Determination of Chemical Formulae:

The Reaction of Zinc and Iodine

Objective:
In this lab you will synthesize zinc iodide from elemental zinc and iodine. From data you
gather you will determine the empirical formula for zinc iodide and evaluate the validity of the
Law of Mass Conservation and the Law of Constant Composition. Finally, you will investigate
chemical reversibility by decomposing a compound (zinc iodide) back into its constituent
elements (zinc and iodine, respectively).
Introduction:
When two elements react, they combine to form compounds with integer atom ratios.
Although the individual atoms are too small to see and count, the simplest chemical formula (i.e.
empirical formula) can be determined by keeping track of the mass of materials that react to form
the compound. From the mass ratio of reactants, mole ratios between elements in a compound
can be determined using the relative molar masses found on the periodic table. This atom
bookkeeping is called stoichiometry, from the Greek stoikheion (element) and metron (to
measure).
In this experiment, zinc iodide will be synthesized by combining granular zinc metal with
elemental iodine dissolved in a slightly acidic aqueous solution. The masses of iodine and zinc
that react will be measured, from which the mole ratio, mol I/mol Zn, can be calculated and the
empirical formula, ZnxIy determined.
If accurate data are obtained, the empirical results for x & y will scale to those for simple
integers, from which you can find the accepted values for x & y. There are at least two
approaches to determine the stoichiometry of this reaction:
(1) analyze a sample of pure zinc iodide to determine the masses of each element
present in the compound;
(2) synthesize zinc iodide by reacting a known mass of iodine with an excess of zinc
and determine the masses of the product obtained as well as the leftover zinc.
In this experiment, you will use the second approach. Because zinc is an insoluble solid
and the reaction product is soluble in water, the product can be easily separated from unreacted
zinc by decantation and washing. Moreover, if the masses of all materials are measured before
and after the reaction, the amount of each present in the product can be determined. The mass of
zinc iodide obtained can be determined by evaporating the water and weighing the resulting solid
product. By comparing the mass of zinc iodide obtained with the sum of the elemental zinc and
iodine masses used in the synthesis, the Law of Mass Conservation can be evaluated. If the Law
of Mass Conservation is obeyed, the mass of zinc iodide formed will be equal (within the limits
of experimental error) to the sum of the mass of zinc and iodine consumed. By carrying out the
reaction with varying amounts of zinc and iodine, you will be able to investigate the validity of
the Law of Constant Composition. Is mass conserved and what is the true formula for zinc
iodide? Do zinc and iodine combine with set ratios, despite being reacted in varying amounts?
To find out, you must complete the experiment.

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Safety Precautions:

Safety goggles must be worn at all times while you are in the laboratory.
Handle iodine with care: the solid and concentrated solutions can cause burns. The
action of iodine on skin and clothing is similar to chlorine bleach, so wash it off
thoroughly with soap and water if it spills on your skin. Iodine can be quite corrosive,
so clean up spills quickly with the 5% sodium thiosulfate solution.
Acetic acid is mildly corrosive: this solution is approximately 6 times the
concentration in household vinegar; avoid spilling the liquid on your skin and rinse
any affected area for at least 15 minutes under copious running water.
Hot glass looks identical to cool glass. Please use caution to avoid burning yourself.

Table 1: Masses of Zinc and Iodine per Synthesis

Assigned Synthesis Number

Initial Mass of Zinc (g)

Initial Mass of Iodine (g)

2.0

3.0

1.0

2.0

2.0

1.0

3.0

2.0

Procedure:
Synthesis of Zinc Iodide
1) Record the mass of a clean, dry small beaker as precisely as possible (with at least
milligram sensitivity).
2) Transfer the assigned mass ( 0.1 g) of 20 to 30-mesh granular zinc metal from weighing
paper to the beaker and reweigh the beaker to the nearest milligram; record the mass of
the added zinc by difference.
3) Next, transfer the assigned mass ( 0.1g) of iodine crystals from glazed weighing paper
to the same beaker, taking care to avoid spilling any iodine crystals. If any iodine does
spill, clean it up immediately with 5% sodium thiosulfate solution in a manner directed
by your instructor. NOTE: Iodine is especially corrosive to balance pans if left in
prolonged contact. Record the mass of the added iodine by difference.
4) Working at your lab desk, add 9 drops of 6 M acetic acid to 15 mL of deionized water in
a graduated cylinder and add 10 mL of this solution to the zinc/iodine mixture. Swirl the
beaker contents and record your observations (especially with respect to any color and/or
temperature changes) while the reaction takes place.
5) After 10 to 15 minutes, the reaction will be complete, as evidenced by the disappearance
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of the dark orange/brown color of the dissolved iodine. When the reaction is complete,
the solution should be nearly colorless and the unreacted zinc granules should be easily
visible.
6) While waiting for the zinciodine reaction to go to completion, add a boiling stone (1 is
enough!) to the tall 200 mL beaker from your drawer. Record the mass of the beaker
with the boiling stone.
7) When the reaction is complete, carefully decant the warm liquid contents of the small
beaker into the previously massed beaker containing the boiling stone. Be careful not to
transfer any of the solid zinc particles during decantation.
8) Next, rinse the zinc granules three times with 1 mL aliquots of the acidified water
solution and decant these washings into the beaker containing the boiling chip.
9) Rinse the zinc granules a final time with the remaining portion of the acidified water and
discard this washing solution into a small beaker, being careful not to lose any of the zinc
in the process.
10) Carefully dry the zinc and beaker on a warm hot plate. Swirl the beaker containing the
zinc granules occasionally to redistribute them and to speed up the drying of the zinc.
When the zinc and beaker are dry, the zinc will flow freely and no longer adhere to the
sides of the beaker.
11) Allow the dried zinc and beaker to cool to room temperature before massing to the
nearest milligram. Determine and record the mass of the dried zinc by difference.
12) Discard the collected washing solution down the drain with running water.

Part 2: Isolation of Zinc Iodide

1) Using a hot plate, gently heat the beaker containing the zinc iodide solution and boiling
stone to evaporate the solvent (water) over a course of 25 minutes or so. If the solution
shows a tendency to boil irregularly or spatter, stir it occasionally with a glass stirring-rod
until nearly all the water has evaporated. When the last traces of water have evaporated,
the crackling sound will cease and some of the product may discolor, becoming off-white
or light yellow. Be careful not to heat the solid too strongly which may lead to
decomposition, as evidenced by a dark yellow color or the emanation of purple vapors.
2) Given that the product is hygroscopic, readily absorbing moisture from the air with mass
increases of 1 to 2 mg/min, briefly allow the beaker to cool enough to allow handling and
then cool to room temperature in a desiccator (plastic baggy with silica gel desiccant) for
10 minutes.
3) Determine the mass of the dried product, beaker and boiling stone and record the mass of
the zinc iodide reaction product, calculated by difference. Compare this mass with the
sum of the masses of zinc and iodine that reacted as determined from your data from Part
1. Do your results confirm the conservation of mass principle?
4) Record the appearance of the zinc iodide product. Is the appearance distinctly different
from that of the zinc and iodine reactants?
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Determination of Chemical Formulae

Part 3: Electrochemical Decomposition of Zinc Iodide
Place a spatula tip of the zinc iodide product on a watch glass and dissolve the solid with
a few milliliters of distilled water. Electrolyze the solution by placing two copper-wire electrodes
in the solution, connected by alligator-clip wires to either end of a 9V battery for approximately
1 to 2 minutes. Record your observations of the reaction that occurs and determine the identities
of the materials formed at each electrode. Dispose of the solution down the drain with running
water.
Available Equipment and Reagents:
You will have access to all the equipment in your lab drawer, as well as:

20 to 30-mesh granular zinc metal

solid iodine
6 M acetic acid
distilled water
ice
5% sodium thiosulfate solution
glazed weighing paper
desiccator (plastic baggies, silica gel desiccant)
copper wire electrodes
9 V battery
alligator-clip electrode connectors

Waste Disposal:
All solutions must be washed down the drain with water. Place any remaining zinc
granules or solid zinc iodide in the appropriately labeled waste jar. Place used silica gel
desiccant beads back in the container; dispose of the plastic baggy in the garbage.

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EXPERIMENT 1
Determination of Chemical Formulae
Pre-laboratory Questions (to be completed in your laboratory notebook):
Write the answers to the following pre-laboratory questions in your lab notebook. Submit the
duplicate copy to your TA at the beginning of the lab period.
NOTE: If you have lab Monday, August 29, you do NOT need to turn in these prelabs at
the start of lab. Attach them to your report sheets, which will be submitted on September
12.
1. Calculate the number of moles of each reagent present in 2.3 g of elemental zinc and 1.3 g of
elemental iodine.
2. If, in a similar experiment, 29.73 g of arsenic reacts completely with 19.08 g of sulfur what is
the empirical formula of the resulting compound?
3. What are the noteworthy safety precautions you must be aware of in each part of the
experiment?
SAFETY VIDEO QUESTIONS
Watch the Laboratory Safety Video on Blackboard and answer the following questions in your
laboratory notebook.
1) Explain the proper procedure for smelling a chemical.
2) Describe the procedure for diluting an acid.
3) If you spill an acid or a base, what compound is used to neutralize the spill before cleaning it
up?
4) Where are most of the safety devices in your lab are located?
5) Describe the procedure for treating a chemical splash to the eye.
6) What color is the fire blanket?
7) What should you do with long hair?

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Determination of Chemical Formulae

NOTE: The following report sheets should be neatly filled out AFTER you have completed the
lab and turned in at the next lab meeting. All the information you need should be recorded in
your laboratory notebook.

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Determination of Chemical Formulae

Name: _________________________________

Date: _____________________________

Lab Instructor: ______________________ Lab Day/Time: ___________________________

Determination of Chemical Formulae: Report Sheets

Results/Observations:
Initial mass of zinc:
Initial mass of iodine:
Observations during zinc iodide synthesis:

Mass of dried, unused zinc:

Mass of zinc consumed during the reaction:
Mass of iodine consumed during the reaction:
Mass of dried, purified zinc iodide product:
Appearance of the zinc iodide product:

Observations during electrolysis:

Identities of the materials produced at each electrode:

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Determination of Chemical Formulae

Post-laboratory Questions: (use the back of the sheet, or another page if necessary)
1. Using the mass data for the samples of zinc and iodine that reacted, determine the empirical
formula for zinc iodide. What observations support the assumption that all of the iodine
reacted with the zinc? Explain.

2. Comment on the statement: The properties of a chemical compound are the averages of the
elements that make up the compound. What evidence do you have from this experiment
about the truth (or falsity) of this statement?

3. Do your observations support the principle that mass is conserved in a chemical reaction?
Explain.

4. An impatient student does not wait for all the iodine to react. Subsequently, the remaining
iodine sublimes away during the product isolation step. Will the calculated mass ratio for the
product, g I/g Zn, to be higher or lower than the correct value? Explain.

2090 Fall 2016