Chemistry Laboratory

Instructor: Huynh Kim Lam

EXPERIMENT # 3

REDOX TITRATION WITH KMnO4

I. INTRODUCTION In an oxidation-reduction or redox reaction, there occurs an exchange of electrons between to reactants, resulting in the changes of oxidation number. The substance that gains electrons is said to be reduced, therefore, it is called the oxidizing agent. The substance that loses electrons is called the reducing agent, thus it is oxidized. One gram equivalent weight (GEW) of oxidizing agent is the weight that gains 6.02x1023 electrons and one gram equivalent weight of reducing agent is the weight that loses 6.02x1023 electrons. According to the definition of gram equivalent weight, one GEW of oxidizing agent reacts with one GEW of reducing agent. GEWox = GEWed

Consider the reaction of potassium permanganate with oxalic acid (H2C2O4) in the presence of excess sulfuric acid. The balanced molecular and net ionic equations are: 2KMnO4 + 5H2C2O4 + 3H2SO4 10CO2 + K2SO4 + 2MnSO4 + 8H2O 2MnO4 + 5H2C2O4 + 6H+ 10CO2 + 2 Mn2+ + 8H2O The oxidation number of Mn in MnO4 is +7 while it is +2 in Mn2+. Hence, each Mn undergoes a change in oxidation number of five. Since each formula unit of KMnO4 contains one Mn, and each Mn gains five electrons, one mole of KMnO4 is five gram equivalent weights in this reaction. As a result, KMnO4 produces 5 moles of electrons per mole of KMnO4 or has five equivalents per mole of KMnO4. Thus, the gram equivalent weight of KMnO4 in this reaction is 31.60 grams.

GEW of KMnO4 =

158.0 g 1 mole 31.60 g = 1 mole 5 eq eq

The oxidation number of carbon in H2C2O4 is +3 while it is +4 in CO2. Thus each carbon undergoes a change in oxidation number of one. However, each formula unit of H2C2O4 contains two carbons, and since each carbon loses one electron, one mole of oxalic acid is two gram equivalent weights in this reaction. Consequently, H2C2O4 produces 2 moles of electrons per mole of oxalic acid or has two equivalents per mole of oxalic acid. The gram equivalent weight of H2C2O4 is 45.0 grams GWE of H2C2O4 = 90.0 g 1 mole 45.0 g = 1 mole 2 eq eq

Summer 2011 Revision 4/3/2012

Chemistry Laboratory

Instructor: Huynh Kim Lam

In this experiment, you will prepare an approximately 0.05N KMnO4 solution and standardize this solution by titrating against a standard solution of H2C2O4 (primary standard). Then the standardized KMnO4 solution (secondary standard) will be used to determine the concentration of unknown oxalic acid solution and unknown Fe+2 solution. For redox titrations, the number of equivalents of oxidizing agent must be equal to the number of equivalents of reducing agent. For the reaction of KMnO4 with H2C2O4: eq of KMnO4 = eq of H2C2O4 Alternatively, this relationship can be expressed as follows: Voxidizing x Noxidizing = Vreducing x Nreducing Where V is the volume of oxidizing or reducing agents used in titrations And N is the normality of oxidizing or reducing agents. At the end of a titration, three of the four variables will be known and the unknown variable can be determined. II. LEARNING OBJECTIVES - Learn about the term of gram equivalent weight - Review of oxidation-reduction reactions - Standardize the concentration of KMnO4 solution and determine the oxalic acid normality. III. EQUIPMENT AND REAGENTS 1. EQUIPMENT One 50 mL burette One 100 mL graduated cylinder Three 250 mL beakers One 10 mL volumetric pipette Three 250 mL Erlenmeyer flasks One glass watch One funnel (small size) One stirring rod One medicine dropper Water bath 2. REAGENTS 0.05N KMnO4 (Potassium permanganate) 0.1N Oxalic acid (H2C2O4) 6N H2SO4 Distilled water Unknown concentration solution of KMnO4 Unknown concentration solution of H2C2O4 Unknown concentration solution of FeSO4 in H2SO4

Summer 2011 Revision 4/3/2012

Chemistry Laboratory IV. EXPERIMENTAL PROCEDUE

Instructor: Huynh Kim Lam

1. Prepare KMnO4 solution: (TA will prepare it for you but you have to understand the procedure) Weight 1.58g KMnO Transfer it to a 250-mL beaker with 100-mL of DW Mix the solution thoroughly by vigorous swirling Transfer the solution into a 250-mL volumetric flask and fill with DW Then transfer it to a dark brown bottle 2. Handling with burette: Clean the burette with distilled water Rinse it three times with 5 mL prepared KMnO4 solution. Discard the rinse solution. Fill the burette with KMnO4 solution and allow it to drain through the burette tip until no air bubbles remain in the tip. Record the burette reading before beginning the titration. Note: as the KMnO4 solution is dark color, read the burette at the top of the meniscus. 3. Standardization of prepared KMnO4 solution: Prepare 10 mL of standard oxalic acid solution into each of three 250 mL Erlenmeyer flasks. Add 40 mL of distilled water to each flask. Add 20 mL of 6N H2SO4 solution to each flask (fume hood). Warm the flasks in the water bath 85C 900C Titrate the hot solutions against the KMnO4 solution. Note: the KMnO4 solution should be added very slowly initially. Endpoint for this experiment refers to the titrate volume needed to keep the faint pink color throughout the stirred solution for at least twenty seconds. Record the burette reading and calculate the normality of the KMnO4 solution. 4. Determination of unknown concentration H2C2O4 solution: Prepare 10 mL of unknown concentration solution of H2C2O4 into each of three 250 mL Erlenmeyer flasks. Add 40 mL of distilled water to each flask. Add 20 mL of 6M HSO solution to each flask (fume hood). Warm the flasks in water bath 85C - 90C. Titrate the hot solutions. Calculate the normality of the unknown concentration H2C2O4 solution; determine the average and the standard deviation. 5. Determination of unknown concentration FeSO4 solution: Prepare 10 mL of unknown concentration solution of FeSO4 solution into each of three 250 mL Erlenmeyer flasks. Add 40 mL of distilled water to each flask. Add 20 mL of 6M HSO solution to each flask (fume hood). Warm the flasks in water bath 85C - 90C. Titrate the hot solutions. Calculate the normality of the unknown concentration H2C2O4 solution; determine the average and the standard deviation.

Summer 2011 Revision 4/3/2012

Chemistry Laboratory

Instructor: Huynh Kim Lam

Lab structure
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4 6
Chemical

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Summer 2011 Revision 4/3/2012