Chemistry 9701/37 — October/November 2025
Cambridge AS Level · Advanced Practical Skills · worked solutions for every part, with the mark scheme
Topics Manipulation, Measurement and Observation · Presentation of Data and Observations · Analysis, Conclusions and Evaluation · Qualitative Analysis
Hydrated ethanedioic acid is a diprotic acid with the formula where is an integer.
Ethanedioic acid reacts with manganate(VII) ions when heated.
You will determine the value of in by titrating a solution containing ethanedioic acid with manganate(VII) ions.
- FA 1 is aqueous ethanedioic acid, .
- FA 2 is potassium manganate(VII), .
- FA 3 is sulfuric acid, .
Method
- Fill the burette with FA 2.
- Pipette of FA 1 into a conical flask.
- Use the measuring cylinder to add approximately of FA 3 to the conical flask.
- Place the conical flask on a tripod and gauze and heat carefully until the temperature of the solution is approximately .
- Remove the flame.
- Carefully lift the hot conical flask and place it on the white tile under the burette.
- Add FA 2 drop-wise for the first . Any initial pink colouring may take several seconds to disappear.
- If the reaction mixture turns brown, reheat it to about . If the brown colour disappears, continue the titration. If the brown colour remains, discard the contents of the flask and begin a new titration.
- The end-point is reached when a permanent pale pink colour is formed.
- Perform a rough titration with FA 2. Record your burette readings in the space below.
The rough titre is .............................. .
- Carry out as many titrations as you think necessary to obtain consistent results.
- Make sure any recorded results show the precision of your practical work.
- Record all your burette readings and the volume of FA 2 added in each accurate titration.
Results
Answer
Record the rough titre and at least two accurate titrations, with all burette readings to the nearest 0.05 cm3. For example (your readings will differ):
| Titration | Initial reading / cm3 | Final reading / cm3 | Titre / cm3 |
|---|---|---|---|
| Rough | 0.00 | 24.85 | 24.85 |
| 1 | 0.00 | 24.60 | 24.60 |
| 2 | 24.60 | 49.25 | 24.65 |
The accurate titres are concordant (within 0.10 cm3 of each other).
Example data: titres 24.60 and 24.65 cm3
Background Concept
In a titration, the aim is to determine the volume of a solution (the titrant) needed to react completely with a known volume of another solution. For reliable results, the titre must be measured accurately and consistently. Burette readings are typically taken to the nearest 0.05 cm3 because the burette scale allows estimation between the 0.1 cm3 divisions. Concordant titres are those that agree within a small tolerance (here 0.10 cm3), indicating that the reaction has been carried out consistently.
Understanding the Question
This part asks you to perform the titration and record your results properly. You need to record the rough titre and then carry out accurate titrations until you have at least two concordant results. The marks are awarded for the quality of your data recording: correct headings, units, precision, and concordance.
Approach
Carry out a rough titration to get an approximate end-point. Then perform accurate titrations, adding the manganate(VII) drop-wise near the end-point. Record initial and final burette readings for each accurate titration. Calculate the titre as final minus initial. Ensure that your accurate titres agree within 0.10 cm3. Record all readings to 0.05 cm3.
Step-by-Step Reasoning
- Fill the burette with FA2 (KMnO4). Record the initial reading.
- Pipette 25.0 cm3 of FA1 into a conical flask, add about 20 cm3 of FA3 (H2SO4), heat to about 70°C, then titrate.
- For the rough titration, add FA2 quickly until the end-point is approached, then drop-wise. Record the rough titre.
- For accurate titrations, start with a clean flask and repeat the procedure. Add FA2 drop-wise near the end-point until a permanent pale pink colour appears. Record the final reading.
- The titre is the difference between final and initial readings.
- Repeat until you have at least two accurate titres within 0.10 cm3 of each other.
- Record all readings to the nearest 0.05 cm3.
Key Takeaways
- Burette readings must be recorded to 0.05 cm3.
- Concordant titres are essential for a reliable mean.
- The titre is calculated as final − initial reading.
Common Mistakes
- Recording readings to only 0.1 cm3 instead of 0.05 cm3.
- Not performing enough accurate titrations to get concordant results.
- Forgetting to record units or headings in the results table.
Things to Be Careful About
- Ensure the burette is filled correctly and there are no air bubbles.
- The end-point is a permanent pale pink colour; a transient pink that disappears is not the end-point.
- If the solution turns brown and does not disappear on reheating, discard and start again.
From your accurate titration results, calculate a suitable mean value to be used in your calculations.
Show clearly how you obtained this value.
of FA 1 required .............................. of FA 2.
Working
Mean titre = = 24.63 cm3 (to 2 dp)
Answer
24.63 cm3
24.63 cm3
Background Concept
The mean titre is the average of the concordant accurate titres. It is used in subsequent calculations. The mean should be quoted to 2 decimal places (0.01 cm3) to reflect the precision of the burette readings.
Understanding the Question
You are asked to calculate a suitable mean titre from your accurate results, showing your working. The mark is awarded for correctly averaging two or more titres that are within 0.20 cm3 total spread.
Approach
Select two or more accurate titres that are concordant (within 0.10 cm3 of each other). Add them together and divide by the number of titres. Round the result to 2 decimal places.
Step-by-Step Reasoning
- Identify the accurate titres that are concordant. For example, 24.60 cm3 and 24.65 cm3.
- Sum them: 24.60 + 24.65 = 49.25 cm3.
- Divide by 2: 49.25 / 2 = 24.625 cm3.
- Round to 2 decimal places: 24.63 cm3 (since the third decimal is 5, round up).
- Show this working clearly.
Key Takeaways
- The mean should be based on concordant titres.
- Rounding to 2 dp is required.
Common Mistakes
- Averaging titres that are not concordant.
- Not rounding correctly (e.g., leaving 24.625 as 24.62).
- Not showing working.
Things to Be Careful About
- The spread of the titres used must be ≤ 0.20 cm3.
- Use all concordant titres, not just two if you have more.
Calculations
Give your answers to (c)(ii), (c)(iii) and (c)(iv) to the appropriate number of significant figures.
Answer
Answers to (c)(ii), (c)(iii) and (c)(iv) are given to 3 significant figures.
3 significant figures
Background Concept
Significant figures indicate the precision of a measurement or calculation. In this experiment, the burette readings are to 0.05 cm3, so calculations based on them should be given to 3–4 significant figures. The mark scheme requires answers to (c)(ii), (c)(iii) and (c)(iv) to 3–4 significant figures.
Understanding the Question
This part is a reminder to give your answers in the subsequent parts to the appropriate number of significant figures. It is not a calculation but a requirement.
Approach
When you calculate the amount of manganate(VII), the amount of ethanedioic acid, the concentration, and the relative molecular mass, ensure your final answers are quoted to 3–4 significant figures.
Step-by-Step Reasoning
- The concentration of FA2 is given to 3 significant figures (0.0200). The volume is measured to 0.05 cm3, which is about 3 significant figures for a titre of ~25 cm3. Therefore, answers to 3 significant figures are appropriate.
- For example, 4.93 × 10^-4 mol has 3 significant figures.
- Ensure you do not round intermediate values; round only the final answer.
Key Takeaways
- Use 3–4 significant figures in final answers.
- Do not round intermediate steps.
Common Mistakes
- Giving too many significant figures (e.g., 4.926 × 10^-4) or too few (5 × 10^-4).
Things to Be Careful About
- The mark is awarded for correct significant figures; even if the value is correct, wrong sf loses the mark.
Calculate the amount, in mol, of manganate(VII) ions, , in the volume of FA 2 calculated in (b).
amount of = .............................. mol
Working
Volume of FA2 = 24.63 cm3 =
Amount of MnO4− =
Answer
4.93 × 10^-4 mol
Background Concept
The amount of a substance in moles is calculated by multiplying concentration (mol dm^-3) by volume (dm^3). Since the volume is given in cm3, it must be converted to dm3 by dividing by 1000.
Understanding the Question
You are asked to calculate the amount of manganate(VII) ions in the volume of FA2 that you calculated in part (b). This is the first step in using the titration results.
Approach
Take the mean titre from part (b), convert it to dm3, and multiply by the concentration of FA2 (0.0200 mol dm^-3).
Step-by-Step Reasoning
- Mean titre = 24.63 cm3.
- Convert to dm3: 24.63 / 1000 = 0.02463 dm3.
- Amount = concentration × volume = 0.0200 × 0.02463 = 4.926 × 10^-4 mol.
- Round to 3 significant figures: 4.93 × 10^-4 mol.
Key Takeaways
- Always convert cm3 to dm3 before calculating moles.
- The unit of amount is mol.
Common Mistakes
- Forgetting to convert cm3 to dm3, leading to a factor of 1000 error.
- Using the wrong concentration (e.g., FA1 instead of FA2).
Things to Be Careful About
- Use the mean titre from part (b), not the rough titre.
- Ensure the concentration is in mol dm^-3.
Calculate the amount, in mol, of ethanedioic acid that reacts with the manganate(VII) ions in (c)(ii).
amount of = .............................. mol
Hence calculate the concentration, in , of ethanedioic acid in FA 1.
concentration of = ..............................
Working
From the equation: 5 mol (COOH)2 react with 2 mol MnO4−.
Amount of (COOH)2 =
This is in 25.0 cm3 = 0.0250 dm3.
Concentration =
Answer
Amount of (COOH)2 =
Concentration =
1.23 × 10^-3 mol; 0.0493 mol dm^-3
Background Concept
The balanced equation shows the stoichiometric relationship between ethanedioic acid and manganate(VII) ions: 5 mol of acid react with 2 mol of manganate(VII). Therefore, the amount of acid is 5/2 times the amount of manganate(VII). The concentration of the acid in FA1 is then found by dividing the amount by the volume of FA1 used (25.0 cm3 = 0.0250 dm3).
Understanding the Question
You need to calculate the amount of ethanedioic acid that reacted, and then its concentration in FA1. This links the titration result to the unknown concentration.
Approach
Use the mole ratio from the equation to convert moles of MnO4− to moles of (COOH)2. Then divide by the volume of FA1 (in dm3) to get concentration.
Step-by-Step Reasoning
- From part (c)(ii), amount of MnO4− = 4.93 × 10^-4 mol.
- Mole ratio: 5 (COOH)2 : 2 MnO4−, so amount of (COOH)2 = 4.93 × 10^-4 × 5/2 = 1.2325 × 10^-3 mol.
- Round to 3 sf: 1.23 × 10^-3 mol.
- Volume of FA1 = 25.0 cm3 = 0.0250 dm3.
- Concentration = 1.23 × 10^-3 / 0.0250 = 0.0493 mol dm^-3.
Key Takeaways
- Use the stoichiometric ratio correctly.
- Concentration = moles / volume (dm3).
Common Mistakes
- Using the ratio upside down (2/5 instead of 5/2).
- Forgetting to convert volume to dm3.
Things to Be Careful About
- The amount of acid is calculated from the reaction with the manganate(VII), not from the volume of FA1 directly.
Calculate the relative molecular mass, , of the ethanedioic acid in FA 1.
= ..............................
Working
FA1 contains 6.20 g dm^-3 of hydrated acid.
Concentration = 0.0493 mol dm^-3
Mr =
Answer
125.8
125.8
Background Concept
The relative molecular mass (Mr) of a substance can be found from its mass concentration (g dm^-3) and molar concentration (mol dm^-3) using the relationship: Mr = mass concentration / molar concentration.
Understanding the Question
You are asked to calculate the Mr of the hydrated ethanedioic acid in FA1, given that FA1 contains 6.20 g dm^-3 of the acid and you have calculated its molar concentration in (c)(iii).
Approach
Divide the mass concentration (6.20 g dm^-3) by the molar concentration (0.0493 mol dm^-3) to get Mr in g mol^-1.
Step-by-Step Reasoning
- Mass concentration = 6.20 g dm^-3.
- Molar concentration = 0.0493 mol dm^-3.
- Mr = 6.20 / 0.0493 = 125.76 g mol^-1.
- Round to appropriate sf: 125.8 (to 4 sf) or 126 (to 3 sf). Since we used 3 sf in concentration, 126 is appropriate. However, for calculation of x, we need a more precise value. We'll use 125.8 for the explanation, but in the solution we gave 125.8. That's 4 sf. That's fine.
Key Takeaways
- Mr = mass concentration / molar concentration.
- Units: g mol^-1.
Common Mistakes
- Using the volume of FA1 incorrectly.
- Forgetting to use the mass concentration of FA1.
Things to Be Careful About
- The mass concentration is given as 6.20 g dm^-3, not the mass in the 25.0 cm3 sample.
Working
Mr of (COOH)2 = 90.0
Mr of water = 18.0
x =
Answer
x = 2
2
Background Concept
The hydrated acid has the formula (COOH)2 · xH2O. Its Mr is the sum of the Mr of anhydrous ethanedioic acid (COOH)2 (90.0) and x times the Mr of water (18.0). Thus Mr = 90.0 + 18.0x. Rearranging gives x = (Mr − 90.0) / 18.0.
Understanding the Question
You need to find the integer value of x using the Mr calculated in (c)(iv).
Approach
Subtract 90.0 from the Mr, then divide by 18.0. The result should be close to an integer; round to the nearest integer.
Step-by-Step Reasoning
- Mr = 125.8 (from part c(iv)).
- Mr of (COOH)2 = 90.0.
- Mass of water = 125.8 − 90.0 = 35.8.
- x = 35.8 / 18.0 = 1.99.
- Round to nearest integer: x = 2.
Key Takeaways
- The formula of the hydrate allows determination of x from Mr.
- Always round to the nearest integer.
Common Mistakes
- Using the wrong Mr for (COOH)2 (e.g., 90.0 vs 90.08).
- Not rounding to an integer.
Things to Be Careful About
- The Mr of (COOH)2 is 90.0 (2×12 + 2×16 + 2×1 + 2×16? Actually (COOH)2: C2H2O4? Let's calculate: (COOH)2 means two COOH groups: each COOH has C=12, O=16, O=16, H=1, so total 45, times 2 = 90. Yes 90.0.
Answer
H+ ions are required in the reaction; they appear in the equation and are used up in the reaction.
H+ ions are required in the reaction.
Background Concept
The reaction between ethanedioic acid and manganate(VII) ions requires H+ ions. The balanced equation shows 6H+ on the left. The sulfuric acid (FA3) provides these H+ ions. Without sufficient acid, the reaction would not proceed as written.
Understanding the Question
You are asked to explain why FA3 (sulfuric acid) is added to each titration. The answer should refer to the need for H+ ions in the reaction.
Approach
State that H+ ions are required for the reaction, as shown in the equation, and that the sulfuric acid supplies them.
Step-by-Step Reasoning
- The equation shows 6H+(aq) as a reactant.
- The manganate(VII) is reduced to Mn2+ in acidic conditions.
- Without H+ ions, the reaction would not occur or would be incomplete.
- Therefore, sulfuric acid is added to provide the acidic medium.
Key Takeaways
- Redox reactions often require acidic conditions.
- The acid is a reactant, not just a catalyst.
Common Mistakes
- Saying it is a catalyst (it is consumed).
- Not mentioning H+ ions specifically.
Things to Be Careful About
- The mark is for stating that H+ is needed/used in the reaction.
Hydrated zinc sulfate has the formula where is an integer.
Hydrated zinc sulfate decomposes when heated, losing only its water of crystallisation and becoming anhydrous.
You will determine the value of in by heating the hydrated salt until it becomes anhydrous.
FA 4 is hydrated zinc sulfate, .
Method
- Weigh the crucible with its lid. Record the mass in the space for Results.
- Add between and of FA 4 to the crucible.
- Weigh the crucible with its lid and FA 4. Record the mass.
- Place the crucible on the pipeclay triangle. Gently heat the crucible and contents for approximately 2 minutes with the lid on.
- Remove the lid. Heat the crucible and contents strongly for approximately 4 minutes.
- Replace the lid and leave the crucible and residue to cool for at least 5 minutes.
You may wish to begin work on Question 3 while the crucible is cooling.
- Weigh the crucible with its lid and its contents. Record the mass.
- Remove the lid. Heat the crucible strongly for approximately 3 minutes.
- Replace the lid and leave the crucible and residue to cool for at least 5 minutes.
- Weigh the crucible with its lid and its contents. Record the mass.
- Calculate the mass of FA 4 used and the mass of residue obtained. Record the masses.
Results
Answer
Results table (example readings — record your own):
| Heading | Mass / g |
|---|---|
| (Mass) crucible + lid | 20.00 |
| (Mass) crucible + lid + FA 4 | 23.25 |
| (Mass) crucible + lid + residue after first heating | 21.85 |
| (Mass) crucible + lid + residue after second heating | 21.83 |
| (Mass) FA 4 used | 3.25 |
| (Mass) residue | 1.83 |
All four weighings are recorded to the same number of decimal places (2 dp). The reading after the second heating (21.83 g) is within +0.02 / −0.05 of the reading after the first heating (21.85 g), confirming constant mass.
Mass of FA 4 = 23.25 − 20.00 = 3.25 g
Mass of residue = 21.83 − 20.00 = 1.83 g
Example readings: FA 4 = 3.25 g, residue = 1.83 g (candidate-dependent)
Background Concept
Water of crystallisation is water chemically bound within the crystal lattice of a hydrated salt. When a hydrated salt such as zinc sulfate is heated, this water is driven off as steam, leaving the anhydrous salt. The mass lost on heating equals the mass of water of crystallisation. By comparing the mass of the anhydrous salt with the mass of water lost, the mole ratio can be found and hence the formula determined. For reliable results, heating must continue until constant mass is reached — two consecutive weighings that agree within a small tolerance show that all water has been removed.
Understanding the Question
This part asks you to carry out the practical procedure and record the data correctly. The five marks are for: (1) a properly headed results table with units, (2) four weighings recorded to a consistent number of decimal places, (3) correct subtraction to find the mass of FA 4 and the residue, and (4–5) the accuracy of the result judged against the theoretical mass ratio. The readings themselves are your own — there is no single correct value.
Approach
Set up the apparatus: crucible with lid on a pipeclay triangle over a tripod, heated with a Bunsen burner. Weigh the empty crucible with its lid. Add 3.20–3.40 g of FA 4 and reweigh. Heat gently with the lid on, then strongly with the lid off, allow to cool, and reweigh. Repeat the strong heating and reweighing until the mass is constant. Record all four weighings to the same number of decimal places (2 or 3 dp). Subtract to find the mass of FA 4 and the mass of residue.
Step-by-Step Reasoning
The six headings required, each with a unit:
- (Mass) crucible + lid / g
- (Mass) crucible + lid + FA 4 / g
- (Mass) crucible + lid + residue after first heating / g
- (Mass) crucible + lid + residue after second heating / g
- (Mass) FA 4 used / g
- (Mass) residue / g
All four weighings must be recorded to the same number of decimal places — either all to 2 dp or all to 3 dp. The reading after the second heating must lie within +0.02 and −0.05 of the reading after the first heating; this is the constant-mass check that proves all water of crystallisation has been driven off. The mass of FA 4 must be between 2.90 and 3.40 g.
Using the example readings:
- crucible + lid = 20.00 g
- crucible + lid + FA 4 = 23.25 g
- crucible + lid + residue after first heating = 21.85 g
- crucible + lid + residue after second heating = 21.83 g
Mass of FA 4 = 23.25 − 20.00 = 3.25 g
Mass of residue = 21.83 − 20.00 = 1.83 g
The mass ratio = mass FA4 / mass residue = 3.25 / 1.83 = 1.78, which matches the theoretical value exactly. This earns both accuracy marks (IV and V).
Key Takeaways
- Record all readings to the same number of decimal places.
- Heat to constant mass — two consecutive weighings agreeing within tolerance proves all water is gone.
- Label every row with a quantity and a unit.
- The accuracy of the result is judged by the mass ratio, not by any single reading.
Common Mistakes
- Forgetting units in the headings — the unit (g) must appear for every row.
- Recording weighings to different decimal places (e.g. 20.0 and 23.25).
- Not heating to constant mass (only one heating), so the residue still contains water and y comes out too high.
- Using the wrong subtraction, e.g. subtracting the residue mass from the FA 4 mass instead of subtracting the empty crucible mass.
- Weighing the crucible without its lid.
Things to Be Careful About
- The lid is included in every weighing — never weigh the crucible without its lid.
- Wait for the crucible to cool before weighing; hot crucibles give false low readings because of convection currents in the balance.
- The mass after the second heating must be within +0.02/−0.05 of the first heating reading — this is the constant-mass check.
Calculations
Calculate the amount, in mol, of anhydrous zinc sulfate residue formed in the decomposition of FA 4.
amount of = .............................. mol
Calculate the amount, in mol, of water of crystallisation lost.
amount of = .............................. mol
Working
Molar mass of ZnSO4 = 65.4 + 32.1 + 4(16.0) = 161.5
Mass of water lost = 3.25 − 1.83 = 1.42 g
Answer
amount of ZnSO4 = 0.0113 mol
amount of H2O = 0.0789 mol
ZnSO4 = 0.0113 mol; H2O = 0.0789 mol (using example masses)
Background Concept
The amount of a substance in moles is found from the relationship , where is the mass in grams and is the molar mass in . The molar mass of anhydrous zinc sulfate ZnSO4 is the sum of the relative atomic masses of its atoms: Zn (65.4) + S (32.1) + 4 × O (16.0) = 161.5 . The molar mass of water is 18 (2 × 1.0 + 16.0).
Understanding the Question
You are given the mass of the residue (anhydrous ZnSO4) and the mass of FA 4 (the hydrated salt). The mass of water lost during heating equals the mass of FA 4 minus the mass of the residue. You must convert both masses to amounts in mol.
Approach
Use for each substance. For ZnSO4, use the residue mass and . For water, first find the mass lost by subtracting the residue mass from the FA 4 mass, then divide by 18 .
Step-by-Step Reasoning
Using the example masses: residue = 1.83 g, FA 4 = 3.25 g.
Amount of ZnSO4 = 1.83 / 161.5 = 0.01133... = 0.0113 mol (3 sf)
Mass of water lost = 3.25 − 1.83 = 1.42 g
Amount of H2O = 1.42 / 18 = 0.0789 mol (3 sf)
The mark scheme requires answers to 2–4 significant figures. Both values are quoted to 3 sf here.
Key Takeaways
- is the fundamental conversion between mass and amount.
- The mass of water lost is found by difference: hydrated mass − anhydrous mass.
Common Mistakes
- Using the mass of FA 4 (3.25 g) instead of the residue mass when calculating the amount of ZnSO4.
- Forgetting to subtract to find the mass of water lost.
- Using the wrong molar mass, e.g. including water in the molar mass of ZnSO4.
Things to Be Careful About
- Molar mass of ZnSO4 = 161.5 — use the precise value, not a rounded 161.
- Give answers to 2–4 significant figures as the mark scheme requires.
- Include the unit mol.
Calculate the value of in the formula .
Show your working.
= ..............................
Working
Answer
y = 7
y = 7
Background Concept
The formula ZnSO4·yH2O means that one formula unit of ZnSO4 is associated with y molecules of water of crystallisation. The mole ratio of water to anhydrous salt equals y. So .
Understanding the Question
You have already found the amounts of ZnSO4 and H2O in part (b)(i). Now divide them to find y, and round to the nearest integer, since y must be a whole number.
Approach
. Evaluate the ratio and round to the nearest integer.
Step-by-Step Reasoning
Since y must be an integer, round 6.98 to 7. The formula of the hydrated salt is therefore ZnSO4·7H2O.
Key Takeaways
- The ratio of moles of water to moles of anhydrous salt gives the number of water molecules per formula unit.
- The answer must be an integer.
Common Mistakes
- Not rounding to an integer (leaving 6.98).
- Inverting the ratio (ZnSO4/H2O instead of H2O/ZnSO4).
- Using the mass ratio instead of the mole ratio.
Things to Be Careful About
- Use the mole amounts from (b)(i), not the masses.
- The value should come out close to a whole number; if it does not, check the arithmetic in (b)(i).
A student suggests using this thermal decomposition method to investigate the number of moles of water of crystallisation in hydrated ethanedioic acid. The teacher says that this method is unsuitable.
Suggest why this method is unsuitable.
Answer
Ethanedioic acid decomposes on heating (it is flammable), so it would not simply lose only its water of crystallisation.
Ethanedioic acid decomposes on heating / is flammable.
Background Concept
Ethanedioic acid (oxalic acid), (COOH)2, is an organic acid. Unlike zinc sulfate, it is not thermally stable — it decomposes on heating and is flammable. Heating it would not simply drive off water of crystallisation; the acid itself would break down, so the mass loss would not equal the water content.
Understanding the Question
The thermal dehydration method works for zinc sulfate because the salt only loses water on heating. The question asks why the same method fails for hydrated ethanedioic acid. The answer is a single point: ethanedioic acid decomposes (or is flammable) on heating.
Approach
Recall the thermal behaviour of ethanedioic acid: it decomposes on heating rather than just losing water.
Step-by-Step Reasoning
The mark scheme accepts: "The (anhydrous ethanedioic) acid would decompose (on heating) / is flammable." Since the acid itself breaks down when heated, the mass lost would include decomposition products as well as water, so the method cannot determine the water of crystallisation.
Key Takeaways
- Thermal dehydration works only for salts that are thermally stable apart from losing water.
- Organic acids like ethanedioic acid may decompose or be flammable when heated.
Common Mistakes
- Saying "it would melt" — melting is not the issue; decomposition is.
- Giving a vague answer like "it's an organic compound" without stating decomposition or flammability.
Things to Be Careful About
- The mark specifically requires the idea of decomposition or flammability — "it would decompose on heating" or "it is flammable" both score.
Qualitative analysis
For each test you should record all your observations in the spaces provided.
Examples of observations include:
- colour changes seen
- the formation of any precipitate and its solubility (where appropriate) in an excess of the reagent added
- the formation of any gas and its identification (where appropriate) by a suitable test.
You should record clearly at what stage in a test an observation is made.
Where no change is observed, you should write 'no change'.
Where reagents are selected for use in a test, the name or correct formula of the element or compound must be given.
If any solution is warmed, a boiling tube must be used. If a solid is heated, a hard-glass test-tube must be used.
Rinse and reuse test-tubes and boiling tubes where possible.
No additional tests should be attempted.
A bottle labelled FA 5 is thought to contain hydrated zinc sulfate. It would therefore contain zinc ions and sulfate ions as well as water of crystallisation.
Devise and carry out tests to investigate whether zinc ions, sulfate ions and water of crystallisation are present.
Record the tests you carry out and the observations you see in the space provided.
Answer
- Heat a few crystals of solid FA 5 in a boiling tube. Observe condensation of water droplets / steam / water vapour on the cooler parts of the tube.
- Make an aqueous solution of FA 5 by dissolving the solid in distilled water.
- To a portion of the solution, add aqueous ammonia dropwise, then add excess. Observe a white precipitate that is insoluble in excess aqueous ammonia.
- To a separate portion of the solution, add aqueous barium chloride (or barium nitrate). Observe a white precipitate.
- Add dilute hydrochloric acid (or nitric acid) to the white precipitate; it remains insoluble. (Alternatively, add acidified potassium manganate(VII) to the solution; the purple colour is not decolourised.)
See working above for the sequence of tests and observations confirming H2O, SO4^2-, and Mg^2+ (not Zn^2+).
Background Concept
Qualitative analysis of unknown substances requires a systematic approach: first testing for water of crystallisation, then preparing an aqueous solution for ion tests. Cations are identified by their reactions with aqueous ammonia, while anions like sulfate are identified by precipitation with barium salts. It is crucial to confirm the identity of the anion (e.g., distinguishing sulfate from sulfite) and to observe the behaviour of precipitates in excess reagent to differentiate between similar cations like Mg^2+ and Zn^2+.
Understanding the Question
The student is given FA 5, which is labelled as hydrated zinc sulfate, but the actual contents must be determined. The task is to devise and carry out tests to investigate the presence of zinc ions, sulfate ions, and water of crystallisation. The student must record observations for each test and then use these to complete a table indicating which species are actually present.
Approach
- Water of crystallisation: Heat the solid and look for condensation.
- Solution preparation: Dissolve the solid in water to test for ions.
- Cation test (Zn^2+ vs Mg^2+): Add aqueous ammonia. Zn^2+ forms a white ppt soluble in excess; Mg^2+ forms a white ppt insoluble in excess. The observation will rule out Zn^2+ and confirm Mg^2+.
- Anion test (SO4^2-): Add barium chloride to form a white ppt of BaSO4.
- Confirmation: Distinguish sulfate from sulfite by adding acid (sulfite ppt dissolves with effervescence, sulfate does not) or acidified KMnO4 (sulfite decolourises it, sulfate does not).
Step-by-Step Reasoning
- M1: Heating the solid FA 5 releases water of crystallisation. The observation is condensation (water droplets, steam, or water vapour) on the cooler upper parts of the boiling tube.
- M2: To test for ions, the solid must be dissolved in distilled water to form an aqueous solution.
- M3: Adding aqueous NH3 to a portion of the solution produces a white precipitate of Mg(OH)2. Unlike Zn(OH)2, Mg(OH)2 is insoluble in excess NH3. This observation rules out Zn^2+ (which would form a soluble complex with excess NH3) and confirms Mg^2+.
- M4: Adding aqueous BaCl2 (or Ba(NO3)2) to another portion produces a white precipitate of BaSO4, indicating the presence of SO4^2-.
- M5: To ensure the anion is sulfate and not sulfite (which also forms a white BaSO3 ppt), add dilute HCl or HNO3. BaSO3 would dissolve with effervescence (SO2 gas), while BaSO4 remains insoluble. Alternatively, acidified KMnO4(aq) would be decolourised by sulfite but remains purple with sulfate.
Key Takeaways
- Always test for water of crystallisation by heating before dissolving the solid.
- Ammonia test is a classic method to distinguish Mg^2+ (insoluble white ppt) from Zn^2+ (soluble white ppt in excess).
- Sulfate confirmation requires showing the barium precipitate is insoluble in acid, or that it does not reduce acidified permanganate.
Common Mistakes
- Writing 'no change' for the ammonia test when a white precipitate forms.
- Claiming the white precipitate is soluble in excess ammonia (this would indicate Zn^2+, which is incorrect here).
- Forgetting to add acid to the barium precipitate to rule out sulfite or carbonate.
- Not specifying that the precipitate is white.
Things to Be Careful About
- State the reagent clearly (e.g., 'aqueous ammonia', not just 'ammonia').
- Describe the precipitate colour (white) and its solubility in excess reagent.
- For the sulfate confirmation, explicitly state that the precipitate is 'insoluble' in acid, or that KMnO4 'remains purple'.
Use your observations in (a)(i) to complete Table 3.1 to show whether each species is present in FA 5.
Use a tick (✓) if the species is present.
Use a cross (✗) if the species is not present.
Table 3.1
| Species | Present |
|---|---|
Answer
| Species | Present |
|---|---|
| Zn^2+ | ✗ |
| SO4^2- | ✓ |
| H2O | ✓ |
Zn^2+: ✗, SO4^2-: ✓, H2O: ✓
Background Concept
Based on the observations from part (a)(i), we can deduce the actual composition of FA 5. The heating test confirmed water. The ammonia test ruled out Zn^2+ and confirmed Mg^2+. The barium chloride test confirmed SO4^2-. Therefore, FA 5 is magnesium sulfate heptahydrate (MgSO4•7H2O), not zinc sulfate.
Understanding the Question
The student must use the observations from part (a)(i) to complete Table 3.1, indicating whether Zn^2+, SO4^2-, and H2O are present in FA 5 using a tick (✓) or a cross (✗).
Approach
- Zn^2+: The ammonia test showed a white ppt insoluble in excess, which is characteristic of Mg^2+, not Zn^2+. Therefore, Zn^2+ is absent (✗).
- SO4^2-: The barium chloride test gave a white ppt insoluble in acid, confirming SO4^2- is present (✓).
- H2O: Heating the solid produced condensation, confirming water of crystallisation is present (✓).
Step-by-Step Reasoning
- Zn^2+: If Zn^2+ were present, the white Zn(OH)2 precipitate would dissolve in excess aqueous ammonia to form a colourless [Zn(NH3)4]2+ complex. Since it did not, Zn^2+ is not present.
- SO4^2-: The formation of a white precipitate with Ba^2+ that is insoluble in dilute acid is the definitive test for sulfate ions.
- H2O: Condensation on the cooler parts of the test tube upon heating is the standard test for water of crystallisation in hydrated salts.
Key Takeaways
- Qualitative analysis results must be directly linked to the specific tests performed.
- A negative result for a suspected ion (like Zn^2+) is just as important as a positive result and must be recorded correctly.
Common Mistakes
- Assuming the label on the bottle is correct and ticking Zn^2+.
- Forgetting that water of crystallisation is 'H2O' and not 'OH-'.
Things to Be Careful About
- Ensure the tick and cross symbols are clear and unambiguous.
- Only include the species asked for in the table.
You are provided with solid FA 6.
Heat a few crystals of FA 6 in a hard-glass test-tube until no further gas is evolved. Record all your observations.
Leave the test-tube until it is cool.
Keep the cooled residue for use in (b)(ii).
Answer
- The solid is purple and jumps / moves around as it is heated.
- A black residue is left in the test tube.
- A glowing splint is inserted into the test tube and relights / glows more brightly.
Purple solid jumps, black residue forms, glowing splint relights.
Background Concept
Potassium manganate(VII), KMnO4, is a purple solid that undergoes thermal decomposition when heated strongly. It breaks down into potassium manganate(VI) (K2MnO4, green), manganese(IV) oxide (MnO2, black), and oxygen gas. The oxygen can be tested with a glowing splint, which will relight.
Understanding the Question
The student is given solid FA 6 (KMnO4) and must heat it until no further gas is evolved, record all observations, and leave the residue for the next part.
Approach
- Note the initial colour of the solid.
- Observe physical changes during heating (jumping/melting).
- Note the colour of the final solid residue.
- Test the evolved gas with a glowing splint to identify it as oxygen.
Step-by-Step Reasoning
- Initial colour: KMnO4 is a deep purple solid.
- During heating: The solid may jump or move around in the tube as oxygen gas is rapidly evolved. It may also appear to melt or decompose vigorously.
- Residue: The solid residue is a mixture of K2MnO4 (green) and MnO2 (black). The overall appearance is often described as a black or dark residue (the black MnO2 masks the green K2MnO4 in the solid state).
- Gas test: Oxygen supports combustion. Inserting a glowing splint into the test tube will cause it to relight or glow more brightly.
Key Takeaways
- Thermal decomposition of KMnO4 produces O2, which is identified by the glowing splint test.
- Always record observations at different stages (initial, during heating, final residue, gas test).
Common Mistakes
- Saying the residue is 'white' or 'colourless'.
- Forgetting to describe the initial colour of the solid.
- Not performing or describing the glowing splint test.
Things to Be Careful About
- The question asks for 'all your observations', so include the initial colour, physical changes, residue colour, and gas test.
- Use precise language: 'glowing splint relights', not 'splint burns'.
To the cooled residue from (b)(i), add approximately depth of distilled water and stir. Filter the solution formed into a test-tube.
The colour of the solution is .............................. .
Answer
(dark) green
dark green
Background Concept
The thermal decomposition of KMnO4 produces K2MnO4 (potassium manganate(VI)) and MnO2 (manganese(IV) oxide). K2MnO4 is soluble in water and produces a dark green solution. MnO2 is insoluble in water and remains as a black solid, which is removed by filtration.
Understanding the Question
The cooled residue from (b)(i) is dissolved in water and filtered. The student must state the colour of the resulting filtrate (solution).
Approach
- The residue contains K2MnO4 (soluble) and MnO2 (insoluble).
- Filtration removes the black MnO2.
- The filtrate contains K2MnO4, which is dark green.
Step-by-Step Reasoning
- When water is added to the cooled residue, K2MnO4 dissolves to form a solution containing MnO4^2- ions.
- Aqueous manganate(VI) ions are characteristically dark green.
- MnO2 does not dissolve and is removed by filtration, so the filtrate is green, not black.
Key Takeaways
- Differentiate between the solubility of decomposition products: K2MnO4 is soluble (green), MnO2 is insoluble (black).
- Filtration separates the soluble product from the insoluble product.
Common Mistakes
- Saying the solution is 'purple' (confusing with unreacted KMnO4 or MnO4-).
- Saying the solution is 'black' (confusing with the insoluble MnO2 residue).
- Saying the solution is 'colourless'.
Things to Be Careful About
- The question asks for the colour of the 'solution', not the residue.
- 'Dark green' or 'green' is acceptable; 'brown' or 'yellow' is incorrect.
You are provided with aqueous solutions FA 7 and FA 8 and with solid FA 9.
FA 7 is an aqueous solution of FA 6.
FA 7, FA 8 and FA 9 contain compounds which all have one metal that is the same but which may be in different oxidation states.
Carry out the following tests on FA 7, FA 8 and FA 9 and record your observations in Table 3.2. For each test use a depth of a solution or a spatula measure of solid.
Answer
Test 1: Add hydrogen peroxide
- FA 7: Bubbles / effervescence; purple solution turns colourless; gas relights a glowing splint.
- FA 8: No change.
- FA 9: Bubbles / effervescence; gas relights a glowing splint.
Test 2: Add aqueous sodium hydroxide, then leave to stand
- FA 8: Off-white precipitate forms; turns brown on standing.
- FA 9: No change.
Test 3: Add aqueous iron(II) sulfate
- FA 7: Purple solution turns colourless / yellow solution formed.
- FA 8: No change.
See table above for observations.
Background Concept
This question explores the chemistry of manganese in different oxidation states: +7 (MnO4- in FA 7), +2 (Mn^2+ in FA 8), and +4 (MnO2 in FA 9).
- MnO4- (+7): Strong oxidising agent, purple solution. Reduced to Mn^2+ (colourless) or Mn^3+ (yellow) by reducing agents like H2O2 or Fe^2+.
- Mn^2+ (+2): Pale pink / colourless solution. Forms a white/off-white precipitate of Mn(OH)2 with NaOH, which is rapidly oxidised by air to brown MnO(OH)2 or MnO2.
- MnO2 (+4): Black insoluble solid. Acts as a catalyst for the decomposition of H2O2 into O2 and H2O.
Understanding the Question
The student must carry out three tests on FA 7 (acidified KMnO4), FA 8 (MnSO4/MnCl2), and FA 9 (MnO2) and record the observations in Table 3.2. Some cells are crossed out (FA 7 for Test 2, FA 9 for Test 3) because the tests are not applicable or would not give a meaningful observation.
Approach
- Test 1 (H2O2): MnO4- oxidises H2O2 to O2 (effervescence, glowing splint relights, purple to colourless). Mn^2+ does not react. MnO2 catalyses H2O2 decomposition (effervescence, glowing splint relights).
- Test 2 (NaOH): Mn^2+ forms Mn(OH)2 (white/off-white ppt), which oxidises in air to brown. MnO2 does not react with NaOH.
- Test 3 (FeSO4): MnO4- oxidises Fe^2+ to Fe^3+ (yellow/brown) and is reduced to Mn^2+ (colourless), so the purple colour disappears. Mn^2+ does not react.
Step-by-Step Reasoning
- Test 1, FA 7: H2O2 is oxidised by MnO4- in acidic solution: 2MnO4- + 5H2O2 + 6H+ -> 2Mn^2+ + 5O2 + 8H2O. Observation: effervescence (O2 gas), purple solution turns colourless (Mn^2+ formed), O2 relights glowing splint.
- Test 1, FA 8: Mn^2+ is already in its lowest common oxidation state and does not react with H2O2 under these conditions. Observation: no change.
- Test 1, FA 9: MnO2 catalyses the decomposition of H2O2: 2H2O2 -> 2H2O + O2. Observation: effervescence, O2 relights glowing splint. (No colour change as MnO2 is a solid catalyst and remains black, but the solution may bubble vigorously).
- Test 2, FA 8: Mn^2+ + 2OH- -> Mn(OH)2 (s). Mn(OH)2 is a white or off-white precipitate. On standing in air, it is oxidised: 2Mn(OH)2 + O2 -> 2MnO(OH)2 (brown). Observation: off-white ppt, turns brown on standing.
- Test 2, FA 9: MnO2 is a basic oxide but does not react with dilute NaOH. Observation: no change (black solid remains).
- Test 3, FA 7: MnO4- oxidises Fe^2+ to Fe^3+: MnO4- + 5Fe^2+ + 8H+ -> Mn^2+ + 5Fe^3+ + 4H2O. Fe^3+ is yellow/brown in solution, and Mn^2+ is colourless. Observation: purple solution turns colourless or yellow (depending on concentration of Fe^3+ formed).
- Test 3, FA 8: Mn^2+ does not react with Fe^2+. Observation: no change.
Key Takeaways
- Manganese exhibits rich redox chemistry across oxidation states +2, +4, and +7.
- MnO4- is a powerful oxidising agent that is decolourised when reduced to Mn^2+.
- Mn^2+ precipitates as a white hydroxide that is easily oxidised in air to a brown product.
- MnO2 acts as a heterogeneous catalyst for H2O2 decomposition.
Common Mistakes
- Saying FA 7 turns 'brown' in Test 1 (it turns colourless as Mn^2+ is formed; Fe^3+ in Test 3 may be yellow/brown, but Mn^2+ is colourless).
- Forgetting to mention the glowing splint test for the gas in Test 1.
- Describing the Mn(OH)2 precipitate as 'white' without noting it turns 'brown on standing'.
- Saying FA 9 reacts with NaOH or FeSO4 (it does not; it is unreactive towards these reagents in this context).
Things to Be Careful About
- Follow the table structure exactly; do not write observations in crossed-out cells.
- For Test 2, separate the immediate observation (off-white ppt) from the observation on standing (brown ppt).
- Use precise colour descriptions: 'purple to colourless', 'off-white', 'brown', 'yellow'.
Suggest the identity of the metal in FA 6/FA 7, FA 8 and FA 9.
The metal is .............................. .
Answer
manganese (or Mn)
manganese
Background Concept
The tests performed in part (c)(i) are characteristic of manganese and its compounds. The purple colour of FA 7, its reaction with H2O2 and Fe^2+, the formation of a white/brown hydroxide with NaOH, and the catalytic activity of FA 9 (MnO2) all point to manganese.
Understanding the Question
The student must suggest the identity of the metal common to FA 6, FA 7, FA 8, and FA 9.
Approach
- FA 6 is purple and decomposes to give O2 and a black residue -> KMnO4.
- FA 7 is purple and acts as an oxidising agent -> MnO4-.
- FA 8 gives a white/brown precipitate with NaOH -> Mn^2+.
- FA 9 is a black solid that catalyses H2O2 decomposition -> MnO2.
- All these are manganese compounds.
Step-by-Step Reasoning
- The purple colour and oxidising properties identify MnO4-.
- The thermal decomposition producing O2 and the green solution (K2MnO4) confirms Mn.
- The hydroxide precipitate behaviour is characteristic of Mn^2+.
- Therefore, the metal is manganese (Mn).
Key Takeaways
- Qualitative analysis can be used to identify an unknown metal by its characteristic reactions and compound colours.
- Manganese has distinctive colours: purple (MnO4-), green (MnO4^2-), pale pink/colourless (Mn^2+), black (MnO2).
Common Mistakes
- Suggesting iron (Fe) or copper (Cu) without justification.
- Not naming the element correctly (e.g., writing 'manganate' instead of 'manganese').
Things to Be Careful About
- The question asks for the 'metal', so write 'manganese' or 'Mn', not 'manganate' or 'permanganate'.
Complete Table 3.3 to suggest the oxidation state of the metal in FA 6/FA 7 and FA 8.
Table 3.3
| FA 6/FA 7 | FA 8 | |
|---|---|---|
| oxidation state |
Answer
| FA 6 / FA 7 | FA 8 | |
|---|---|---|
| oxidation state | +7 | +2 |
FA 6/FA 7: +7, FA 8: +2
Background Concept
Oxidation states can be determined from the chemical formulae of the compounds. For manganese:
- KMnO4 (potassium manganate(VII)): K is +1, O is -2. 1 + x + 4(-2) = 0 => x = +7.
- MnSO4 or MnCl2 (manganese(II) sulfate/chloride): SO4 is -2, Cl is -1. Mn must be +2 to balance.
Understanding the Question
The student must complete Table 3.3 to state the oxidation state of manganese in FA 6/FA 7 and in FA 8.
Approach
- FA 6 and FA 7 contain the MnO4- ion (from KMnO4). The oxidation state of Mn in MnO4- is +7.
- FA 8 contains Mn^2+ ions (from MnSO4 or MnCl2). The oxidation state is +2.
Step-by-Step Reasoning
- FA 6 / FA 7: The purple colour and oxidising behaviour identify this as potassium manganate(VII), KMnO4. In MnO4-, oxygen is -2, so Mn + 4(-2) = -1 => Mn = +7. The oxidation state is +7.
- FA 8: The formation of Mn(OH)2 with NaOH and lack of reaction with H2O2 or Fe^2+ identifies this as a manganese(II) salt, e.g., MnSO4. The ion is Mn^2+, so the oxidation state is +2.
Key Takeaways
- Oxidation states can be calculated from formulae using known oxidation states of common ions (O = -2, K = +1, SO4 = -2, Cl = -1).
- The Roman numeral in the name of a compound (e.g., manganate(VII)) directly gives the oxidation state of the central metal.
Common Mistakes
- Writing '7' instead of '+7'.
- Confusing the oxidation state of Mn in MnO4- (+7) with Mn in MnO2 (+4).
- Not including the '+' sign.
Things to Be Careful About
- Always include the sign (+ or -) for oxidation states.
- Ensure the oxidation state matches the correct substance (FA 6/FA 7 is +7, FA 8 is +2).
