EXPERIMENT 4 STANDARDISING A SOLUTION OF AN IRON(II) SALT USING POTASSIUM MANGANATE(VII)

In this experiment you are going to investigate an iron(II) compound. In the main experiment you will carry out a redox titration using potassium manganate(VII) . You are provided with three chemicals. D is a solution of potassium manganate(VII), KMnO4, containing 3.00 g dm-3 of solid E is the iron (II) compound. Dilute sulphuric acid In solution, the reaction is as follows: MnO4 + 5Fe2+ + 8H+ Mn2+ + 5Fe3+ + 4H2O From the equation: MnO4 5Fe2+

Procedure Weigh the empty bottle provided. Add 8.9 to 9.0 g of the iron (II) compound E. Reweigh the bottle + its content Tip the entire contents of the bottle into a beaker, and weigh the empty bottle. Record all your weighings in the space provided. Dissolve the solid E in a mixture of about 20 cm3 of dilute sulphuric acid and 80 cm3 of distilled water. Stir the mixture. When all the solid has dissolved, make up the solution to exactly 250 cm3 in a volumetric flask. Mix the solution thoroughly before use. Pipette 25.0 cm3 of the iron(II) solution into a conical flask and add about an equal volume of 1.0 mol dm-3 sulphuric acid using a measuring cylinder. Titrate with solution D from a burette until a permanent pink colour is observed. Repeat for consistent results. Question 1 Why does this titration not require an indicator ...KMnO4 acts as the indicator. Mn2+ is colourless. At end point there is a slight excess of MnO4-. and the solution appears slightly pink

In the space below record all the data collected in a suitable format, including the mass of the weighing bottle with and without solid E, the mass of E used and the volumes of the solutions used in the titrations. Draw up a table in which you can record the results from your titration. Label the rows and columns, using the appropriate units. Results Weighing Mass of bottle + residue /g Mass of bottle + E / g Mass of empty bottle /g Mass of solid E used /g (b) (a b ) (a) 62.71 62.82 53.76 8.95

Titrations

1 Final burette reading / cm3 Initial burette reading /cm3 Volume of solution D used /cm3

26.00 26.10 25.65 0.45 0.60 0.15

25.55 25.50 25.50

Summary ___25.0__ cm3 of the acidified iron(II) solution required ____25.50___ cm3 of potassium manganate(VII) solution for reaction. Skill Assessment Analysis a. Calculate the concentration of the potassium manganate(VII), KMnO4, solution in mol dm3. Concentration = 3.00 g dm-3 158.1 g mol-1 = 0.01897 mol dm-3

b.

Calculate the moles of the KMnO4 used in your mean titre. Moles = 0.01897 mol dm-3 0.025 dm3 = 4.744 10-4 mol

c.

Calculate the moles of Fe2+ which reacted with KMnO4 in the titration. 5 moles Fe2+ reacts with 1 mole MnO4 moles of Fe2+ = (4.744 10-4) 5 = 2.372 10-3 moles

d.

Using your answer in (c), calculate the moles of E used for this experiment. 25 cm3 of Fe2+ contains 2.372 10-3 mols 250 cm3 of Fe2+ will contain (2.372 10-3) 10 = 2.372 10-2 mols

e.

Calculate the relative molar mass of E. 2.372 10-3 moles of iron (II) compound weighs 8.95 g 1.0 mole of iron(II) compound will weigh, 8.95 g 2.372 10-2 mol = 377.3 g mol-1

f.

E is called a double salt because it contains two different cations but the same anion. Its name is ammonium iron(II) sulphate. The formula of E can be written as (NH4)2SO4FeSO4.xH2O. Use the relative molar mass calculated in (e) to calculate x. Mass of H2O in molar mass = 377.3 284.1 = 92.9 g Mols of H2O = 92.9 = 5 18 x =5 What is the percentage error in the volume of manganate added at end point? 0.1 2 100% = 0.8% 25

g.

Skill Assessment Evaluation (a) Before starting the titrations what precautions did you take? 1 pipette was washed with deionised water and rinsed with solution of E 2 Burette was washed with deionised water and later with KmnO4. 3 Conical flask was washed with deionised water 4 Ensure that there was no air bubble trapped in the burette nozzle

(b) The manganate solution is intensely coloured. How did you measure the volume of solution used during the titrations? Use the upper meniscus

(c) 1 2

If you were to repeat this experiment how would you make sure that your result was as accurate as possible? Dry the solid Use a more accurate balance that can weigh upto 3 decimal places

................................................................................................................................................... ................................................................................................................................................... ................................................................................................................................................... ................................................................................................................................................... .... Skill Assesment: Analysis and evaluation. A student determined the relative molar mass of E by another method described below. He weighed out 0.17 g of E on a balance reading to 0.01 g. He dissolved the solid in about 10 cm3 of water. He added aqueous barium chloride to his solution of E. This reaction produced a precipitate of barium sulphate, BaSO4. He filtered the precipitate using a pre-weighed filter paper. Then he placed the filter paper and precipitate in a hot oven for about 5 minutes. Finally, he weighed the filter paper with the precipitate. He obtained 0.22g of barium sulphate. a. Use the students results to calculate (i) the moles of barium sulphate formed; 0.22 g = 9.438 10 -4 mol -1 233.1 g mol

(ii) The relative molar mass of E. 1 mol E will form 2 moles of BaSO4 9.438 10-4 mol BaSO4 is produced by 9.438 10 -4 mol = 4.719 10 -4 mol E 2 Molar mass of E = 0.17 g 4.719 x 10-4 mol = 360.2 g mol-1

b.

Calculate the % error in the weighing of barium sulphate. Suggest and explain how the % accuracy in weighings could be improved. 0.01 100% = 4.55 % 0.22

Reduce the number of weighing e.g. if the process to estimate the weight of BaSO4 had involved (1) weighing the dry filter paper then (2) weighing the filter + BaSO4, then the process involves 2 weighing, each giving an error. Then percentage error = error when weighing paper + error weighing the paper + BaSO4

c. State and explain two ways whereby the student could improve the accuracy and reliability of determining the molar mass. 1 BaSO4 + paper should be completely dried . Heat the paper for longer period. Repeat weighing and heating until constant mass is obtained 2 During filtering, fine particles may pass through the pores. So warm the solution before filtering. This will cause the precipitate to coagulate, or use a thicker filter paper. 3 Ensure that the reaction is complete. Use excess BaCl2 4 Repeat the experiment to obtain consistent results

d.

The titration method for determining relative molar mass that you carried out is more accurate and reliable than the students method. Explain why.

1 burettes an pipettes are accurately calibrated. 2 3 percentage error of the equipment are known and can be calculated The end point is clear and easily seen