CHEM 201 Study Guide - Final Guide: Redoxon, Volumetric Flask, Equivalence Point

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 “Acids and Bases” 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^–(aq) + 8 H⁺(aq) → 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) → 2 Fe²⁺(aq) + Zn²⁺(aq) (reduction of the Fe3+)

Zn(s) + 2 H⁺(aq) → 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 “Laboratory Techniques and Measurements,” 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.

pre lab questions:

I am unable to solve these questions due to a time constraint. I received help on part 1 of the unknown acid. Need help with the rest! I really appreciate it!

Lab: ACID-BASE TITRATION

Objective: To use titration to determine in Part 1, the concentration (molarity) of an unknown acid solution and in Part 2, the purity of a sample of KHP acid. Background: Titration is a volumetric technique used to determine the concentrations of solutions, molar masses of solids, and purity of samples. A titration inolves the addition of a titrant (a solution of known concentration) to an analyte ( a solution of unknown concentration), or vice versa, using a piece of glassware called a burette. The titration is carried out until it reaches an equivalence point (the exact point at which the reaction between the two solutions is complete). A chemical indicator is often used to aid in the identification of the equivalence point. An indicator changes color upon reaching the equivalence point of endpoint. Since we will be carrying out an acid-base titration, the indicator must change color upon reaching the endpoint at a specific pH. An example of such an indicator is phenolphthalein, which changes from colorless to pink near the equivalence point when pH approaches 7. It should be noted that the indicator selected is dependent upon a given titration, so that the observed color change is close to the ideal equivalence point. Once the titration is completed, we can use the volumes measured for each solution, as well as the concentration of the titrant, to determine the concentration, molar mass, or purity of the unknown analyte. Procedure Note: During lab, record all measurements and data in a clearly labeled table. Part 1: 1. Obtain ~80mL of ~0.1M of base (sodium hydroxide, NaOH) into a labeled beaker. Make sure to report the actual concentration from the bottle. 2. Obtain ~25mL of unknown acid into a second labeled beaker. Record whether your acid is monoprotic, diprotic, or triprotic. 3. Using a funnel, or carefully pouring, fill the burette with sodium hydroxide NaOH. Make sure a labeled waste beaker is under the buretter to catch any drippings. Rinse your burette by filling it with ~5-10mL of NaOH. Turn the knob to let ~2 mL out the tip into the waste beaker. Make sure your waste beaker is under the burette to catch any drips. Next, turn the Burette upside down and pour the remaining NaOH into your waste beaker while twisting the burette to coat the inside with NaOH. 4. Fill your burette with sodium hydroxide. Turn the knob to fill the tip of the burette with NaOH. Record the initial volume to the correct number of significant figures. 5. Using a volumentric pipette, transfer 10.00 mL of your unknown acid into the Erlenmeyer flask. 6. Add 3 drops of pH indicator and magnetic stirrer to the Erlenmeyer. 7. Under the burette, place the Erlenmeyer on a hot plate and turn on the stir knob. Heat should be off. 8. Titrate the unknown acid until the solution turns pink and remains pink. 9. Record the final volume on the burette to the correct number of significant figures. 10. Repeat (4) to (7). Pre-plan the whole lab and who will do which task. MY RESULTS: PART 1 The actual concentration of NAOH is 0.5939, 80 mL Initial Final 24.9 mL 44.5mL 26.1 mL 45.57mL PART 2 Impure KHP (SAMPLE B ) Only Paper: 0.280 g Impure KHP Mass: 0.526 g Initial volume: 22.30 mL + water +26.10 mL Final Volume: 26.80 mL QUESTIONS: 1. Calculate the concentration (molarity) of your unknown acid. 2. Calculate how many grams in your impure KHP sample was indeed KHP. 3. Calculate the percent (by mass) KHP in the sample. Part 2: 1. What would happen to the final result( state what the final result is ) if the tip of the burette was not filled when reading the initial volume? 2. What would happen to the final answer if you used Ca(OH)2 instead of NaOH and DID NOT know it? 3. What would happen to the final result if the Erlenmeyer flask was contaminated with other types of acid? 4. Recalculate the concentration of your unknown acid if it was given as a diprotic acid. 5. Draw a molecular level picture (showing Na+, H+, OH-, H2O, etc...) of what is in your beaker before, at half point, at equivalent point, and at end point of the titration. Part 3: 1. What would have happened to the final result if the impurity in the sample was also acidic? 2. What would have happend to your final result if you used ~25mL of water to dissolve the solid acid instead of 20mL? Summary data: Create a clearly labeled table of all your final data results for each run, and athe average of multiple runs. Part 1: Unknown #, Vol base, M base, Vol acid, M acid. Part 2: Sample #, % KHP (purity)