Advanced Chemistry

GRAVIMETRIC ANALYSIS

Goals consumed to fulfill the daily requirement of

1. Use the method of solution and
precipitation to separate substances
2. Gain a better understanding of
gravimetric analyses
Materials and Equipment
Beaker, plastic 30 mL
Beaker, plastic 150 mL
Coffee filters, large white (4)
Cup, plastic 12 oz
Digital balance
Funnel
Glass beaker, 50 mL
Glass stir rod
Magnesium sulfate, MgSO4
Rubber band
Materials Not Included
Distilled water
Household ammonia, NH4OH (The regular
or lemon scent types will work .)
Paper towels
Plant food
Plates (2)
Background
Gravimetric analysis is one of many
techniques that analytic chemists use to
determine the composition of a mixture
of substances. Suppose, for example, that
you needed to know the precise amount
of calcium in milk or the amount of iron in
raisins. You might perform experiments to
separate the desired chemical from all the
other substances. By comparison of the
amount of iron to the total weight of the
raisins you could solve for the percentage
of iron in the raisins. With that information
and the known daily requirements you could
establish how many raisins would need to be
iron intake.
Gravimetric analysis uses measurements
of mass as a technique. The mass of the
mixture is compared to the mass of the entire
substance to establish percent composition,
as illustrated in the example above. This
is commonly accomplished by dissolving
a substance and re-precipitating only one
of the components to recover the desired
substance.
Since gravimetric analysis is a quantitative
analytical technique rather than a qualitative
technique, you will need to be as careful as
possible, especially in product transfers, so
that product loss is minimized. Analytical
techniques will be explained throughout the
laboratory. Follow them precisely and your
results will be better. You will also use the
technique of repetition and averaging to give
better results.
Plant food has phosphorus in the form of
ammonium phosphate and urea phosphate.
The plant food box will give the percent of the
available phosphate in the form of P2O5. The
plant food is dissolved and the phosphate
precipitated with MgSO4 (Epsom salts) and
NH4OH (ammonia). This forms a precipitate of
MgNH4PO4• 6H2O which is a hydrated complex,
as can be seen by the 6H2O in the formula.
Procedure
The following are instructions for operat-
ing a balance.
1. If the balance does not work, check to
see that the plastic has been removed
from the batteries. Remove any cover
that protects the balance plate.
2. Place the balance on a firm surface and
turn it on. The balance may or may not
read 0.00 when you first turn it on. Push

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the mode button and scroll through the
different kinds of weight units. Keep
pushing until you see “g” which stands
for grams.
3. Press the “tare” button to zero the
balance. Once you do this you should see
0.00 on the display. Note: the balance is
very sensitive; handle it with care.
4. Place a small object on the balance plate
and practice using the “tare” function until
you are comfortable with using it. Notice
that the balance records negative values
after you have performed the tare function
and removed the item from the balance
plate. If you put the item back onto the
plate it should measure zero again.
Experimental Procedures
1. Prepare the balance for use. Place a 30
mL plastic beaker on the balance and
tare it. The balance should read 0.00 g
with the beaker on it.
2. Add approximately 1.0 gram of plant
food to the beaker. Record the exact
amount of plant food used in the table
in your lab workbook. Note: Some
plant foods absorb water (they are
hydroscopic). If you notice that the plant
food is moist make a note of that for later
discussions.
3. Remove the beaker from the balance
and add 20 mL of distilled water to the
beaker to dissolve the plant food. Stir
this for about one minute until the plant
food is dissolved.
4. Place a filter in the funnel and place the
funnel into the 150 mL plastic beaker.
Slowly pour the solution from Procedure
3 into the filter. Be very careful that you
do not spill any of the solution.
5. Wash the 30 mL beaker with an
additional 10 mL of distilled water and
pour this into the 150 mL beaker from
Procedure 4.
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Gravimetric Analysis
Note: Do not do this procedure later
in the lab. In this section water is a
solvent so a little more water just
1
washes the sample. Later on when
you have a precipitate, water will
dissolve the precipitate and lower
your yield.
6. After the solution has been collected in
the 150 mL plastic beaker, remove the
funnel and discard the filter paper.
7. Prepare a 10% MgSO4 (Epsom salts)
solution by weighing 2.5 grams of MgSO4
into a 50 mL beaker. Add 25 mL of
distilled water. Stir the MgSO4 for about
two minutes to dissolve it. Ignore any
fine crystals that don’t dissolve.
8. Pour the MgSO4 solution into the filtrate
you collected in the 150 mL plastic
beaker in Procedure 6. Stir the solution
for 15 seconds to ensure it is well mixed.
9. Make sure you have a well ventilated
area. Pour about 40 mL of ammonia
into the 50 mL glass beaker. With the
glass stir rod, slowly pour and stir the
ammonia into the plant food filtrate.
You should see a white precipitate form.
Wait a few minutes until the reaction is
complete.
10. With a pencil, write #1 on a dry piece of
filter paper. Tare the balance and weigh
the filter paper. Record the mass in the
table in your lab workbook.
11. Place a filter
paper over the
plastic cup so
that it forms a
shallow “cup.”
Fold the outside
edges down and
secure them with
a rubber band.
See Figure 1.1.
12. Use the stir rod
to briefly stir the
solution from Figure 1.1
3
Advanced Chemistry

Procedure 9. Carefully pour this solution e. Divide the mass of P2O5 by the mass
into the filter (Procedure 11). The of the original plant food and multiply by
precipitate is very fine and it will take 100% to get percent P2O5, and record the
some time (45 min.), so you will need to value.
be patient.
f. Repeat for each trial and determine
13. Once the filtering is complete, put the averages.
filter paper on folded paper towels. The
g. Calculate percent error, using average
towels will draw off some of the liquid
percent P2O5 in your sample and percent
and lessen the drying time. Be very
P2O5 reported on the container of plant
careful to not lose any precipitate.
food.
14. When most of the excess moisture is out
of the filter paper, put it on a reaction
plate to dry overnight. Develop Your Own Procedure
Describe and perform a procedure to
15. Clean all your lab equipment and repeat answer one of the following questions:
the experiment from the beginning
in order to average the results. In 1. Is the amount of phosphorus the same in
Procedure 10, write #2 on the filter paper different brands of plant food?
for the second trial. 2. Does the amount of phosphorus differ in
16. Once you are confident that the filter different sample sizes of the same plant
paper is dry, weigh the paper and the food? (Is the plant food a homogeneous
precipitate. (Remember to zero the or a heterogeneous mixture?)
balance before you weigh anything.) 3. Is the amount of phosphorus in different
Record the value in the table. plant foods related to the cost of
17. Solve for the mass of the precipitate by the plant foods? Be sure to identify
subtraction. dependent and independent variables as
well as controls and constants.
18. Record your data and results of your
calculations in Table 1.1.
a. You will find the percent phosphorus
(as P2O5) listed on the label of the plant
food container.
b. Record the mass of the
MgNH4PO4•6H2O precipitate and
determine the number of moles of
MgNH4PO4•6H2O precipitate formed
(gram molecular mass = 245 g/mol).
c. Determine the moles of P in the
precipitate and record. Convert the
moles to grams P.
d. Assume that available phosphorus is
in the form P2O5 and solve for grams P2O5
in the original plant food using the gram
molecular mass of P2O5 (142 g/mol) and
percent P in P2O5, and record the values.

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