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Introduction:
Hydrogen Sulfide, along with many other gases, can be safely generated in a large
syringe. Zinc sulfide and hydrochloric acid are mixed to produce 50-55mL of H2S. The
production of H2S is rapid, taking about 15 seconds to fill the syringe. The reaction is:
Purpose:
The purpose of this experiment is to generate hydrogen in a syringe and to perform
several experiments with it.
Equipment/Materials:
ZnS powder syringe
6M HCl latex syringe cap
6M NaOH pipet
DI water 15cm length of latex tubing
universal indicator one-holed stopper
conc. NH4OH birthday candle
6% H2O2 well plate
30% H2O2 >/= 4gal Ziplok bag
MnO2 powder gloves
2% CuSO45H2O 400mL beaker
2% Cd(NO3)24H2O 250mL beaker
2% Pb(NO3)2 18x150mm test tube (30mL) w/ stopper
0.5% Bi(NO3)35H2O Pasteur pipet
500mL Roundbottom flask
Safety:
Procedure:
1. Neutralization Solution. Pour 100 mL of 6M NaOH into a 400-mL beaker, and place
it inside the hood for later use. This solution will be used to neutralize excess reagents
and can be used in an emergency to neutralize and absorb the reagents, should they
spill or accidentally discharge.
2. Remove the plastic cap that covers new syringes. Break in the plunger by moving it
up and down several times.
7. Place the latex syringe cap over the luerLOK fitting. The
set-up should look like that in Figure 2. Shake the syringe
to mix the reagents and generate the hydrogen sulfide. It
may be necessary to help the plunger move up the barrel.
After gas generation has stopped, pull the plunger further
outward an additional 5 mL in order to create a slightly
reduced pressure inside the syringe. While working inside
the fume hood, remove the latex syringe cap while it is
directed upwards. Note: Never remove the cap with the
syringe aimed downward; acid will spray from
the syringe. Figure 2. Set-up for generation of hydrogen
8. Carefully turn the syringe so that the top is down, and discharge the excess acid into
the neutralizing solution. Immediately cap the syringe to prevent loss of the hydrogen
sulfide.
9. Washing H2S. In order to remove traces of unwanted chemicals from the inside
surfaces of the H2S-filled syringe, the syringe must be “washed” prior to use in
experiments. To do this, suction 5 mL distilled water into the syringe without
discharging any gas, cap the syringe, and tip the syringe from side to side in order to
move the water around to dissolve the contaminants on the inside of the syringe.
Remove the cap, and discharge the wash water into the beaker of 6 M NaOH. Do not
discharge any of the gas. Repeat the washing procedure at least once. Note: H2S(g) is
somewhat soluble in water so the volume of gas will decrease by a few mL with
every wash.
Suitability. Because hydrogen sulfide is extremely toxic, all of these experiments should
only be conducted by those individuals who are experts with syringe manipulation of
gases.
Experiments with Hydroden Sulfide
Experiment A. H2S is Slowly Oxidized. Hydrogen sulfide is fairly soluble in water;
100 mL water at 0o C will dissolve up to 437 mL H2S(g), producing a solution that is about
0.2 M. However, the solution process is fairly slow so that we are able to wash the gas as
described above. Fresh solutions of H2S(g) are clear and colorless but become cloudy
white upon standing. The white suspension of elemental sulfur begins to appear within
an hour and is produced from the reaction between H2S(g) and dissolved oxygen in water:
1. Place 10 mL distilled water in a 18 x 150 mm test tube (capacity 30 mL). Stopper the
test tube with a rubber stopper.
2. Prepare a syringeful of H2S as described above. Wash the gas. Before removing the
syringe cap, pull the plunger outward by 5 mL, thus creating slightly reduced pressure
within the syringe.
3. Replace the syringe cap with a 15-cm length of latex tubing, and bubble 10 mL of the
gas below the surface of the water in the test tube. Remove the syringe/tubing
assembly, and pull about 5 mL air into the syringe to remove most of the H2S from the
latex tubing. Replace the tubing with the syringe cap, and set the syringe aside for use
in Experiments B and C.
4. Stopper the test tube and shake the it vigorously to dissolve some of the H2S(g). Set the
stoppered test tube aside, and observe it over the next several hours. After 24 hours
most of the H2S will have been destroyed by oxidation. Discard the resulting solution
by adding it to the Neutralization Solution.
1. If necessary, prepare a syringeful of H2S as described above. Wash the gas. Before
removing the syringe cap, pull the plunger outward by 5 mL, thus creating slightly
reduced pressure within the syringe.
2. Remove the syringe cap, suction 20 mL of the universal indicator/pH 8 solution into
the H2S-filled syringe, replace the latex cap, and shake to mix the reagents. The pH of
the solution will drop from 8 to 4 as the H2S dissolves in the solution.
3. Discard the resulting solution by adding it to the Neutralization Solution. Keep the
syringe capped when not in use. Excess H2S(g) can be used in Experiment C.
1. Pour 25 mL 6 M NaOH into a 150 mL beaker. Use the H2S(g) that remains from
Experiments A and B or prepare a fresh syringeful of H2S as described above. It is
unnecessary to wash the gas for this experiment.
2. Remove the latex syringe cap from the H2S-filled syringe, and suction a few milliliters
of NaOH(aq) into the syringe. Hydrogen sulfide reacts instantaneously with the
NaOH(aq). The plunger may move rapidly inward and/or the NaOH solution will be
drawn rapidly into the syringe. The reaction is so rapid, it could be surprising. The
beaker is used because the beaker walls will contain any splashed NaOH(aq). This
solution can be slowly discarded down the drain with large amounts of water. If
possible, use a sink in the hood and wear gloves.
Experiment D. H2S Burns in Oxygen with a Blue Flame.
1. Fit a 15 cm piece of latex tubing into the end of a glass Pasteur pipet (Flinn GP 7043)
as shown in Fig. 1. It should make a snug fit.
4. Equip a one-holed rubber stopper with a birthday candle. Set the candle a safe
distance away from the syringe and light the candle.
5. The general arrangement of the experimental apparatus is shown in Figure 2. Fit the
syringe with the pipet/tubing assembly. Two people are needed to complete this
procedure.
6. Move the tip of the pipet into the vicinity of the candle flame. Slowly discharge the
H2S into the candle flame at a rate suitable to ignite the gas and maintain a flame.
7. Carefully move the burning pipet into the O2-filled flask. The H2S will burn with a
hotter flame, and the characteristic blue flame will be evident. An audible “roar” will
be heard coming from the mouth of the flask.
Important! Never withdraw the plunger while the pipet is lit! H2S forms explosive
mixtures with air.
Sulfur dioxide is an acidic oxide. In order to test for the presence of SO2, withdraw
40-50 mL of the gas mixture (lf SO2 and O2) from the flask with a clean syringe
equipped with a length of latex tubing. Suction 10 mL of a slightly basic aqueous
solution of universal indicator into the SO2/O2-filled syringe and it will turn to its
acidic color. Excess H2S(g) can be used in other experiments or should be destroyed as
described above in the Disposal section.
2. Transfer 3 mL of the appropriate metal ion solution to each well of a 12=well plate
shown in Figure 3. Transfer 5 mL of 6 M NaOH to each of two wells (labeled “OH-)
and 5 mL of 30% H2O2(aq) to each of two wells. (If Experiment F is not being
performed, only one well of each metal ion is required, and the wells of H2O2(aq) are
not required.)
Prepare a syringeful of H2S(g) and wash the gas. Cap the syringe with a latex cap. Place
the filled well plate along with the H2S-filled syringe and a plastic disposable pipet
into a large >4 L or gallon size Ziplock bag. Zip the bag shut with a pocket of trapped
air to support the bag above the well plate. Dispense all of the H2S(g) above the
surface of the metal ion solutions. (Avoid dispensing it over the NaOH and the H2O2
solutions.) An immediate reaction will be noted for each of the metal ions. Blue
Cu+2(aq) will produce a brown web-like film of CuS(s) on the surface. Colorless
Cd+2(aq) will produce a distinctive yellow precipitate of CdS(s). Colorless Pb+2(aq)
will produce a spectacular silvery mirror of PbS(s) on the surface. The reactions
between the various metal ions and H2S(g) are similar; the reaction for Cd+2(aq) is:
Allow the reactions to proceed for at least 5 minutes before going on to Experiment 56.
Do NOT open the ZipLock bag. The two wells of NaOH(aq) will absorb the excess
H2S(g) overnight. Clean-up: No clean-up is necessary at this point if Experiment 56 is
being performed. If Experiment 56 is not being performed, follow the Clean-up
procedure at the end of Experiment 56.
Experiment 56. Reoxidation of Metal Sulfides. Without opening the ZipLock bag, use
the plastic disposable pipet to transfer at least 3 mL of H2O2(aq) to one of each pair of
wells for each metal sulfide. Within a few minutes, bubbles will appear in the well
containing CuS. Within 40 minutes the solutions containing CdS and PbS will have
returned to clear. In both cases, the sulfide anion has been oxidized to the sulfate ion
as per:
Within 2 – 3 hours the dark color of bismuth sulfide will be replaced with white,
insoluble bismuth sulfate:
Bi2S3(s) + 12 H2O2(aq) → Bi2(SO4)3(s) + 12 H2O(l)
Clen-up: Allow the bag to stand overnight. The NaOH(aq) will react with excess H2S(g).
Without opening the ZipLock bag, suction a few mL of the NaOH(aq) into the syringe
1
“Skunk Non-scents,” Nancy Toughette, Chem Matters, page 7, October, 1996.
to remove traces of H2S(g). Wear gloves to avoid contact with unreacted H2O2(aq). It
is now safe to open the bag indoors. Remove the contents carefully and discard the
bag and pipet in the trash. Discard metal ions according to local regulations. Wash the
syringe contents (NaSH(aq)) down the drain with plenty of water.