Honors Lab 4: Gravimetric Analysis

Gravimetric analysis is a technique by which analyzing the mass of a precipitate allows for the
determination for the original chemical makeup of an analyte. The analyte must be soluble, and after
dissolving, another solution that causes precipitation must be added in order to remove one of the ions
from solution.

For instance, if an alkali sulfate (the alkali cation being represented as M+) is added to water, the
following reaction will occur:

M2SO4 (s) → 2 M+ + SO42-

If a solution of barium is added to the solution, the barium ions will combine with the sulfate ions to
form a precipitate of barium sulfate as follows:

Ba2+ + SO42- → BaSO4 (s)

If the sulfate is filtered out of solution, dried, and then massed, the number of moles of the precipitate
(and thus the number of moles of sulfate, as it is a 1:1 ratio in BaSO4) can be determined. The moles of
sulfate can be converted into mass of sulfate, which would be the same as the mass of the sulfate in the
original analyte sample via conservation of mass. By determining the mass percent of sulfate in the
original sample, the formula of the original analyte can be determined. In order to ensure that all sulfate
ions precipitate out, it is beneficial to ensure that the precipitation occurs as slowly as possibly, as the
slower the rate of solid formation, the larger the crystals will be that will form and thus the easier it will
be to filter them.

Objectives

To determine the identity of an unknown sulfate via gravimetric analysis.

Materials

* 250 mL beaker * 50 mL beaker * Hot Plate

* Stirring rod * Funnel
* Filter paper * Graduated cylinder * Weigh Boat
* Distilled water * Lab Quest * Beaker tongs
* 0.10 M BaCl2 * 6 M HCl * Sample of unknown sulfate

Pre-Lab

1. Calculate the mass percentage of sulfate for a) lithium sulfate, b) sodium sulfate, and c)
potassium sulfate.
2. Identify at least one place in the procedure where sulfate ions may be lost through laboratory
error. Be specific (identify how the error leads to a loss of ions)!
3. Calculate the mass BaCl2 that would be necessary to create 150. mL of 0.10 M solution.
Data Table – Make your own!
You should have 5 mass measurements including the final mass of the precipitate, which is
calculated!

Calculations

1. Calculate the number of moles of BaSO4 created.

2. Calculate the number of moles of SO42- ions are present in the BaSO4.
3. Determine the mass of SO42- in the BaSO4.
4. Assuming all mass was conserved, calculate the experimental mass percent of sulfate ions in the
original sample.
5. Get the identity of your unknown, and using the accepted mass percent of your sulfate
calculated in the pre-lab, calculate your percent error.

|experimental – accepted| * 100% = percent error

accepted

Analysis

1. Quantitatively prove that the Ba2+ ions are in excess during the precipitation reaction.
2. Why is it unsafe to pour a solution containing excess Ba2+ ions down the drain?
3. Calculate the concentration of your alkali ion and the chloride ion in your ending solution.
4. Draw the following diagrams:
a) A dissolution diagram of BaCl 2 dissolved in water. Make sure to size the ions and the atoms in
the water molecules correctly relative to each other, as well as orienting the water molecules correctly
b) A precipitation diagram of all species present in the beaker (both in the precipitate and those
still in solution) after the precipitation reaction has gone to completion

Error Quantification

Describe how each of the following errors would affect the determination of the percent by
mass of sulfate in the original compound, if at all.

1. Not all the original sample was successfully transferred into the beaker during step 1
2. 40 mL of BaCl 2 was added in step 3 instead of 30 mL
3. The final product is not completely dry when obtaining the mass
Procedure:

1. Write down the letter of the sample you were assigned. At the balance, zero out a weigh boat
and then mass out between 0.25 g and 0.30 g of the sample. Record the mass in your data table, and
then transfer the sample into a 250 mL beaker.
2. Add approximately 50 mL of distilled water to your beaker. Next, go to the hood and add about
20 drops of 6 M HCl to your beaker. Stir the beaker until all of your sample dissolves. Leave your
stirring rod in the beaker when you are finished.
3. On the hot plate, heat the solution in the beaker to approximately 90oC. Use a Lab Quest with a
temperature probe to track the temperature. (You can turn your hot plate all the way up to speed this
up.) After the solution has reached 90 oC, remove it from the hot plate.
4. Add 30 mL of 0.1 M BaCl 2 to a 50 or 100 mL beaker.
5. SLOWLY (using a dropper) add the BaCl 2 to the beaker while stirring. Adding all of the BaCl 2
should take 2-3 minutes, but no more than that. Rinse your stirring rod off into the solution when you
are done, and allow the BaSO4 precipitate to settle for about 5 minutes. Cover with Parafilm and put it
into a cabinet for tomorrow.

*STOP HERE* Day 2 is below

6. Put your group name on some labeling tape and then attach the tape to a weight boat. Once the
tape is added, obtain the mass of the weigh boat.
7. While the precipitate is settling, set up a filtration apparatus using a funnel and filter paper.
Mass the filter paper before placing it into the funnel. Seal you filter paper to the inside of the
funnel by adding some distilled water and turning on the sink to begin filtration.
8. After the precipitate has settled in the solution, pour it into the funnel to filter out the solid.
Make sure to rinse your beaker and stirring rod with distilled water to get all the precipitate onto the
filter paper. If your filtrate is cloudy after the first filtration, re-filter it to ensure you have caught all of
the precipitate. Filter your solution up to three times if necessary, but not more than that.
9. Before removing your funnel from the flask, rinse the precipitate with a small amount of
distilled water.
10. Using a spatula, carefully remove the filter paper from the funnel and place it on a weigh boat.
If any precipitate remains in the funnel, rinse it into the weigh boat. Take the weigh boat and put it into
the drying oven.
11. The filtrate in your flask is not safe to pour down the drain. Please pour it in the
appropriate labeled waste beaker.
12. Clean up your station.
13. The next day, obtain the mass of the dried filter paper, weight boat, and precipitate. The BaSO4
may be thrown into the trash along with the filter paper and the weigh boat.