LAB 3: DETERMINATION OF AN EMPIRICAL FORMULA This lab requires a lab report. You will work with a partner for this lab. I Introduction To find the empirical formula of a compound, we need to find the moles of each element in a given sample of that compound. For example, we might resolve a 40gram sample into its elements and obtain about 23 grams of sodium, 16 grams of oxygen, and 1.0 gram of hydrogen. Dividing by the molar mass of each element, we find the sample contains 1 mole of Na, 1 mole of O, and 1 mole of H. 23 g Na 16 g O 1.0 g H 1.0 mol Na 1.0 mol O 1.0 mol H Taking the ratio of these three elements, we determine the compound’s empirical formula to be NaOH: we probably have sodium hydroxide. 1.0 mol Na 1.0 mol O 1.0 mol H Na1O1H1 Usually, however, the numbers are not so simple, not to mention the question that keeps nagging you: how do we determine the mass of each element in the first place? In this experiment, you’ll do just that. Over the next two days, we will use a three-step process to determine the empirical formula of a hydrated copper salt, CuxClyzH2O (you will recall that, although the chloride ion always has a charge of –1, the charge of copper ions can vary between +1 and +2). In the first step, we will dehydrate the sample, turning the enchanting bluegreen crystals of the hydrate into dehydrated crystals of an ever-so-lovely shade of tobacco brown (not that you minors would know what tobacco looks like). From the mass lost, we will be able to determine the moles of water lost; this will later be useful in determining z in the mystery formula above. In the second step, we will reduce the copper ions (which are dissolved in solution) into copper atoms (which are solid and are not dissolved in solution). After dissolving the copper chloride in water, we will add aluminum foil to the solution, causing the aluminum to precipitate out the copper in a fairly exothermic single replacement reaction, as shown by the following unbalanced equation: Al (s) + Cuy+(aq) Al3+(aq) + Cu(s) By measuring the mass of copper metal produced, we can determine the moles of copper present in the sample. This will help us in determining the x in the mystery formula. Finally, after we have subtracted the masses of water and copper, we can determine the mass and moles of chloride present in the sample. This will allow us to calculate y in the mystery formula. At last, with the moles of water, copper, and chloride in the initial sample, we can find the simplest whole-number ratios of the three and thus deduce the empirical formula of our mysterious hydrated copper chloride compound. Equipment and Reagents Evaporating dish 100-mL beaker Bunsen burner Ring stand with clay triangle Stir rods, etc. Filtering apparatus Analytical balance Hydrated copper chloride, CuxClyzH2O(s) Aluminum foil, Al(s) Hydrochloric acid, 6 M HCl(aq) Ethanol, 95% CH3CH2OH(aq) ! Warnings! The 6 Molar hydrochloric acid is extremely corrosive. Use goggles and apron(s). Ethanol is very flammable. Keep away from open flames and sources of heat. Procedure This lab is straightforward and excellent results can be obtained if you are careful and thorough. When transferring substances, be sure to get every last drip, drop, and scrap! Part 1: Determining the Moles of Water Set up your lab notebook. Using the same technique we practiced as a class, determine the mass and moles of water present in about 1 gram of the hydrated copper chloride. To do this, dry an evaporating dish, record its mass, record the mass of your hydrated copper chloride sample, and heat until the aforementioned blue-tobrown color change is complete. Use gentle heat and stir frequently with a glass stir rod. Be careful that none spatters out. It’s easy to tell when the end product is reached because it will be a uniform brown color. Re-weigh the dish and nowdehydrated copper chloride. Be sure to record all necessary data, procedures, and observations. Part 2: Determining the Moles of Copper Transfer the dehydrated product to a 100-mL beaker and rinse the residue from the evaporating dish into the beaker with distilled water. Swirl the beaker to dissolve the crystals; the solution should return to a pleasant blue-green hue as the copper ions are rehydrated. Add more distilled water if necessary until all of the crystals are dissolved. Record your observations and procedure. Measure out about 0.25 g of aluminum foil and tear it into small pieces (smaller pieces make the ensuing reaction go faster). Drop these pieces into your solution. Sit back and enjoy the show after recording your observations. The brown substance forming is the fine particles of copper precipitating out. Our goal is to measure the mass of solid copper only, so first we must get rid of the excess aluminum. Once the reaction is finished (how can you tell when all the copper ions are gone?), carefully add several mL of 6 M HCl (CAREFUL!). If the reaction between aluminum and HCl stops and there are still visible aluminum chunks, add HCl and repeat as necessary until all of the aluminum is gone. At this point, you have pure, solid copper setting in a solution of aluminum chloride. Filter to isolate the pure copper metal, being sure to weigh your fluted filter paper in advance. Once the copper has filtered, “wash” the copper with at least two ~5 mL portions of distilled water. Then rinse with ~10 mL of 95% ethanol. Carefully set your filter on a paper towel labeled with your name and allow to dry overnight. STOP HERE ON DAY 1. The next day, weigh your copper metal and perform the necessary calculations to determine the empirical formula of your hydrated copper chloride compound. Data and Calculations (to be recorded on your lab Data Sheet) Procedure used Mass of hydrated sample and dehydrated sample (and any necessary measurements needed to calculate those) Observations of dehydration Observations of reactions Mass of dry copper product Mass and moles of water, copper, and chloride in sample Empirical formula of compound ? Questions to Answer 1) Oops! In Part 2, suppose you accidentally dissolved the copper chloride in 100 mL of water instead of 10 mL. The voice on the left side of your head says you screwed it up and need to start over; the voice on the right side of your head says it doesn’t matter, just keep on going. Which of your voices should you listen to? Why? 2) Why do we use hydrochloric acid to react with the excess aluminum metal instead of, for example, nitric acid? (Hint: Think back to Lab 2 and the sterling silver necklace)