EXPERIMENT ELECTROCHEMISTRY (OXIDATION-REDUCTION) 14A Oxidation-Reduction Reactions of Elements and Their lons Oxidation is the process whereby electrons are lost by a chemical species (an atom, molecule, or ion). Conversely, reduction is the process whereby electrons are gained by a chemical species. Before electrons can be added to a chemical species, they must be removed from another chemical species; therefore, the processes of oxidation and reduction must occur together. The overall reaction is called an oxidation-reduction reaction or, in shorter form, a redox reaction You have already encountered a number of redox reactions in earlier exper- iments; for instance, reactions in which a metal reacts with an acid, giving pos- itive ions of the metal and hydrogen gas, The reaction between magnesium. and hydrogen ions to give magnesium ions and hydrogen gas is a good exam- ple of a redox reaction: ‘Mag(s) + 2H*(aq) + Mg*(aq) + H,(g) ‘The reaction consists of two distinct parts, which can be written as separate reactions, each involving electrons. These are called half-reactions. ‘Mg(s)_ > Mg?*(aq) + 2e7 (oxidation — loss of electrons) 2H(aq) + 2° H(@) (reduction — gain of electrons) The magnesium brings about reduction of H* to H,, so it is called the reducing agent. The H* brings about oxidation of Mg to Mg”* and therefore is called the oxidizing agent ‘The overall equation for the reaction is obtained by adding the equations for the two half-reactions in such a way that the electrons cancel out. (This may mean that one or both of the equations for the half-reactions must be multiplied by some number to make the electrons involved in the oxidation and reduction numerically equal.) Note that the oxidizing agent is the species which itself becomes reduced in the process and the reducing agent is the species which itself becomes oxidized in the process. Because the reaction pro- ceeds in the direction shown, it can be concluded that magnesium is a stronger reducing agent than H, and that H* is a stronger oxidizing agent than Mg”". In Part I of this experiment, you will examine reactions between metals and aqueous solutions of ions of other metals. Then in Part Hl, you will investigate some reactions between free halogen molecules and aqueous solutions of ions of other halogen elements. From your results you will be able to arrange the equations for the reduction half-reactions in sequence from the strongest oxi- dizing agent to the weakest. This arrangement will show that any oxidizing agent on the left will be able to react with any reducing agent on the right that is lower on the list. Such a list can be expanded with other experimental results and is very useful for predicting whether or not a reaction will proceed. 230 Experiment 148 Copying the experiment is prohibited. ©8MG Lab Books Ls. ee| OBJECTIVES 1. to investigate various combinations of metals with metal ions and dis- . cover which combinations undergo redox reactions 2, to investigate various combinations of the halogen elements chlorine, bromine, and iodine with the felated halide salts and discover which combinations undergo redox reactions 3. to listall the reduction half-reactions studied in such a way that the halo- gen elements and metal ions are arranged in decreasing order of strength as oxidizing agents SUPPLIES Equipment 20 test tubes (13 mm x 100 mm) test-tube rack steel wool or emery paper water-soluble marker rubber stoppers (size 00) lab apron safety goggles Chemical Reagents 0.1M Cu(NO,), 0.1MZn(NO3) 0.1M MgwNO,), 0.1M PD(NO,)» small strips of copper, zinc, ‘magnesium, and lead 0.1M NaCl 0.1M NaBr 0.1M Nal chlorine water bromine water iodine (50% ethanol solution) . n-heptane : 0.1M AgNO, and silver metal strips . (for instructor demonstration) PROCEDURE | Part |: Reactions between Metals and Metal lons (Cu, Zn, Mg, Pb, and Ag) 1, Put on your lab apron and safety goggles. 2, Obtain 3 small strips of each metal (Cu, Zn, Mg, and Pb) and rub each P with steel wool or emery paper to remove surface corrosion and reveal | the shiny surface underneath, Rinse with water. 3. Place the strips in separate 13 mm x 100 mm test tubes (12 in all) and use uur water-soluble marker to identify which metal is in each tube each of the 3 test tubes containing copper metal, add in turn about 3 mL (one thitd of a test tube) of a 0.1M solution of the nitrate of each of the other metals. (It is not necessary to try to react copper metal with its own nitrate, Cu(NO,)..) 5. Repeat with the other three metals, until you have all 12 possible combi- nations of metals with the nitrates of the others. Label all the combinations. . Record your observations in ‘Table 1 in your notebook. (©SIG Lab Books Lid. Copying the experiment is prohibited Sy XSF The metal nitrate solutions used in this experiment are poisonous. Do not get any in your mouth and do not swallow any. Experiment 4a 231i Your instructor will display an additional 8 combinations, consisting of silver metal (Ag) with nitrates of Cu®, Zn?*, Mg, and Pb**, and 0.1M AgNO, with each of Cu, Zn, Mg, and Pb, Observe which combinations show evidence of reaction and record your results in Table 1 7. In some of the combinations you prepared, a metal will be produced from the positive lon in solution, Note that the metal may be very finely divided and may therefore appear as a black powder. The color and lus- ter of metals are apparent only when the crystals formed are somewhat larger. Any change in the appearance of a metal or a solution will there- fore indicate that a reaction has occurred. Some reactions are slower than others are, so leave the test tubes in the rack and take a final look at the results after doing Part 11 Part Il: Reactions Between Halogens and Halide lons Le vomine and iine sottions which ar sed and which may be produced CAUTION in this part of the procedure sometimes appear similar in color at certain con- J centrations, The purpose of Steps 1 and 2 in this part is to demonstrate a way y of distinguishing between the two substances Br, and T,. Note that no reaction The n-heptane used in occurs — the effect seen is simply a selective solubility for the Br, and I, out Part Il is highly of the aqueous phase into the n-heptane phase. flammable and its 1. Place 3 mL of bromine water, Br,(aq), in a test tube and add 1 mL of vapors are hazardous if inhaled. Make sure there are no open n-heptane. Stopper and shake vigorously. Note that the heptane and the water solution do not mix. You will be able to tell which is the heptane 1e. Note the color of ‘lames in the layer by observing which layer has the smaller vol laboratory. Avoid the n-heptane and record it in Table 2 in your notebook. See 2. Repeat Step 1 with 3 mL of the 1, in 50% ethanol solution. Again reco: Do not get any on your skin. If you do, the color of the heptane layer. call your instructor. 3. To 3 ml of 0.1M Nabr and 3 ml. of 0.1M Nal in separate test tubes, add 1 mL of chlorine water, Observe any changes, then to each add 1 ml. of YY heptane, stopper the tube, and shake. Observe the color of the heptane layer and record what you see in Table 2. ww 4, Repeat Step 3, but use 1 mL of bromine water with 0.1M NaCl and 0.1M Nal The solutions of 5. Repeat Step 3, but use 1 mL of iodine solution in 50% ethanol with 0.1M chlorine water, NaCl and 0.1M NaBr. ee 6. Now make final observations of the results for Part [to check for any fur- iodine in 50% ethanol are very poisonous and corrosive. Avoid breathing their fumes. Do not get any on your skin. If you do, ther changes. Before leaving the laboratory, wash your hands with soap and water. rinse your skin with REAGENT DISPOSAL the sodium thiosulfate solution Part I: Return all solutions and metals from Part I to the designated container which your instructor DO NOT pour the solutions or the small pieces of metal down the sink. has available for any such emergencies, Part Il; Pour the solutions from Part II Into the designated beaker, which con- ‘then with plenty tains a solution of sodium thiosulfate, The sodium thiosulfate can react with, of water. unchanged chlorine, bromine, and iodine, which could otherwise be hazardous. 232 experiment 144 Copying the experiment is prohibit. ©5MG Lab Books Lid_ POST LAB CONSIDERATIONS Note that for every combination of element and ion there is a combination in, which the element and ion are reversed. For example, you will have the Cu/Zn?* combination and the Zn/Cu”* combination. Only one of these will react. If the reaction occurred, the conclusion is that the metal ion in the reactant (or in Part JL, the halogen molecule) is a stronger oxidizing agent than the other metal ion (or halogen molecule) produced during the course of the reaction. EXPERIMENTAL RESULTS Part |: Reactions Between Metals and Metal Ions (Cu, Zn, Mg, Pb, and Ag) ‘Table 1 fama Reactants (Metal+ | Gpcervations Reaction Jon that is the Stronger Metal Ion) (ies or No) Oxidizing Agent Mg + Cu Mg + Zn Mg + Pb Ag+ Cu ‘Ag+ Zn™* Ag + Mg Ag+ Pb cus age zn+ Ag Mg + Ag™ Pb + Ag’ SMG Lab Books Lid Copying the experiment is prohitited Experiment 44-233 ae:Reactions Between Halogens and Halide Ions Halogen Color of aqueous layer Color of n-heptane layer Bromine 4 vou 7 Iodine | Observations Reactants (Halogen + | Reaction Halogen that is the Halide Ion) (Yes or No) | Stronger Oxidizing Agent Cl, +Br Ch+r Br, +C Br +P ye < i +c ANALYSIS OF RESULTS 1, Write a balanced equation for the reduction half-reaction of each metal ion. Then arrange the equations in order of decreasing strength of these fons as oxidizing agents. (This is the same as saying “decreasing ease of reduction of the ion.") Write a balanced equation for the reduction half-reaction of each halo- gen molecule and then arrange the equations in order of decreasing strength of these molecules as oxidizing agents. 3. Other experiments have determined that Ag* is a stronger oxidizing agent than [,, but a weaker oxidizing agent than Br. Also, Ip is a stronger oxidizing agent than Cu’. Using this information, put all the half-reac- tion equations together in one list, from strongest oxidizing agent to weakest 4, For every instance in which a reaction did occur, write the balanced over- all redox equation by adding together two half-reaction equations, one for the oxidizing agent and one for the reducing agent (by reversing one from the list). In some instances you will have to multiply the half-reac- tion equation by an appropriate number in order to make the number of electrons equal, so that they cancel out. 234 Experiment 144 Copying the experiments probibite. SMG Lab Books Lis es esFOLLOW-UP QUESTIONS 1. On the basis of the results of this experiment, state whether you would expect a redox reaction to occur spontaneously in each of the following situations. Give the balanced equation if a reaction does occut. a. Br, and Pb b. rand Zn © Cl, and Cu d 1, and Mg 2. ‘What would happen to sterling silver jewellery (an alloy of 92.5% Ag and 7.5% Cu) if it were exposed to fumes of bromine? 3. Some laboratory waste pipes used to be made of lead. What would hap- pen if waste Cu solutions were allowed to go down such pipes? 0 remove Cu wastes from a solution before discharging it down the sink, steel wool (an alloy of iron) can be added. This produces copper ‘metal on the steel wool. The solid copper can then be disposed of safely. Is iron a stronger or a weaker reducing agent than copper? CONCLUSION 1. State whether halogens are generally oxidizing or reducing agents and give the periodic trend you observed, ate whether metals are generally oxidizing or reducing agents (©5MG Lab Books Lid Copying the experiment is prohibited Expacment 144 235