Gravimetric Analysis

Determination of Phosphorus Content of

Fertilizer: Skill Building Lab
! 2011, Sharmaine S. Cady
East Stroudsburg University


Skills to build:

! Using vacuum filtration
! Using a digital balance
! Using mass stoichiometry
! Doing a gravimetric analysis






Fertilizer

Scientists estimate that the earth's soil contains less than twenty percent of the
necessary organic nutrients needed to meet our current food production. Carbon,
hydrogen, and oxygen used to synthesize compounds needed for structural integrity are
readily available from air and water. Nitrogen, phosphorus,
and potassium, the building blocks for healthy plants, are
usually not present in sufficient amounts in the soil to
support plant growth. These are known as macronutrients.
In addition, micronutrients, such as calcium, sulfur, and
magnesium, are also necessary, but in smaller
amounts.Table 1 shows the role of these nutrients in plant
growth.
Commercial fertilizers are inorganic or organic
compounds that replenish the soil with additional nutrients
to increase growth and keep plants healthy. In 2001, 53
million tons of fertilizer was used by the agricultural industry in the United States.
Nitrogen fertilizers use ammonia as the building block for the production of water-soluble
nitrogen-containing compounds, such as ammonium nitrate. Phosphorus is mined from
natural geological deposits and mixed with sulfuric acid to make water-soluble
phosphate compounds. Potassium is supplied as potash (potassium chloride) from
evaporation of sea water.
In the United States, the Association of American Plant Food Control Officials
(AAPFCO) is concerned with consumer protection. AAPFCO works with industry to
promote the safe and effective application of fertilizers in an effort to protect soil and
water resources. It also oversees standard methods for fertilizer analysis to ensure that
fertilizer labels are accurate and consistent with nutrient content.
Fertilizers
2

Table 1. Role of Nutrients in Plants

Nutrient Role
N
Essential component of amino acids used
to make proteins
Component of DNA and RNA
Necessary for chlorophyll production
Produces the greatest yield response in
crops
P
Essential component of enzymes used in
photosynthesis
Essential component of nucleic acids (DNA
and RNA)
Stimulates root growth
Essential for seed germination
Aids in efficient use of water
K
Ensures carbon assimilation
Aids in transporting and storing sugars and
proteins
Activates enzymes
Essential for water regulation and uptake
Ensures resistance to frost, drought, and
disease
S
Essential component of two amino acids
Essential component of Vitamin B1 and
enzymes
Ca
Component of cell membranes
Necessary for plant growth and cell
division
Necessary for pollen development
Prevents leaf fall
Mg
Essential component of chlorophyll
Activates enzymes
Other micronutrients (Cu, Mn, Mo, Zn, B
among others)
Essential components of metabolic
enzymes






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3


The label on a fertilizer bag or
container contains three numbers.
These numbers give the percentage of
nitrogen, phosphorus, and potassium,
respectively, available to plants based
upon chemical analysis. Note that the
phosphorus analysis is reported as
percent by mass P
2
O
5
and potassium as
percent by mass K
2
O. Originally,
fertilizers were heated in air to convert
the phosphate and potash into these
compounds, which were then used to
report the nutrient content. Although
analysis techniques have changed, the
label definition has not. In this
experiment, a sample of fertilizer is analyzed for phosphorus using gravimetric analysis
to determine if its label percentage is accurate.


Gravimetric Analysis

Gravimetric analysis is a technique that involves the determination of the mass of
a chemical species of known composition that can be related to the analyte by mass
stoichiometry. You should review mass stoichiometry relationships before starting the
experiment. The Stoichiometry link listed for this experiment provides some examples
of using mass stoichiometry.
The most common gravimetric technique involves precipitation. In this
experiment, the water-soluble phosphate in fertilizer is precipitated from solution with
magnesium sulfate. The precipitate is magnesium ammonium phosphate hexahydrate.
The chemical reaction equation may be written as

PO
4
3-
(aq) + Mg
2+
(aq) + NH
3
(aq) + 7 H
2
O (l) " MgNH
4
PO
4
6H
2
O(s) + OH
-
(aq)

The sulfate ion is a spectator ion and is not included in the chemical reaction equation.
Based on the mass of fertilizer dissolved and the fertilizer analysis, you will need to
calculate the volume of MgSO
4
solution needed to form your precipitate. See the online
theory section for an example calculation. The solution is made basic with aqueous
ammonia in order to precipitate the entiremass of phosphate ion. If the solution is not
sufficiently basic, the following reaction occurs, and some of the phosphate is not
precipitated,which produces inaccurate results:

PO
4
3-
(aq) + H
3
O
+
(aq) ! H
2
PO
4
2-
(aq) + H
2
O (l)

The precipitate must be dried at room temperature to prevent the waters of hydration
from being lost. Once the mass of MgNH
4
PO
4
6H
2
O(s) is obtained, the stoichiometric
ratios between P, P
2
O
5
, and the product will yield the amount of P
2
O
5
in the fertilizer.


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4
3D Molecules
Go to the web site and click on the diphosphorus pentoxide link. Use the radio
buttons to show different views and properties of each molecule. Answer the questions
based on the manipulation of the molecules.








Experimental Methods and Materials





Safety considerations

Wear suitable protective clothing, gloves, and eye/face protection!


You should read the online MSDS for:

Ammonia

Magnesium Ammonium Phosphate

Magnesium Sulfate





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5

Preparation of fertilizer sample

Weigh between 3 and 5 g of fertilizer. Record the brand and type of fertilizer
and the percentage analysis. Place in a 1000-mL beaker. Add 20 mL of distilled
water, a magnetic stir bar and stir to dissolve the fertilizer. If it does not completely
dissolve, add another 20 mL of distilled water and stir. Continue until all the fertilizer is
dissolved or no more solid appears to dissolve. Do not exceed 100 mL of distilled
water. If water-insoluble components remain in the beaker, vacuum filter and save
the filtrate (liquid).



Precipitation of phosphate

Determine the volume of 0.400 M MgSO
4
needed to precipitate the
phosphate based on the label analysis and your mass of fertilizer (see online
example). Add this volume to the beaker. Calibrate the pH meter. Place the
pH probe into the beaker and record the pH. Add 6 M aqueous ammonia
(NH
3
) to the beaker in 5-mL increments until the pH is at least 9.0. Stand the
mixture in an ice bath for 30 minutes. Place a piece of filter paper into the top
of a Buchner funnel. Weigh the top of the Buchner funnel with the filter paper.
Use vacuum filtration to isolate the product (see diagram at right). First, using
distilled water, seal the filter paper over the holes before you filter the solution.
Rinse with 2 15-mL portions of distilled water. Pull a vacuum for 5 minutes
to dry the product as much as possible.



Product purification

The product contains excess water which must be allowed to evaporate. Remove
the top of the Buchner funnel and cover with a Kimwipe. Give to instructor to dry until
the next lab period. Reweigh the Buchner funnel top. Determine the mass of P
2
O
5
in
your fertilizer sample and its mass percentage.








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6


Laboratory Report

Answers to the following questions should appear in the conclusion section of your
report:

1. How does your percentage P
2
O
5
compare with the given value on the label?
Explain any differences.
2. Use Excel to calculate the average percentage P
2
O
5
for the class and the
standard deviation. A large standard deviation indicates that the data points are
far from the average. Does the standard deviation indicate that the class as a
whole had more or less success in obtaining precise results? See the online
instructions for using Excel.




References

European Manufacturers Fertilizer Association Home
Page.http://www.efma.org/(accessed August 2005)

The Fertilizer Institute Home Page.http://www.tfi.org/ (accessed August 2005)

Wink, D. J.;Gislason, S. F.; Kuehn, J. E.Working with Chemistry, 2e; W. H. Freeman &
Company: New York, 2000; pp C-11-C-12.