CHEA 1201 L

UNKNOWN ANALYSIS
EXPERIMENT 2. GRAVIMETRIC DETERMINATION OF SULFUR

Unknown No. 4 Jay Meng S. Jusgado

I. Experimental Data

TRIAL 1 TRIAL 2

1. Mass of sample 0.5048 0.4937

2. Mass of empty crucible + lid 35.4570 38.5970

3. Mass of crucible + lid + ash 35.8451 38.9919

4. Mass of unknown sample (ash) 0.3971 0.3949

5. % _____ (unknown) 78.66 79.99

6. Average % unknown 79.33

II. Calculations

1. Calculate the mass of ZnSO4 in the unknown sample. Clearly show

each step of your calculation. Report to 5 significant figures.

Trial 1 = (m crucible +lid + ash) – (m empty crucible + lid)

= 35.8451g – 35.4570g
= 0.3971 g
Trial 2 = (m crucible +lid + ash) – (m empty crucible + lid)
=38.9919 g – 38.5970 g
= 0.3949 g
 2. Calculate the percentage by mass of the unknown sample for both trial 1 and 2.
Show your work. Report your final answer to 2 significant figures.
Trial 1
%Unknown sample = (m unknown / m sample) x 100
= (0.3971 g / 0.5048 g) x 100
=78.66 %
Trial 2
%Unknown sample = (m unknown / m sample) x 100
= (0.3949g / 0.4937g) x 100
=79.99%
Average % of unknown = (%unknown trial 1 + % of unknown trial 2) / 2
= (78.66% + 79.99%) / 2
= 79.33%

III. Guide Questions

1. Explain the purpose of desiccator in the experiment and what is the white material at the
bottom of the desiccator. Give examples of this material.

It prevents the sample or beaker from gathering moisture as it cools. The material at the bottom
is called desiccants and it can be in the form of granulated anhydrous calcium sulfate, calcium
chloride, or silica.

2. Why is it that only pencil was used in labelling the crucibles?

Because graphite has a higher boiling point than ball point inks, thus it will not boil or
melt if heated.

3. In the dissolution of sample, what is the chemical reaction when HCl is added to the
sample? Does this render the sample more, or less, soluble? Explain.

When the HCl is added to the sample, it lowers the pH increasing the BaSO4 ‘s solubility
resulting to the decrease in rate of the precipitation.

4. Give the balanced chemical equation for the reaction between your unknown and barium
chloride solution.

BaCl2(aq)+ZnSO4(aq)-----------=>ZnCl2(s)+BaSO4(aq)
5. In washing the precipitate, explain why hot (and not cold) water was used to wash the
precipitate.

Because hot water  cause molecules to move around relatively faster, thus it can cause the
bonds of the precipitate to break faster.

6. What reagent was used to test for completeness of washing? Write a balanced chemical
equation for this reaction
7. The unknown metal sulfates are hygroscopic and will absorb water from air. The
unknowns must thus be kept in desiccators to remove any absorbed water. How would
your results be affected if your unknown sample was not desiccated? Would this error
cause your calculation of the mass percent of sulfate in the unknown to be too high or
too low? Explain.

Your results will be affected in a way that the mass percent will increase or be too high
rather than too low. If the metal sulfates will not be placed in the desiccator immediately,
it will absorb moisture from the air altering (increasing) its mass and therefore increasing
your mass percent.

8. In this experiment you used an excess of the BaCl 2 solution. How would your results be
affected if you did not use an excess of the BaCl 2 solution? Would this error cause your
calculation of the mass percent of sulfate in the unknown to be too high or too low?
Explain.
9. In the last step of the procedure, you vigorously heated the BaSO 4 precipitate wrapped
in filter paper in a crucible. How would your results be affected if tiny pieces of the filter
paper still remained mixed in with the BaSO4 after heating? Would this error cause your
calculation of the mass percent of sulfate in the unknown to be too high or too low?
Explain.

Even tiny bits of paper can cause error on your calculations because it also has mass. It
can increase the mass percent to a certain degree if it is mixed with the sample.

IV. Problem solving.

1. Suppose that 0.323 g of an unknown sulfate salt is dissolved in 50 mL of water.

The solution is acidified with 6M HCl, heated, and an excess of aqueous BaCl2 is
slowly added to the mixture resulting in the formation of a white precipitate.
Assuming that 0.433 g of precipitate is recovered calculate the percent by mass
of SO42- in the unknown salt.
2. Suppose an unknown metal sulfate is found to be 72.07% SO42-. Assuming the
charge on the metal cation is +3, determine the identity of the cation.