Percent Composition and Empirical Formula Based on an experiment written by Dr. Anne Glenn Mr. David MacInnis, Jr. Dr. Rob Whitnell Guilford College Purpose The purpose of this experiment is to determine the percent copper in a compound containing only copper and chlorine by reducing the copper(II) ions to metallic copper with zinc by the following oxidation (redox) reaction: 2+ 2+ Cu (aq) + Mg(s) → Cu(s) + Mg (aq) The solid metallic copper will be collected by filtration, washed, dried and weighed. You will then be able to calculate the mass percentages (percent composition) of copper and chlorine in the compound. From this you will be able to determine the empirical formula of your original copper containing compound. This experiment will demonstrate the technique of reducing a compound to its elements in order to determine its empirical formula. The Details Chloride-containing salts of copper are soluble in water. 2+ 1- CuClx(s) + H2O(l) → Cu (aq) + x Cl (aq) 2+( The aqueous copper(II) ion (Cu aq)) exhibits a characteristic blue color that can provide visual cues as to the extent of any reaction involving that ion. The copper(II) can then be reduced to elemental copper in an oxidation-reduction (or cation displacement) reaction as shown above. Any excess solid elemental magnesium can be removed from 2+ the flask by oxidizing it to Mg (aq) using an acid such as hydrochloric acid: 1+ 2+ Mg(s) + 2 H (aq) → H2(g) + Mg (aq) Assuming the initial mass of the copper-chlorine sample known, and assuming all of the copper from that sample is collected in the form of elemental copper, it is possible to calculate the mass of chlorine in the original sample, and, in turn, the percentage composition of those two elements in the original sample. It is also possible to convert the masses of copper and chlorine to the number of moles of those two elements in the original sample, and, in turn, the mole ratio of chlorine to copper in the compound. That mole ratio can be easily converted to the empirical formula for the compound. Safety Information 6M HCl is a strong acid. Gloves are recommended when handling it. If you spill some on you wash it off immediately with a large quantity of water. Large spills in your laboratory area should be treated with sodium bicarbonate. Be sure to ask your lab instructor for assistance. Ethanol and acetone are extremely flammable. Do not use any open flames during this experiment. Equipment Two 250 mL beakers 100 mL graduated cylinder Two stirring rods with rubber policemen (scrapers) Filter paper Two funnels Two 250 mL flasks for collecting the copper filtrate Vial of copper-chlorine compound Magnesium turnings (≈ 1.5 g) Dropper bottle of 6M HCl (10 to 15 mL total) Dropper bottles of ethanol and acetone Procedure 1. Obtain an approximately 4 g sample of the copper chlorine compound. Divide the sample between two clean 250 mL beakers (tared and labeled), recording the mass of the compound each time. 2. Place a clean stirring rod with rubber policemen in each beaker and leave them there. Add approximately 50 mL of distilled water to each beaker and then add 2 mL (approximately 40 drops) of the 6M HCl. Stir until the compound has completely dissolved. If solid residue remains after 5 minutes of stirring add 6M HCl in 2 mL increments stirring 1 min. each until the solid has dissolved. Be sure to record the color of these solutions. 3. Add approximately 0.7 g of magnesium turnings and stir well. Let the mixture stand with frequent stirring for approximately 15 min. after which there should be a deposit of metallic copper on the bottom of the beaker. The solution should be colorless and the evolution of hydrogen gas should be slow. If the solution becomes cloudy during this time add 6M HCl drop by drop with stirring until the solution clears. 4. Label with pencil and weigh two individual pieces of filter paper. 5. To destroy any excess metallic magnesium that might be present in the solution add 2 mL of 6M HCl to each beaker and stir. If hydrogen gas is not evolved you probably did not have enough magnesium present to reduce all the copper. In this case you should add another 0.2 g of magnesium to the solution and stir for 5 minutes. In either case when the gas evolution becomes slow add about 0.5 mL of 6M HCl to each beaker and stir until no more gas is evolved. 6. Filter each solution through its own weighed filter paper. Use your rubber scraper to ensure that you transfer all the copper solid to the filter (be sure to rinse all the copper from the beaker into the filter paper with distilled water as required). Wash each filter with approximately 100 mL of distilled water to clean the copper precipitates. 7. Wash the filters containing the solid copper with 10 mL of alcohol to remove all the water. Wash again with 10 mL of acetone to completely remove the water and spread the filter papers on a paper towel and allow them to dry. The solution in your flask is known as the filtrate. For this lab it can be washed down the sink with plenty of water. 8. When the filter papers containing the recovered elemental copper have completely dried, weigh each one. User your data to calculate the mass percentages of copper and chlorine in the original sample. Use this information to determine the empirical formula of the compound. After you are confident that you have collected and weighed the copper correctly, the solid copper and filter paper can be disposed of in the trash. Data Trial #1 Trial #2 Trial #3 Mass of empty beaker _______ _______ _______ Mass of beaker plus CuClx _______ _______ _______ Mass of clean, dry filter paper _______ _______ _______ _______ _______ _______ o Mass of filter paper plus dry Cu Calculations Please complete the calculations using Excel. Be sure to do all calculations in terms of cell addresses. Please name the file CuClx_AB where AB represent your first and last initials. Be prepared to submit the spreadsheet as required by your laboratory instructor. 1. Calculate the mass of elemental copper recovered in each successful reaction. 2. Calculate the mass of chlorine that had been combined with the copper in each successful reaction. 3. Calculate the percent by weight of copper and chlorine present in each trial. If these percentages are significantly different it may be necessary to do a third trial. 4. Calculate the number of moles of copper used in each successful reaction. Round the answer off to 3 significant figures. Use 63.55 gm as the mass of 1.00 mole of copper. 4. Calculate the number of moles of atomic chlorine that reacts with the copper in each successful reaction. Round the answer off to 3 significant figures. Use 35.45 gm as the mass of 1.00 mole of atomic chlorine. 5. From the results of calculations 3 and 4 determine the empirical formula for the compound. Use 3 significant figures in these calculations and round off answers to 3 significant figures. Divide the results of the calculations in 3 and 4 by the smaller of the two numbers. Convert these results into integers by either rounding or by multiplying both by the same integer. 6. The empirical formula for this copper chloride (CuClx) is _________________. Additional questions 1. In step three of the procedure, you added 0.7 g of magnesium metal to the solution containing the copper-chlorine compound. How many moles of magnesium is this and how does it compare to the number of moles of your copper chlorine compound? Why do you have to use so much magnesium? 2. What error would result if you did not add excess hydrochloric acid to dissolve the magnesium in the sample? 3. It is important to analyze what errors or other uncontrollable factors might have affected your results and how your results might have changed had these errors been corrected. For each of the following, state how the error affects the mass percentage of the copper in your compound and in turn the empirical formula. a. The original sample of the compound was wet. b. An impurity containing neither copper or chlorine was present in your sample of the compound. c. Not all of the excess magnesium was oxidized. d. The copper was not completely dry when you weighed it.