EXPERIMENT 8 DETERMINATION OF THE PERCENTAGE OF OXYGEN IN THE AIR To measure the amount of oxygen in air we will use the same principle employed by the pneumatic chemists--a sample of air will be trapped in a test tube along with something that uses up all of the oxygen in the tube, allowing the water to rise in the tube. Rather than use a candle or a mouse, we will employ the reaction of oxygen with iron in the form of steel wool. When conditions are arranged properly, oxygen reacts rapidly and completely with the iron, as described by the following (unbalanced) reaction (the balancing of this reaction will be left as an exercise for you): Fe + O2---> Fe2O3 This reaction is more complex than just the direct combination of oxygen with iron. It also requires the presence of water and is accelerated by acids. However, the solution in contact with the iron must not be allowed to become too acidic; otherwise some hydrogen will form by the reaction Fe + 2 H+ —> Fe2+ + H2 EXPERIMENT: Avoid breathing the acetone vapor or spilling it on your skin. Acetone is a flammable solvent. There must be no open flames in the hood. Attach a strip of masking tape (on which to mark the water level) to two large culture tubes (lipless test tube). Attach a set of clamps to your ring stand so that the test tubes can be mounted, inverted, in a 1-L beaker filled nearly to the brim with tap water. Weigh two 1.0-g portions of fine (size 00) steel wool. Do not compress the material. Obtain 100 ml each of acetone, l.0 M acetic acid and 0.1 M acetic acid. To save materials, please arrange with a nearby student to share your acetone and 1.0 M acetic acid, as these materials may be used by two students to clean their steel wool pieces. However, each student should obtain their own 0.1 M acetic acid. Using forceps, rinse a piece of steel wool in acetone for about 30 seconds to remove any oily material from the surface of the steel wool. Shake off the excess acetone, drain the steel wool briefly on a paper towel, and transfer it to the 1.0 M acetic acid solution. With your forceps, agitate the steel wool occasionally for about a minute. Then shake off the excess, drain on a paper towel briefly, and put the steel wool in the beaker containing 0.1 M acetic acid, agitating it for about 30 s. Using forceps, remove the steel wool and shake it vigorously to remove as much solution as possible. Then insert the steel wool in the 20- x 150-mm culture tube, pushing it to the bottom half of the tube. Do not compress the steel wool. It should be spread over most of the bottom half of the test tube. Immediately invert the test tube and carefully lower it into the beaker of water and clamp it in position. The mouth of the test tube must be below the water level throughout the experiment. The initial volume of air is assumed to be the total volume of the test tube (minus the volume of steel wool and adhering solution, which will be determined later). Rinse the forceps in tap water and dry. At 5- to 10- min intervals, mark the rising water level on the masking tape. Using a second test tube, prepare the remaining piece of steel wool and carry out a duplicate run. While you are waiting for the reaction to be completed, weigh a clean dry 250-mL beaker to the nearest 0.1 g. Record its mass. When no further change in water level can be detected (usually 20 to 30 min are required), wait 5 min longer, then adjust the height of the test tube so that the water levels inside and outside the tube are the same. (When the levels are the same, the pressure inside the tube will be equal to the atmospheric pressure.) Now trap the water that has risen in the tube by pressing a rubber stopper firmly against the mouth of the tube. (The stopper should be larger than the mouth of the tube so that it does not enter the tube.) Ask a laboratory neighbor to unclamp the tube while you are holding the stopper against the mouth of the tube. Carefully transfer the water you have trapped into the previously weighed 250-mL beaker. Reweigh and record the mass of the beaker plus water. The volume of this water corresponds to the volume of oxygen that has reacted with the steel wool. With forceps, remove the steel wool and put it in the same previously weighed beaker containing the water. Reweigh and record the mass. Finally, fill the empty test tube to the brim with water and add it to the same beaker and reweigh and record the mass again. The initial mass of the empty beaker and the subsequent three weighings will provide data from which you can calculate the total volume of the test tube, correcting for the volume occupied by the steel wool and adhering acetic acid solution. Alternative method: Instead of attaching tape to the side, you may use a ruler submerged in the water to follow the progress of the rising water. You will need to record the rulers measurements at 5-10 minute intervals Name __________________ Date___________________ DETERMINATION OF THE PERCENTAGE OF OXYGEN IN THE AIR (WORKSHEET) DATA: Density of water = 0.997 g/mL Density of steel wool = 7.70 g/mL Run # Mass of Steel wool Mass of Beaker Mass of Beaker + Water Mass of Beaker + Water + Wet Steel Wool Volume of Test Tube Mass of Water to Fill Test Tube CALCULATIONS: Volume of oxygen in moist air: (mass of beaker and water - mass of beaker)/density of water Volume of steel wool: (mass of Fe/density of Fe) Volume of adhering solution: ((mass of beaker, water and steel wool - mass of beaker and water - mass of Fe) / density of water) Volume of test tube: ((mass of water, beaker, steel wool and water to fill test tube - mass of water, beaker and steel wool) / density of water) Volume of air in tube (volume of test tube - volume of steel wool - volume of adhering solution) Percent Oxygen in the Air (volume of oxygen / volume of air in tube) x 100 Results Run # Percent Oxygen Avg = Conclusions Sources of Error PROBLEMS 1. Consider the reactions given on the first page of this handout. How many grams of iron are required to convert 80 mL of oxygen at STP? 2a. Calculate the total pressure in the flask after all of the oxygen has been removed from the air in the flask. Assume that the temperature is 25̊C, the initial barometric pressure is 760 torr and that air is 21% oxygen by volume. 2b.Actually the air inside the flask was in contact with water. Water vapor accounted for 23.6 torr of the total 760 torr of "wet" air inside the flask. If the O2 was removed from this air, would the pressure be higher or lower than in 2a?
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