Paper 3 Advanced Practical Skills 1
9701/31 · October/November 2025
Question 1 — Redox titration: ethanedioic acid vs manganate(VII)
Heat FA 1 with dilute sulfuric acid to about 70°C, then titrate against acidified potassium manganate(VII) to a self-indicating pale pink end-point, and use the stoichiometry to find x in (COOH)₂·xH₂O.
RUN IT ON THE BENCH
Your readings feed straight into the answer table below as you record them.
ON YOUR BENCH — FROM THE CONFIDENTIAL INSTRUCTIONS
Question 1 — solutions
- FA 1(150 cm³)
- FA 2(150 cm³)
- FA 3(100 cm³)
Question 1 — apparatus
- 25 cm³ pipette(1)
- pipette filler(1)
- 50 cm³ burette(1)
- burette stand and clamp(1)
- funnel(1)
- 150 cm³ or 250 cm³ conical flask(2)
- 25 cm³ measuring cylinder(1)
- 100 cm³ beaker(1)
- white tile(1)
- thermometer(1)
- tripod(1)
- gauze(1)
- Bunsen burner and means to light it(1)
- heat-proof mat(1)
- wash bottle of distilled water(1)
THE BENCH — 25.0 cm³ FA 1 + FA 3, HEATED · FA 2 (ACIDIFIED KMnO4) IN THE BURETTE — ROUGH TITRATION
Why does the purple flash and then fade — until it suddenly doesn't?
While oxalic acid remains in the flask, every drop of MnO₄⁻ that lands is reduced to near-colourless Mn²⁺ almost as fast as it arrives — a purple flash that fades as you swirl it in. The moment the oxalic acid runs out, the next drop has nothing left to reduce it: that drop's colour stays, and the whole flask turns and holds a pale pink. KMnO₄ is its own indicator here — nothing needs to be added.
Why heat to about 70°C, and not just react at room temperature or boil it?
At room temperature the reaction between MnO₄⁻ and ethanedioate ions is slow to start — it only speeds up once some Mn²⁺ has formed, which then catalyses the rest (it's autocatalytic). Warming the flask gives the reaction a head start. Boiling is avoided because it would decompose ethanedioic acid and boil off some of the solution, throwing off the very titre you're trying to measure.
Why add FA 3 (dilute sulfuric acid) at all?
The equation needs H⁺ on the left: 2MnO₄⁻ + 5(COOH)₂ + 6H⁺ → 2Mn²⁺ + 10CO₂ + 8H₂O. Without enough acid present, manganate(VII) is reduced instead to brown manganese(IV) oxide, MnO₂ — a different reaction with a different, unusable stoichiometry. FA 3 keeps the solution acidic enough that Mn²⁺ is the only product forming.
What if I overshoot?
A flask that's gone from pale pink to a clear, deep purple means you've added MnO₄⁻ well past the point where any oxalic acid remained — the titre reads high and the run doesn't count. Take a fresh flask, heat it again, run in quickly to just under your rough titre, then go drop by drop.
YOUR TASKS · 0/4
- ✓Heat FA 1 + FA 3 to ~70°C, then run a rough titration
- ✓Run accurate titration 1 to a permanent pale pink
- ✓Run accurate titration 2 to a permanent pale pink
- ✓Get two concordant accurate titres (within 0.10 cm³)
LAB NOTEBOOK — YOUR TITRES
| ROUGH | ACC. 1 | ACC. 2 | |
|---|---|---|---|
| initial reading /cm³ | 0.35 | 0.60 | 0.25 |
| final reading /cm³ | — | — | — |
| titre /cm³ | — | — | — |
| verdict | — | — | — |
YOUR ANSWERS
Perform a rough titration of FA 1 (heated with FA 3) against FA 2, then carry out as many accurate titrations as you need for consistent results. Record all your burette readings and titres.
| Rough titration | Accurate titration 1 | Accurate titration 2 | |
|---|---|---|---|
| initial burette reading /cm³ | |||
| final burette reading /cm³ | |||
| titre / volume of FA 2 added /cm³ |
From your accurate titration results, calculate a suitable mean value to be used in your calculations: 25.0 cm³ of FA 1 required ___ cm³ of FA 2.
Give your answers to (c)(ii), (c)(iii) and (c)(iv) to the appropriate number of significant figures.
Calculate the amount, in mol, of manganate(VII) ions, MnO₄⁻, in the volume of FA 2 calculated in (b).
Calculate the amount, in mol, of ethanedioic acid that reacts with the manganate(VII) ions in (c)(ii). Hence calculate the concentration, in mol/dm³, of ethanedioic acid in FA 1.
Calculate the relative molecular mass, Mr, of the ethanedioic acid in FA 1.
Calculate the value of x in (COOH)₂·xH₂O. Show your working.
Explain why it is necessary to add FA 3 in each titration.