In this experiment you will determine the oxidation number of iodine in one of its compounds by titration. FA 1 is a 0.0197 mol dm-³ solution of the iodine-containing compound. FA 2 is dilute sulfuric acid, H₂SO₄. FA 3 is aqueous potassium iodide, KI. FA 4 is 0.105 mol dm-³ sodium thiosulfate, Na₂S₂O₃. starch indicator FA 1 reacts with excess acidified potassium iodide to produce iodine, I₂. This iodine is then titrated with aqueous sodium thiosulfate using starch indicator.
- (a)Method • Fill the burette with FA 4. • Pipette 25.0 cm³ of FA 1 into a conical flask. • Using the measuring cylinder, add 10 cm³ of FA 2 to the same conical flask. • Using the same measuring cylinder, add 20 cm³ of FA 3 to the mixture in the conical flask. • The mixture will now be a red-brown colour, due to iodine produced. • Carry out a rough titration by adding FA 4 from the burette until the mixture becomes light brown. • Then add 10 drops of starch indicator. The mixture will change to a dark blue colour. • Continue titrating until the mixture becomes colourless. This is the end-point. The rough titre is ...................................... cm³. Carry out as many accurate titrations as you think necessary to obtain consistent results. Make sure any recorded results show the precision of your practical work. Record in a suitable form below all of your burette readings and the volume of FA 4 added in each accurate titration.[7]
- (b)From your accurate titration results, obtain a suitable value for the volume of FA 4 to be used in your calculations. Show clearly how you obtained this value. The iodine produced required .............................................................. cm³ of FA 4.[1]
- (c)(i)Calculate the number of moles of sodium thiosulfate in the volume of FA 4 calculated in (b). moles of Na₂S₂O₃ = .............................................. mol[1]
- (c)(ii)The equation for the reaction of iodine with sodium thiosulfate is shown. I₂(aq) + 2Na₂S₂O₃(aq) → Na₂S₄O₆(aq) + 2NaI(aq) Calculate the number of moles of iodine that reacted with the sodium thiosulfate calculated in (i). moles of I₂ = .............................................. mol[1]
- (c)(iii)Use the information on page 2 to calculate the number of moles of iodine-containing compound in the 25 cm³ of FA 1 used in each titration. moles of iodine-containing compound in 25 cm³ FA 1 = .............................................. mol
- (c)(iv)Use your answers to (ii) and (iii) to calculate the number of moles of iodine produced when 1 mole of the iodine-containing compound in FA 1 reacts with excess FA 3. Give your answer as an integer. moles of I₂ = .............................................. mol[1]
- (c)(v)The anion in FA 1 is IOₓ⁻ where x is the number of oxygen atoms present in the formula. Use your answer to (iv) to balance the ionic equation for the reaction between FA 1 and FA 3 under acidic conditions. Hence deduce the value of x in the formula IOₓ⁻. IOₓ⁻ + .........I⁻ + .........H⁺ → .........I₂ + .........H₂O x = ......................................[2]
- (c)(vi)Calculate the oxidation state of iodine in FA 1. (If you were unable to calculate x in part (v), assume that x = 4.) oxidation state of iodine = ......................................[1]
Mark scheme
Marking points from the official mark scheme (Oct/Nov 2017). The mark or mark type is shown in brackets.
- [1] I All the following data is recorded both burette readings and the titre for the rough titration initial and final burette readings for two (or more) accurate titrations Headings and units are not required for this mark
- [1] II Titre values recorded for accurate titrations, and appropriate headings and units in the accurate titration table initial / start (burette) reading / volume / value final / end (burette) reading / volume / value titre or volume / FA 4 and used / added unit: / cm³ or (cm³) or in cm³ (for each heading) or cm³ unit given for each volume recorded
- [1] III All accurate burette readings are to the nearest 0.05 cm³. The requirement to record to 0.05 applies to burette readings, including 0.00 cm³ (if this was the initial reading), but it does not apply to the titre. Do not award this mark if: 50(.00) is used as an initial burette reading more than one final burette reading is 50.(00) any burette reading is greater than 50.(00)
- [1] IV The final accurate titre recorded is within 0.10 cm³ of any other accurate titre. Examiner rounds any accurate burette readings to the nearest 0.05 cm³, checks subtractions and then selects the "best" titres using the hierarchy: identical titres then accurate titres within 0.05 cm³, then accurate titres within 0.10 cm³, etc. These best titres should be used to calculate the mean titre, expressed to nearest 0.01 cm³. Examiner compares candidate's mean titre value with that of the Supervisor.
- [1] Award V, VI and VII if δ ≤ 0.20 (cm³)
- [1] Award V and VI if 0.20 < δ < 0.40
- [1] Award V, only, if 0.40 < δ < 0.60
- [1] Candidate must take the average of two (or more) titres that are within a total spread of not more than 0.20 cm³. Working/explanation must be shown or ticks must be put next to the two (or more) accurate readings selected. The mean should be quoted to 2 dp, and be rounded to nearest 0.01 cm³. (e.g. 26.666 cm³ must be rounded to 26.67 cm³) Two special cases, where the mean need not be to 2 dp: Allow mean expressed to 3 dp only for 0.025 or 0.075 (e.g. 26.325 cm³) Allow mean if expressed to 1 dp, if all accurate burette readings were given to 1 dp and the mean is exactly correct. (e.g. 26.0 and 26.2 = 26.1 is allowed) (e.g. 26.0 and 26.1 = 26.1 is wrong – should be 26.05) Do not award this mark if: The rough titre was used to calculate the mean. The candidate did only one accurate titration. Burette readings were incorrectly subtracted to obtain any of the accurate titre values. All burette readings used to calculate the mean were recorded as integers
- [1] Correctly calculates No of moles of thiosulfate used = 0.105 x mean titre / 1000 to 3 or 4 sf
- [1] Correct use of data in both parts (ii) moles I₂ = 0.5 × ans (i) and (iii) moles FA1 = 0.025 × 0.0197 (= 0.000493, 0.0004925)
- [1] Correctly calculates answer, expressed as integer No of moles = (ii) / (iii)
- [1] First mark: integer in answer (iv) shown in front of I₂ and correct number of moles of I⁻ entered in equation
- [1] Second mark: any equation fully balanced IO₃⁻ + 5I⁻+ 6H⁺ → 3I₂ + 3H₂O
- [1] Oxidation state = 2x - 1.
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