Using the balanced equations given below, determine the overall molar ratio between aqueous oxygen and thiosulfate. Using the known concentration and added volume of sodium thiosulfate solution along with this molar ratio, it is possible to calculate the amount and concentration of dissolved oxygen in the original sample.

Determination of Dissolved Oxygen. Our determination of dissolved oxygen relies on several coupled reactions. Ultimately, the oxidation of manganese by dissolved oxygen drives oxidation of iodide to iodine, which is titrated using the iodine-reducing agent sodium thiosulfate. The water sample is first treated with a manganese(II) solution and a solution of potassium Mn2+(aq) + 2 OH-(aq) â Mn(OH)2(s) oxygen dissolved in the water oxidizes a portion of the manganese( hydroxide to manganese(ID hydroxide. (Note that dissolved oxygen is the limiting reagent throughout these reactions.) To dissolve the manganese(III) cations back in the water completely, a small amount of sulfuric acid is added--the acid protonates the hydroxides, allowing the freed manganese(I) ions to return to solution. 4 Mn(OH)2(s)-O2(aq) + 2 H20() â 4 Min(OH)3(s) 2 Mn(OH)3(s) + 3 HSO4(aq) â 2 Min'"(aq) + 3 SO42-(ag) + 6 H20() Iodide now enters the picture, as the newly dissolved manganese(II) ions have the ability to oxidize iodide. Dissolved molecular iodine forms, producing a yellow-brown solution. Iodide remaining in solution coordinates to the newly produced iodine, yielding the triiodide ion which turns blue in the presence of dissolved starch. L(aq) + rag) â 13-(aq) Finally, sodium thiosulfate solution is added dropwise to the mixture until all of the triiodide has been reduced back to iodide. At this point, the blue color of the starch-triiodide solution will disappear, leaving a colorless solution.

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INTRODUCTION

Many transition metal cations can have more than one possible charge (Worksheet 1). Differently charged species of the same element can have different chemical and physical properties. Knowing the charge can allow separation of the different ions based on their properties. For example, Cu²⁺ is blue and stable in solution, while Cu⁺ is colorless and reacts with oxygen. Hemoglobin contains iron as Fe²⁺, but it is inactive at binding oxygen when the iron gets oxidized to Fe³⁺. There are many similar situations in which it is important to always properly indicate charges of ions.

This laboratory experiment uses the difference in chemical properties of Fe²⁺, iron(II), and Fe³⁺, iron(III), to quantify the amount of each present in a solution of unknown concentrations of each. You will first determine the amount of iron(II) in your sample by titrating with a reagent that does not react with iron(III). You will then titrate a second sample after converting all the iron(III) to iron(II) in order to determine the total iron present. The percent composition of Fe²⁺ in the unknown mixture will be calculated.

BACKGROUND

The concentrations of both iron(II) and iron(III) ions in a solution can be determined by titration with potassium permanganate. The reaction is an oxidation-reduction reaction, or redox, for short. A brief introduction to oxidation-reduction reactions is given in the background of the âAcids and Basesâ experiment. The permanganate ion effectively oxidizes iron(II) to iron(III) in an acidic solution while being reduced to manganese(II) ion. The balanced net ionic reaction is:

5 Fe²⁺(aq) + MnO4^â(aq) + 8 H⁺(aq) â 5 Fe³⁺(aq) + Mn²⁺(aq) + 4 H₂O(l)

Iron(III) is not oxidized by the permanganate ion, and thus does not react. Thus in order to determine the concentration of iron(III) ions, they must first be reduced to iron(II) ions. Zinc metal is used as the reducing agent, also under acidic conditions.

Zn(s) + 2 Fe³⁺(aq) â 2 Fe²⁺(aq) + Zn²⁺(aq) (reduction of the Fe3+)

Zn(s) + 2 H⁺(aq) â Zn²⁺(aq) + H₂(g) (a side reaction that oxidizes excess Zn)

The Zn2+ formed does not interfere with the subsequent titration because Zn2+ is not oxidized by permanganate. Notice that converting all the iron(III) to iron(II) means that the total iron concentration ([Fe2+] + [Fe3+]) is titrated, not just the iron(II) originally present.

Techniques

This is a lab will utilize several of the techniques introduced in the experiment âLaboratory Techniques and Measurements,â the procedures for which are given in Appendix B. Poor laboratory technique and misuse of the glassware will result in poor data results, which will affect the grade you receive on the laboratory report. In order to use your time efficiently in lab, review how to properly:

rinse glassware prepare a standard solution use a volumetric pipette

weigh by difference set up and use a burette use a graduated cylinder

heat samples on a hot plate

Analysis of Iron by Oxidation-Reduction Titration

This lab uses the common quantitative technique of titration. The only difference between the titration you will be doing in this lab and that done in the Molar Mass of a Known Acid lab is the type of reaction used: this lab will use a redox reaction in place of the acid-base reaction performed in the previous experiment.

In order to determine the concentrations of iron(II) and iron(III) ions in a solution containing both ions, two portions of the same sample must be titrated separately. This first titration will determine only the iron(II) concentration. A second sample will be treated with zinc metal in order to reduce the iron(III) to iron(II). The resulting solution will be titrated with potassium permanganate. The result of this titration will give the total iron concentration in the sample. The difference between the first and second titration is the equal to the iron(III) concentration.

In this titration, potassium permanganate serves as its own indicator. The intense purple color of the permanganate solution becomes colorless when the permanganate is reduced to manganese(II). Thus, as iron(II) is oxidized with the addition of the permanganate solution from the burette it will impart a purple color that will fade. However, once there is no iron(II) left in solution a faint purple color will remain, marking the endpoint of the titration. This color can be slightly altered by the presence of iron(III), which is yellow in solution. Remember that iron(III) is generated by the reaction between iron(II) with permanganate, increasing the yellow appearance of the solution and which can interfere with the detection of the endpoint. Phosphoric acid is added to help minimize this effect.

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