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PREPARATION AND PROPERTIES OF OXYGEN


* PURPOSE

The objectives of this experiment are to prepare, collect and investigate the properties of oxygen gas.

* DESCRIPTION

This experiment is appropriate for a general or first-year college-prep course. Many common household bleaches contain oxygen in the form of sodium hypochlorite, NaClO. If the hypochlorite ion, ClO-, is decomposed, oxygen gas can be produced. In this experiment, cobalt(II) chloride, a catalyst, will be used to increase the rate of production of oxygen. The properties of oxygen will then be investigated.

* TIME REQUIRED

Two lab periods.

* MATERIALS

Chemicals:
cobalt(II) chloride
magnesium ribbon
charcoal
sulfur
distilled or deionized water
chlorine bleach
steel wool
Equipment:
candle
one hole stopper
250-mL Erlenmeyer flask
Bunsen burner
ring stand
utility clamp
pneumatic trough
eye dropper
rubber tubing
litmus paper
forceps
small gas collecting bottles
glass plates
deflagrating spoon
*See Modifications / Substitutions.

* HAZARDS

Chlorine bleach has a strong odor and should be handled carefully. Never mix ammonia with chlorine bleach; chlorine, which causes severe lung damage is produced. Avoid breathing the sulfur dioxide produced when sulfur burns; it is poisonous. Do not look at burning magnesium; retinal damage may result. Goggles must be worn throughout the experiment.

* MODIFICATIONS/SUBSTITUTIONS

  1. Magnesium sparklers such as those used on the Fourth of July may be used in place of magnesium ribbon.
  2. Charcoal is available in a variety of forms. Old fashioned stick charcoal is preferred.
  3. Sulfur is available from garden supply stores in products such as Ortho's "Flotex".
  4. A 12-oz soda bottle may be substituted for the Erlenmeyer flask.
  5. Any type of fairly deep tray or pan can be used in place of a pneumatic trough.
  6. Baby food jars and their lids may be substituted for the gas collecting bottles and the glass plates.
  7. An old bent spoon or piece of bent copper foil can be used in place of the deflagration spoon.
  8. If cobalt(II) chloride is not available or too expensive, an alternate reaction can be carried out in which 3 or 6% hydrogen peroxide, H202, is used in place of bleach and allowed to react with controlled amounts of the dark royal blue copper amine complex, Cu(NH3)62+. The 3% hydrogen peroxide is available from grocery or drug stores, while 6% hydrogen peroxide can be obtained from drug or beauty supply stores under the brand name "Clairoxide." The copper complex can be prepared by mixing an ammonia solution (household ammonia works fine) with 25 mL of 0.1 M copper(II) sulfate (available under the name "Rooteater" from a garden supply store) until the copper hydroxide precipitate dissolves, leaving the transparent, dark blue amine complex ion. If this alternate preparation is used, a two-hole stopper should be substituted for the one-hole stopper in the flask. The copper amine complex is added to the hydrogen peroxide from an eye dropper inserted in the second hole in the stopper. A trial run should be done by the teacher to determine the amounts of copper amine complex and hydrogen peroxide necessary to fill the five jars with oxygen.

* PROCEDURE

  1. Clamp the neck of a 250-mL Erlenmeyer flask to a ringstand. This will prevent it from tipping over.
  2. Insert the glass tube from an eye dropper in a one-hole stopper that fits the flask and attach a 0.5-m piece of rubber tubing.
  3. Fill five gas collecting bottles to the very top with water; cover with glass plates. Fill the trough 1/4 full of water, and invert the bottles of water into the water. Carefully remove the glass plates, keeping the mouth of the bottle below the water level in the tray.
  4. Put 150 mL of bleach into the Erlenmeyer flask.
  5. Measure out approximately 4 grams of cobalt(II) chloride. Crush any chunks.
  6. When all is ready, add the cobalt(II) chloride to the flask and quickly insert the stopper/hose assembly into the bottle's mouth. Lead the rubber hose from the generator into the tray of water and allow bubbles to escape for a short time to purge the system of air.
  7. Insert the end of the rubber hose under the mouth of one of the bottles of water. As the oxygen bubbles from the hose, it will displace the water from the bottle. When one bottle is full of oxygen, move the hose to one of the remaining bottles.
  8. Lift each bottle of oxygen just enough to slip a glass plate over the mouth. Do not lift the bottle completely out of the water while this is being done. Once the glass plate is over the mouth of the bottle, the bottle can be removed from the trough.
  9. If the reaction stops or slows, swirl the contents of the flask to mix the reactants. When this no longer works, measure another 50 mL of bleach, quickly remove the stopper and add it to the generator. For steps 10-15 an observation table should be prepared.
  10. Light a candle. Remove the plate from one inverted bottle of oxygen just enough to let out any water. Then hold the inverted bottle over a burning candle and remove the glass plate. Observe the flame of the candle.
  11. With forceps hold a small tuft of steel wool in the flame of a Bunsen burner for a few seconds. As soon as it begins to glow red, quickly remove the cover from a second upright bottle of oxygen and hold the hot steel wool in the oxygen gas. While holding the steel wool, use the glass plate to close off as much of the mouth of the bottle as possible. You want to collect any products from the reaction between the oxygen and steel wool. Observe the steel wool. When the reaction stops add 10 mL of distilled water to the bottle, replace the glass plate and shake up the water and collected gas.
  12. In a similar fashion, heat the magnesium in the flame. When the magnesium begins to burn, test it in a similar fashion as that used with the steel wool. Don't forget to add the distilled water before shaking.
  13. Repeat step 11 with a small piece of charcoal.
  14. Use a deflagration spoon to test the reaction of burning sulfur in oxygen. Put a small piece of sulfur about the size of a pea on the spoon. Hold the Bunsen burner soon as the sulfur begins burning, hold the spoon in a bottle of oxygen, and cover the mouth of the bottle as much as possible with a glass plate. When the reaction is over, add the distilled water, replace the plate and shake.
  15. Test the water in each of the bottles with litmus paper, and record your observations.

* SUGGESTED QUESTIONS

  1. What physical properties must oxygen gas possess to allow it to be collected by water displacement instead of air displacement? (Remember ALL gases are less dense than water.) Would this method of gas collection be good for collecting ammonia gas too?
  2. What physical and chemical properties of oxygen were illustrated in step 10 when the oxygen-was poured over the candle?
  3. Write a balanced equation for each burning reaction which occurred in steps 11-14. Write a second balanced equation for those reactions with water which produced a color change in litmus paper.
  4. Give a reason for the difference between how things burned in the air compared to how they burned in oxygen.
  5. Compare the litmus paper results in steps 11 through 14. Suggest a reason why the results may have been the same or different.
  6. Suggest how you can "predict" the litmus paper results based upon the substance you heat in the Bunsen burner.

* DISPOSAL

Decant all solids and place in chemical waste receptacle. The remaining liquid waste may be flushed down the drain with copious quantities of water.

* DISCUSSION

This experiment is a variation of the preparation of oxygen used in kinetic studies. The reaction for the preparation is:
2 NaOCl (aq) ----> 2 NaCl (aq) + O2 (g)

Other reactions for this experiment are listed in order below.

4 Fe (s) + 3 O2 (g) ----> 2 Fe2O3 (s)

2 Mg (s) + O2 (g) ----> 2 MgO (s)

C (s) + O2 (g) ----> CO2 (g)

S (s) + O2 (g) ----> SO2 (g)

* TIPS

  1. If the magnesium oxide produced by the burning of magnesium ribbon proves to be insoluble in water, suggest that students transfer the mixture to a test tube and warm gently before testing with litmus paper.
  2. Do not use activated charcoal. After heating, it produces very little change when held in the oxygen gas.
  3. The z-shaped spoons used to burn sulfur should be made up ahead of time and tested to be certain they'll fit easily into the gas collection jars. If old spoons are not available, a piece of copper foil or light gauge copper metal can be bent into a spoon shape and used.
  4. The experiment should not be done with more than the 150 mL of bleach called for or the reaction may force black cobalt oxide into the delivery tube and into the collection bottles.

* REFERENCES

Alyea, H.N. and Dutton, F.B., Tested Demonstrations in Chemistry, American Chemical Society, Washington, 1960 pp. 7, 87, 91. -- Experiments using oxygen are described.

Joseph, A., Bandwein, P.F., Marhott, E., Pollack, J.F., Castka, J.F., A Sourcebook for the Physical Sciences, Harcourt, Brace and World, Inc., New York, 1961, pp. 32, 136, 150. -- The preparation of oxygen from hypochlorite and hydrogen peroxide are described.

Summerlin, L.R., Chemistry of Common Substances, Silver Burdett Co., New York, 1979, p. 25. -- Describes experiments with oxygen.

Metcalfe, H.C., Williams, J.E., and Castka, J.F., Modern Chemistry, Holt, Rinehart, and Winston Publishers, New York, 1982, p. 185. -- This work describes the chemistry of oxygen.



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