Determination of Iron by Redox Titration

Rachel Hofer February 3, 2012 Second Period Lab Partner: Nikki Shah

Pre-Lab Questions:
1. Another common analysis for iron is titration of iron(II) with potassium dichromate, K2Cr2O7. Divide the following reaction into half-reactions, balance the half-reactions, and combine the balanced half-reactions into the balanced overall equation for the reaction. Fe2+ + Cr2O72- + H+ Ox: [Fe2+ Fe3+ + e-] x 6 6Fe2+ 6Fe3+ + 6eRed: 6e- + 14 H+ + Cr2O722Cr3+ + 7H2O 6Fe3+ + 6e- + 2Cr3+ + 7H2O 6Fe2 + 6e- + 14 H+ + Cr2O726Fe2+ 14 H+ + Cr2O72Fe3+ + Cr3+ +H2O

6Fe3+ + 2Cr3+ + 7H2O

2. Use the internet to list several other uses of potassium permanganate (other than in the analysis or iron samples as in this experiment). Potassium permanganate can be used as a disinfectant and deodorizer, wastewater treatment (it neutralizes hydrogen sulfide), treatment for ulcers, and it is used in the synthesis of many organic compounds.

3. If 26.23 mL of potassium permanganate is required to titrate 1.041 g of ferrous ammonium sulfate hexahydrate, FeSO4(NH4)2SO46H2O, calculate the molarity of the KMnO4 solution. 1.041 g FAS x 0.026544911 mol FAS x = 0.026544911 mol FAS = 5.308922151x10-4 mol KMnO4 = 0.02024 M KMnO4

4. If a 2.893-g sample of an unknown containing iron requires 28.45 mL of the permanganate solution described in Pre-Laboratory Question 3 to reach the endpoint, calculate the % Fe in the unknown. .02845 L (.02024 M KMnO4) = 5.308922151x10-4 mol KMnO4 5.308922151x10-4 mol KMnO4 x 0.00287914 mol Fe x = 0.00287914 mol Fe

= 0.160799969 g Fe

x 100= 5.558% Fe

Data:
Standardization of KMnO4 solution
Sample 1 Mass of FAS taken Initial KMnO4 volume Final KMnO4 volume Volume of KMnO4 used Moles of iron present Moles of KMnO4 Molarity of KMnO4 solution 0.02267 M 0.0217 M 0.0231 M 0.0209 M 1.000 g 37.7 mL 15.2 mL 22.5 mL 2.550x10-3mol 5.100x10-4mol Sample 2 0.991 g 41.4 mL 18.1 mL 23.3 mL 2.53x10-3mol 5.05x10-4mol Sample 3 0.997 g 44.0 mL 22.0 mL 22.0 mL 2.54x10-3mol 5.08x10-4mol Sample 4 1.015 g 41.0 mL 16.2 mL 24.8 mL 2.59x10-3mol 5.18x10-4mol

Mean molarity: 0.0221 M

Analysis of Unknown #1
Sample 1 Mass of unknown taken Initial KMnO4 volume Final KMnO4 volume Volume of KMnO4 used Moles of KMnO4 present Moles of iron present Mass of iron present Percent of iron present 0.50 g 40.2 mL 28.6 mL 11.6 mL 2.56x10-4 mol 0.00128 mol 0.0716 g 14% Sample 2 0.50 g 35.0 mL 23.2 mL 11.8 mL 2.61x10-4 mol 0.00130 mol 0.0728 g 15%

Mean % iron present: 14%

Sample calculations:
Standardization of KMnO4 Solution: Sample 1
37.7 mL (initial KMnO4 volume)-15.2 mL (final KMnO4 volume) = 22.5 mL of KMnO4 used 1.000g FAS x = 2.5499146x10-3 mol FAS = 5.099829156x10-4 mol KMnO4

2.5499146x10-3 mol FAS x

= 0.0226659076 M KMnO4 = 0.0221 average molarity

Analysis of Unknown #1: Sample 1

40.2 mL (initial KMnO4 volume) - 28.6mL (final KMnO4 volume)= 11.6 mL KMnO4 used 0.0116 L x .0221 M KMnO4= 2.5636x10-4 mol KMnO4 2.5636x10-4 mol KMnO4 x 0.0012818 mol Fe x = 0.0012818 mol Fe = .07158853 g Fe

x 100= 14.317706% Fe = 14% Fe

Post Lab Questions:

1. Typically, a solid iron unknown for titration is dried in an oven to remove absorbed water before analysis (the unknowns used in this experiment were dried before dispensing). How would the % Fe determined be affected if the unknowns had not been dried and had contained absorbed water? The percent of iron would not be accurate if the unknowns had not been dried and contained absorbed water. The absorbed water would have added excess mass to the sample which would have lowered the percent of iron.

2. For what purpose was sulfuric acid added to the iron samples before titrating? Sulfuric acid was added to the iron samples to provide the hydrogen ions that are required for the reduction of the permanganate ion.