Activity 3 Determination of Sulfate

Activity 3
Gravimetric Determination of Sulfate in an Unknown Sample
Objective
The objective of this experiment is to determine the concentration of sulfate ion in an unknown
sample by using gravimetry.
Introduction
Gravimetric analysis is based on the measurement of the mass of a substance of known

composition that is chemically related to the analyte. Gravimetric analysis includes precipitation,
volatilization and electrodeposition methods.
In precipitation gravimetry of the analyte is carried out by the use of inorganic or organic
precipitating agents. The two common inorganic precipitating agents are silver nitrate, which is
used to precipitate halide ions such as chloride, and barium chloride for precipitating sulfate ion.
Additionally, potassium, ammonium, rubidium, and cesium ions can be precipitated by sodium
tetraphenylborate.
Sulfate is quite common in nature and may be present in natural water in concentrations ranging
from a few to several thousand milligrams/liter. Sulfates are of considerable concern because
they are indirectly responsible for two serious problems associated with the handling and
treatment of wastewater. Odor and sewer corrosion problems result from the reduction of sulfates
to hydrogen sulfide under anaerobic conditions.
In an aqueous solution, sulfate ion undergoes the following reaction with barium:
Ba2+(aq) + SO42−(aq) ⇌ BaSO4 (s) Ksp = Ba2+SO 2− = 1.1x10−10 at 25 C
Barium sulfate which forms as a crystalline precipitate, is collected on a suitable filter, washed
with water, then ignited and weighed. From the mass of BaSO4, the amount of sulfate present in
the original sample is calculated.
Reagents Apparatus
 unknown sulfate sample  3.0 mL of 6.0 M HCl  50.0 mL of 0.25 M BaCl2

 ashless filter paper  3 porcelain crucibles  3- 250 mL beakers
 watch glass  desiccator  glass stirring rods
 wash bottle 50 mL graduated cylinder
Procedure
A. Preparation of crucible
1. The crucible should be cleaned and rinsed thoroughly with distilled water.
2. For drying, place the cleaned crucibles in the oven set at 110oC for 2 hrs. Remove the
crucibles with tongs (never touch crucibles with your hands or with paper for the duration
of the experiment) and allow them to cool for 5 minutes before placing them in a
desiccator for cooling to room temperature. Cooling will take about 15 min in the
desiccator.
3. Weigh crucibles to the nearest 0.0001 g. Return them to the oven for 1 hour and repeat
the weighing process which should be carried out until two consecutive masses agree to
within  0.0010 g. It is extremely important that the crucibles should be treated exactly in
the same way during this process and later on when they contain the precipitate.
4. Leave the crucibles in the desiccator
Note: You need to use the same balance throughout the course of this experiment. Use of
different balances, when weighing the crucibles, will introduce an error into your
calculations (a common cause for not being able to bring the crucibles to constant mass).
B. Preparation and Precipitation of the Unknown Sample
1. Measure 0.30-0.50 g unknown sample to the nearest 1 mg and transfer quantitatively into
a 250 mL beaker.
2. Add approximately 50 mL water and 2 mL of 6 M HCl. Stir until the sample is totally
dissolved.
Note. Solubility of BaSO4 at room temperature is around 0.3-0.4 mg per 100 g of water.
Its solubility increases when excessive amount of mineral acid is present. On the other
hand, precipitation should be done in acidic medium. Because in neutral and basic
solutions Ba2+ ions precipitate with PO4 3- , CO3 2- or OH– ions which are present in the
solution. Therefore, precipitation is carried out in weakly acidic medium and addition of
excess acid is avoided. Precipitation in a weakly acidic medium provides precipitate to
occur in the form of large particles.
3. Heat the solution in a hot plate to nearly boiling.

4. Slowly add with stirring 15 mL 0.25 M BaCl2 to the heated solution of unknown.
5. Rinse the stirring rod with distilled water to wash down any remaining precipitate into the
beaker. Set aside for about 10 minutes to allow the precipitate to settle.
6. Meanwhile, heat the crucible in the hottest part of the flame for 2 minutes. Cool to room
temperature and weigh.
7. Prepare a piece of medium ashless paper by folding the paper in half and then in quarters.
Tear off a corner of the outside fold as shown in Fig. 1, so it catches all of the precipitate.
8. Place the filter paper in a funnel and dampen the filter paper with distilled water so it
adheres to the funnel.
9. Pour the mixture with the precipitate into the filter paper using a glass rod as shown in
Fig. 2, until all the mixture have been poured into the funnel.
10. Rinse the beaker and stirring rod with distilled water using a wash bottle into the funnel
to quantitatively transfer the precipitate into the filter paper.
11. Place the filter paper and its contents into a crucible that has been brought to a constant
mass previously. Gently char off the paper on a Bunsen burner.
12. Place the crucible vertically on a triangle supported by a ring stand and adjust the ring so
that the bottom of the crucible is positioned 10 to 15 cm above a flame which is 1 to 2 cm
in height as shown in Fig. 3. Place the lid on the crucible but displace it to one side so
that steam can escape through a slit of ~2 mm in width. Apply heat slowly and gently so
that violent boiling of the water and bursting of the package avoided.
13. When drying is complete, fully cover the crucible and char the paper by increasing the
heat applied to the crucible. Escaping gases should not burst into the flame. Occasionally
lift the lid and check the progress of the charring operation, by observing the blackening
of the paper and the disappearance of white areas.
14. Remove the cover and heat vigorously until the bottom of the crucible turns red hot.
Continue heating until the charred filter paper disappears inside the crucible and what is
left is the white precipitate of BaSO4.
15. Cool the crucible with the precipitate to room temperature in a desiccator.
16. Weigh the crucible with the precipitate.
17. Make 3 trials. Record your data in the table.
Data
Trials
1 2 3
weight of sample (g)
weight of crucible (g)

weight of filter paper
(g)
weight of crucible +
filter paper with
precipitate (g)
weight of precipitate,
BaSO4 (g)
weight of SO42– (g)
% SO42– in the sample

average % SO42– in the
sample
standard deviation
Watch the video on “Gravimetric Determination of a Sulfate” and get the data for trial 1. Data
for trials 2 and 3 are already given in the table.
Calculations
On the basis of the 3 trials, calculate the following:
1. weight of precipitate (BaSO4)
2. weight of SO42–
3. % SO42– in the sample
4. average % SO42– in the sample
5. standard deviation
Guide Questions:
1. What is the importance of making the sulfate solution slightly acidic before the addition
of BaCl2 solution?
2. From the following list, identify the interfering species in the sulfate determination
method used in this experiment: Pb2+, Na+, NO3 -, CO3 2-, PO4 3-. How will they interfere in
the analysis (show the equation for the reaction?
3. If the precipitate is heated at very high temperature (>800oC), the BaSO4 will decompose
as follows:
BaSO4 (s)  BaO (s) + SO3 (g)
What mass of BaO will be produced if the mass of the precipitate (BaSO4) is 0.6825 g?
Reference:
http://users.metu.edu.tr/chem223/Sulfate.pdf

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Activity 3

Gravimetric Determination of Sulfate in an Unknown Sample

Gravimetric analysis is based on the measurement of the mass of a substance of known

Ba2+(aq) + SO42−(aq) ⇌ BaSO4 (s) Ksp = Ba2+SO 2− = 1.1x10−10 at 25 C

 unknown sulfate sample  3.0 mL of 6.0 M HCl  50.0 mL of 0.25 M BaCl2

B. Preparation and Precipitation of the Unknown Sample

3. Heat the solution in a hot plate to nearly boiling.

weight of sample (g)

weight of crucible (g)

% SO42– in the sample

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