2918% S
2
S = (0.0011)2 + (0.0011)2 = 0.0016%
= 11.2918% 0.0016%
2
= 5.6459% X
X = 5.6459% 0.0016 2 = 0.0008%
11.2918
Average = 5.6459% 0.0008% P
Average %Pdry basis
X = Xi = (6.0873% 0.0013%) + (5.8345% 0.0013%)
n
2
= 11.9218% S
2
S = (0.0013)2 + (0.0013)2 = 0.0018%

= 0.003%

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= 11.9218% 0.0018%
2
= 5.9609% X
X = 5.9609% 0.0019
11.9218

Lab Book # 28.13

= 0.0009%

Average = 5.9609% 0.0009% P

Average %P2O5 as received basis
X = Xi = (13.136% 0.0003%) + (12.737% 0.0003%)
n
2
= 25.873% S
2
S = (0.0003)2 + (0.0003)2 = 0.004%
= 25.873% 0.004%
2
= 12.937% X
X = 12.937% 0.004 2 = 0.002%
25.873
Average = 12.937% 0.002% P2O5
Average %P2O 5dry basis
X = Xi = (13.948% 0.0003%) + (13.369% 0.0003%)
n
2
= 27.317% S
2
S = (0.0003)2 + (0.0003)2 = 0.004%
= 27.317% 0.004%
2
= 13.659% X
X = 13.659% 0.004 2 = 0.002%
25.873
Average = 13.659% 0.002% P2O5

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Lab Book # 28.13

DATA
Table 1. Percent Phosphorus in Plant Food
Trial

1
2

Weight
of
Sample,
g (as
received
)
3.5000
0.0002
3.5000
0.0002

Weight
of
Sample,
g (dried)

Weight
of Filter
Paper, g

3.2963
0.0003
3.3346
0.0003

0.5038
0.0002
0.4420
0.0002

Constant
Weight
of Filter
Paper +
Sample,
g
2.0936
0.0002
1.9835
0.0002

Constant
Weight
of
Sample,
g

% P (as
received/
wet basis)

1.5898
0.0003
1.5415
0.0003

5.7330
0.0011
5.5588
0.0011

Average

5.6459
0.0008

% P (dry
basis)
6.0873
0.0013
5.8345
0.0013
5.9609

0.0009

% P2O5 (as
received/
wet basis)

% P2O5
(dry
basis)

13.136
0.003
12.737
0.003

13.948
0.003
13.369
0.003

12.937
0.002

13.659
0.002

Discussion
There are two types of gravimetric analysis, the precipitation method and the
volatilization method. In this experiment, the precipitation method was implemented to
determine phosphorus in the plant food samples. The samples were prepared first by oven
drying to remove moisture and by determination of its moisture content. This was done in the
previous experiment (Experiment 2: Moisture determination of plant food samples Constant
weighing). The weights of the dried samples were obtained also from the previous experiment.
The prepared dried samples were then dissolved in distilled water since the analyte
phosphorus is soluble in water. Undissolved solids were removed by filtration. The filtrate was
then treated with solutions of MgSO 47H2O and NH3, which were the precipitating agents. The
formation of the white precipitate MgNH4PO46H2O separates the analyte phosphorus from the
other substances dissolved in the filtrate of the sample. The precipitation reaction was:
5H2O(l) + HPO42-(aq) + NH4+(aq) + Mg2+(aq) + OH- MgNH4PO46H2O(s)
The precipitating agents should precipitate the analyte completely and quantitatively and
should react specifically or selectively with the analyte. Other substances should not react with
the precipitating agent so that the analyte is completely separated from the other constituents of
the sample. Substances that will react with the precipitating agents are called interferences.
Reaction of these interferences with the precipitating agents should be prevented by removal or
by adding masking reagents to convert them to other forms that are unreactive with the
precipitating agents.
The precipitate must be filterable and free of contaminants. It should be non-volatile to
prevent decomposition when it is exposed to the atmosphere. It should have a low solubility to
have a complete precipitation and to avoid loss of precipitate during filtration and washing. The
precipitate must be of known composition and of high purity after air-drying.
After the addition of the precipitating agents, the sample was allowed to stand for about
15 minutes for the precipitation to be complete. To improve filterability other gravimetric
analysis include the process of digestion, wherein the precipitate is heated for an hour or more
from the solution it was formed or the mother liquor.

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Lab Book # 28.13

The precipitate was then filtered and washed to remove impurities. Water was used in the
first few washings, then 95% ethanol was then used to remove polar substances. After the
filtration and washing, the precipitate was allowed to dry. The weight of the air-dried precipitate
was obtained.
The weight of the precipitate was related to the weight of the phosphorus by the
gravimetric factor. The percentage phosphorus and percentage diphosphorus pentoxide based on
the as received weight and the dry weight were determined through gravimetric calculations.
The values obtained for the as received or wet basis were: 5.6459% P 0.0008% P and 12.937%
P2O5 0.002% P2O5. The dry basis values were: 5.9609% P 0.0009% P and 13.659% P 2O5
0.002% P2O5.
The results of the two trials were precise and it can be seen from the correlation plots that
the dry basis data of the group were close to the class means, 6.1461% P dry and 14.083% P2O5dry
which means that the data is accurate. Q-test was done for the data of Group 5 (which had the
highest value) and Group 9 (which had the lowest value) and both values were accepted. The
relative standard error was 5.89%, which means that the class had precise results.
There were several possible sources of error that made the data inaccurate. The
undissolved plant food samples, which were discarded, might contain phosphorus. It is also
possible that some of the analyte was lost when the precipitate was filtered and washed. Some of
the precipitate particles may be unfilterable. Air-drying might not be enough to remove moisture
from the precipitate. Errors from Experiment 2 could also contribute to errors in this experiment
since the sample used was prepared during the previous one.

Summary and Conclusions

The phosphorus content of the plant food samples were determined to be 13.659% P 2O5
0.002% P2O5 based on the dry weights of the samples. The method used was gravimetric
analysis, where the analyte was separated from the sample to obtain a pure precipitate of
MgNH4PO46H2O, which was of known composition. The percentage phosphorus was
determined by gravimetric calculations.
To obtain accurate results, each step should be followed carefully, specially the slow
addition of the reagents to obtain filterable crystalline precipitate. It is important to obtain
filterable precipitate to prevent loss of the analyte. Proper filtration technique should also be
implemented. The precipitate should be completely dried before weighing to minimize errors.

Reference
Skoog, West, Holler. 1996. Fundamentals of Analytical Chemistry. 7/e. USA. Saunders College
Publishing.

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Lab Book # 28.13

Appendix

% Phosphorus
(dry basis)

Correlation Plot of the Class Data

7.0000
6.0000
5.0000
4.0000
3.0000
2.0000
1.0000
0.0000

group data
class mean

9 10

Group #

% Dihosphorus
Pentoxide (dry basis)

Figure 1. Percentage Phosphorus (reported as %P, dry basis) Data of All Groups

20.000
15.000
group data
class mean

10.000
5.000
0.000
1

9 10

Group #
Figure 2. Percentage Phosphorus (reported as %P2O5, dry basis) Data of All Groups
Statistical Calculations of Class Data
Percentage Phosphorus (% Pdry basis)
Q-test:
n = 10
Qtab,95% = 0.466
range = highest value lowest value
= 6.6148 (Grp. 5) 5.3604 (Grp. 9)
= 1.2544
Qlowest = |lowest/suspect value nearest value|
range

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Lab Book # 28.13

= |5.3604 (Grp. 9) 5.9042 (Grp. 2)|

1.2544
= 0.434
Qlowest < Qtab, therefore accept 5.3604%
Qhighest = |highest/suspect value nearest value|
range
= |6.6148 (Grp. 5) 6.4846 (Grp. 3)|
1.2544
= 0.104
Qhighest < Qtab, therefore accept 6.6148%
Mean:
X = Xi
n
= 5.9889 + 5.9042 + 6.4846 + 6.2310 + 6.6148 + 6.3844 + 6.1711 + 6.3608 + 5.3604 + 5.9609
10

X = 6.1461
Standard Deviation:
s = |Xi X|2
n1
= (5.9889 6.1461)2 + (5.9042 6.1461)2 + (6.4846 6.1461)2 + (6.2310 6.1461)2 +
(6.6148 6.1461)2 + (6.3844 6.1461)2 + (6.1711 6.1461)2 + (6.3608 6.1461)2 +
(5.3604 6.1461)2 + (5.9609 6.1461)2
9

s = 0.3621
Relative Standard Deviation:
rsd = s x 100% = 0.3310 x 100%
X
6.1461
rsd = 5.891%
Percentage Diphosphorus Pentoxide (% P2O5 dry basis)
Q-test:
n = 10
Qtab,95% = 0.466
range = highest value lowest value
= 15.157 (Grp. 5) 12.283 (Grp. 9)
= 2.874
Qlowest = |lowest/suspect value nearest value|
range
= |12.283 (Grp. 9) 13.529 (Grp. 2)|
2.874
= 0.434
Qlowest < Qtab, therefore accept 12.283%
Qhighest = |highest/suspect value nearest value|
range

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Lab Book # 28.13

= |15.157 (Grp. 5) 14.859 (Grp. 3)|

2.874
= 0.104
Qhighest < Qtab, therefore accept 15.157%
Mean:
X = Xi
n
= 13.723 + 13.529 + 14.859 + 14.278 + 15.157 + 14.629 + 14.140 + 14.575 + 12.283 + 13.659
10

X = 14.083
Standard Deviation:
s = |Xi X|2
n1
= (13.723 14.083)2 + (13.529 14.083)2 + (14.859 14.083)2 + (14.278 14.083)2 +
(15.157 14.083)2 + (14.629 14.083)2 + (14.140 14.083)2 + (14.575 14.083)2 +
(12.283 14.083)2 + (13.659 14.083)2

s = 0.830
Relative Standard Deviation:
rsd = s x 100% = 0.830 x 100%
X
14.083
rsd = 5.89%