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Chem 151L, Spring 2013 Expt. 6.

Estimation of Iron
As with all redox reactions, the number of electrons delivered is always equal to the number of electrons taken up. The reaction must therefore be designed to produce the analyte in an appropriate oxidation state, followed by titration with a standardized oxidizing or reducing agent. The neutral point is characterized by a large jump in electrical potential, just as acid/base titration endpoints are characterized by a rapid pH change. Consequently, a greater difference of standard potentials gives greater titration accuracy. Standardize the Titrant: While waiting for the unknown iron to reduce (see below), set up a burette with ~ 25 mL potassium dichromate titrant. Accurately weigh out ~ 1.0 g Fe(NH4)2(SO4)26H2O and dissolve in 100 mL distilled water. Add 12 mL of 3 M H2SO4, 5 mL of 85% H3PO4 and enough distilled water to bring the volume to ~ 150 mL. Add 8 drops of the indicator diphenylamine sulfonate and titrate with the potassium dichromate until the solution assumes a murky bluish-green or gray-green tint. Then add the dichromate drop-wise, maintaining an interval of a few seconds between each drop and gently swirl the flask. Keep titrating until the addition of one drop causes the formation of an intense violet color and permanently remains after agitation. Balance the following reaction and calculate the molarity of the potassium dichromate solution: [1] Fe2+ + K2Cr2O7 Fe3+ + K+ + Cr3+ Quantification of Iron in an Unknown Solution: The unknown sample is initially dissolved in acid and is present as Fe3+ in solution. The iron in the unknown sample must first be quantitatively converted to Fe2+ prior to carrying out reaction 1. The reduction to Fe2+ is affected by production of nascent hydrogen (as in Expt. 4). Pipet 10 mL of the unknown solution of ferric salt into a 500 mL Erlenmeyer flask. Add 1 mL conc. HCl (12 M), mix in 2 g of Zn metal (30 mesh, not mossy Zn) and immediately cover with a watch glass. Wait 5 min, periodically swirling the mixture gently. Add a second 1 mL portion of conc. HCl, and repeat treatment. Finally, add a third 1 mL portion and repeat. The faint yellow color of the solution should now be absent. Add 20 mL of 3 M H2SO4 and swirl occasionally until the last particle of zinc is consumed and evolution of hydrogen has ceased (the black speck impurities from the zinc release no gas and can be ignored). Rinse the watch glass, draining into the flask and also rinse down the internal walls of the flask. Add 5 mL of 85% H3PO4 and enough distilled water to bring the volume to ~ 150 mL. Add 8 drops of the indicator diphenylamine sulfonate and titrate with the K2Cr2O7 as before. Repeat three times to increase accuracy and determine precision. Report the average and standard deviation of the amount of iron in your aliquot and the molarity of the unknown solution. Questions: 1) Write balanced chemical equations for all the half reactions and the overall equation. Comment on the reduction potentials for each half reaction. 2) Discuss the role of pH as well as the specific reductant in the reaction. 3) How does the indicator detect the oxidation of the iron? Hint: see Kaufman, S.; Devoe, H. J. Chem. Ed. 1988, 65, 183-184.