A Colorful Cycle of Copper Reactions Prelab: read the entire laboratory before beginning. Create a data table for your information. Create a flow chart of expected steps. Create a hypothesis. Get stamped prior to starting the laboratory. Prelab Questions 1. How to you perform an error calculation. 2. What are the primary safety concerns in the laboratory. In other words of what do you need be aware? 3. How could this laboratory be applied to real life? Ask your instructor to explain any aspects of the procedures that you do not understand. As you work, keep full, legible records of your observations in the proper sections of your printed Report Form. Preparation At your bench, start two hot water baths for later use: 1) Determine the equipment needed for the section on which you are working. Do not gather equipment until you are approaching the end of one section and are ready to proceed to the next one. Chemistry Department, University of Southern Maine Lab Procedure Page 1 of 8 2) Keep an eye on the clock as this is a multiple day laboratory and you will need to complete the data gathering to the next to last section in three days. 3) Put 150 mL of tap water in a 400-mL beaker on a hot plate. Keep the water at a simmer. Add water from time to time to keep the level between 100 and 150 mL. You will use this bath to heat a flask during part 3. 4) Start a smaller hot-water bath of about 40 mL distilled water in a 100-mL beaker. You will use this hot distilled water to wash a filtered residue in part 3. NOTE: In all operations, be careful to avoid losses of even small amounts of solids or liquids containing copper compounds. If your lab technique is good, you will be rewarded in part 5 with a high percent recovery of the copper with which you start in part 1. Part 1: Converting copper metal to aqueous Cu2+ ions WARNING: Concentrated nitric acid is corrosive and causes severe burns. Handle with care. Dilute and wash up spills with plenty of water. 1. Clean some copper wire with steel wool, and then cut a 3- to 4-cm piece of wire. Chemistry Department, University of Southern Maine Lab Procedure Page 2 of 8 2. Weigh the wire to the full precision allowed by your balance, and record its mass. 3. Make a flat coil of the wire, and place it in a dry 125-mL Erlenmeyer flask. 4. In the fume hood, carefully add 1.5 to 2 mL of concentrated (6 M) nitric acid (HNO3), to cover the copper wire in the flask. 5. Gently warm the flask to speed the reaction if needed, but don’t get the flask hot. 6. If any copper remains undissolved after 5 minutes, carefully add another 0.5 to 1 mL of nitric acid and continue warming. 7. Finally, still in the hood, dilute the resulting solution with about 30 mL of deionized water. Now you may remove the flask from the hood, and continue working at your lab bench. Part 2: Precipitating copper (II) hydroxide WARNING: Concentrated sodium hydroxide is corrosive and causes severe burns. Handle with care. Dilute and wash up spills with plenty of water. 1. Add 6 M sodium hydroxide (NaOH) to the flask slowly, with thorough mixing, until a precipitate forms. 2. Continue adding small amounts of NaOH until the solution is basic to litmus paper. Chemistry Department, University of Southern Maine Lab Procedure Page 3 of 8 3. Then add two additional drops of NaOH and mix well. Part 3: Converting copper (II) hydroxide to copper (II) oxide 1. Increase the volume of solution in the flask to about 100 mL by adding deionized water. 2. Use a screw clamp to suspend the flask containing the reaction mixture in your large hot water bath. 3. Heat for 4 or 5 minutes after the temperature rises to near 100 oC, stirring constantly (glass stirring rod), and then remove from heat and allow to cool. 4. Next, fold a piece of filter paper as shown in Figure 1. 5. Place the paper in a filter funnel mounted in a utility clamp attached to a support stand. 6. Place another Erlenmeyer flask under the funnel to collect the filtrate. 7. Use distilled water from your wash bottle to wet the filter paper. Press the top edges of the filter paper against the sides of the funnel to form a seal. Avoid touching the wet filter paper—even a touch can tear it and allow the filtrate to pass through. Chemistry Department, University of Southern Maine Lab Procedure Page 4 of 8 8. When the 125 mL flask is cool enough to handle, filter the contents, using another flask to collect the colorless filtrate. Do not allow the liquid level in the filter to rise above the top of the paper. 9. Transfer the last traces of the solid CuO from the flask into the funnel, using a stream of distilled water from the wash bottle. 10. Wash the residue on the filter paper three times, using 5-mL portions of hot distilled water from your smaller water bath. 11. Use beaker tongs to handle the hot beaker when pouring the hot water. 12. Allow each portion of hot water to drain through the filter paper into the flask before adding the next portion. 13. Retain the solid CuO on the filter paper for use in Part 4. Part 4: Dissolving copper (II) oxide to form aqueous Cu2+ ions WARNING: Sulfuric acid solution is toxic. Handle it carefully. Prevent eye, skin, and clothing contact. If you spill any acid, immediately notify your laboratory instructor. 1. Place a clean 250-mL beaker under the funnel stem. 2. Dissolve the CuO on the filter paper by allowing about 15 mL of 1M H2SO4 solution to pass through the CuO and the filter paper. 3. Allow the acid solution to drain through the funnel into the 250-mL beaker. Chemistry Department, University of Southern Maine Lab Procedure Page 5 of 8 4. If the solid does not completely dissolve, pour the liquid from the beaker back into the funnel, using a second clean beaker to collect the filtrate. 5. Repeat this procedure until the solid has completely dissolved. 6. Wash the empty filter paper with distilled water from the wash bottle. Collect the water in the 250-mL beaker containing the acid solution. Combine all the acid solution in one beaker. 7. Rinse the second beaker with 10 mL of distilled water and add to the acid solution. Retain acid solution for use in Part 5. Part 5: Precipitating Cu2+ ions as copper metal WARNING: Concentrated hydrochloric acid is corrosive and causes severe burns. Handle with care. Dilute and wash up spills with plenty of water. 1. In the hood, add 0.25 to 0.3g of magnesium metal to the beaker containing the blue-green solution of Cu2+ ions, and heat the solution to near boiling on the hot plate. 2. Using a glass stirring rod, agitate the solution to speed the precipitation of copper granules. Continue stirring and heating until the solution is colorless. 3. If bubbling stops but the solution is still blue, add additional magnesium to completely precipitate the copper and eliminate the Chemistry Department, University of Southern Maine Lab Procedure Page 6 of 8 blue color of the supernatant. Then decant the supernatant into a waste container. 4. Wash the copper metal in the beaker with two portions of 20 mL deionized water. 5. Allow the solids to settle and decant after each wash. 6. In the hood, carefully add small amounts of 6 M hydrochloric acid (HCl) to completely dissolve any remaining magnesium. 7. If bubbling stops, but silvery Mg is still present, add 1-2 drops more 6 M HCl. 8. Allow the copper granules to settle, and then decant the supernatant liquid into a waste container. Wash the copper granules three times with 25 mL of warm deionized water. 9. Pre-weigh a piece of filter paper and label as to period and tem number. 10. Set up a filter apparatus as before and filter the copper solid from the supernatant liquid. 11. Place filter paper in fume hood under the lamps and allow drying at least 48 hours. 12. Determine if the filter paper/copper solid is dry, if it is mass and calculate the resultant amount of copper. If not, let it dry for another day. Chemistry Department, University of Southern Maine Lab Procedure Page 7 of 8 Use the percentage error calculation and determine the amount of copper recovered. Your true will be the original measured amount of copper wire. Your observed value will what you measured at the end of the lab. Chemistry Department, University of Southern Maine Lab Procedure Page 8 of 8