Chemistry 9701/34 — May/June 2024
Cambridge AS Level · Advanced Practical Skills · worked solutions for every part, with the mark scheme
Topics Analysis, Conclusions and Evaluation · Manipulation, Measurement and Observation · Presentation of Data and Observations · Qualitative Analysis
In this experiment you will determine the relative formula mass, , of a basic metal carbonate, , by a titration method.
FB 1 is the basic metal carbonate .
FB 2 is a solution containing hydrochloric acid, , and , prepared using FB 1 as follows.
- of FB 1, , is weighed out.
- of hydrochloric acid (a small excess) is added to FB 1.
- The mixture is left to allow FB 1 to react completely.
- The resulting solution is made up to with distilled water.
- This solution is FB 2.
FB 3 is potassium hydroxide, , of concentration .
FB 4 is thymolphthalein indicator.
Method
- Fill the burette with FB 2.
- Pipette of FB 3 into a conical flask.
- Add a few drops of FB 4 to the conical flask.
- Perform a rough titration and record your burette readings in the space below.
The rough titre is .............................. .
- 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 in the space below, all your burette readings and the volume of FB 2 added in each accurate titration.
Answer
Rough titration
Record the initial and final burette readings and the rough titre. For example:
initial reading = 15.00 cm³, final reading = 24.10 cm³, rough titre = 9.10 cm³
Accurate titrations
Carry out at least two accurate titrations until two titres agree within 0.10 cm³. Record all readings in a table with headings and units, for example:
| Titration 1 | Titration 2 | Titration 3 | |
|---|---|---|---|
| final burette reading / cm³ | 24.00 | 33.00 | 42.05 |
| initial burette reading / cm³ | 15.00 | 24.00 | 33.00 |
| titre / cm³ | 9.00 | 9.00 | 9.05 |
All burette readings recorded to the nearest 0.05 cm³.
Candidate-dependent: rough titre plus two or more accurate titrations, readings to 0.05 cm³, concordant within 0.10 cm³ (representative titres: 9.00, 9.00, 9.05 cm³)
Background Concept
A titration is a quantitative technique for determining the concentration of a solution by reacting a measured volume of it with a solution of known concentration until the reaction is complete. The end-point is detected with an indicator. This experiment uses a back-titration: a known amount of hydrochloric acid is added in excess to the basic metal carbonate so that all of the carbonate reacts; the unreacted (excess) HCl is then titrated against a standard solution of KOH. Knowing how much HCl was added and how much remained unreacted tells us how much reacted with the carbonate, which leads to the molar mass of the carbonate.
Thymolphthalein is the indicator: it is colourless in acid and blue in alkaline solution. In this titration, FB2 (acidic) is run from the burette into the conical flask containing FB3 (KOH, which turns blue with the indicator). The blue colour disappears at the end-point when all the KOH has been neutralised.
The reliability of the whole experiment rests on careful technique and accurate recording, which is exactly what part (a) rewards.
Understanding the Question
Part (a) asks you to perform the titration and record your results properly. The marks are awarded for:
- recording the rough titre (initial and final burette readings plus the titre),
- recording initial and final burette readings for at least two accurate titrations,
- using correct table headings with units,
- recording all burette readings to the nearest 0.05 cm³,
- obtaining concordant titres (within 0.10 cm³ of each other).
Approach
- Fill the burette with FB2, making sure there are no air bubbles in the jet below the tap.
- Pipette 25.0 cm³ of FB3 into a conical flask and add a few drops of thymolphthalein; the solution turns blue.
- Do a rough titration first: run FB2 in fairly quickly until the blue colour just disappears. Record the initial and final readings and the rough titre.
- Do accurate titrations: repeat the procedure, adding FB2 dropwise as the end-point approaches. Record the initial and final readings each time.
- Continue until two titres agree within 0.10 cm³.
Step-by-Step Reasoning
Rough titration — its purpose is to find the approximate end-point volume so that accurate titrations can be done efficiently without overshooting. A typical record might be: initial = 15.00 cm³, final = 24.10 cm³, rough titre = 9.10 cm³.
Accurate titrations — repeat the procedure, adding the acid dropwise near the end-point. Record every reading to the nearest 0.05 cm³. A typical set:
- Titration 1: initial 15.00, final 24.00, titre 9.00
- Titration 2: initial 24.00, final 33.00, titre 9.00
- Titration 3: initial 33.00, final 42.05, titre 9.05
The titre is always the final reading minus the initial reading. The two titres of 9.00 cm³ are identical and concordant; the third (9.05 cm³) is within 0.10 cm³ of them.
Table format — each column needs a heading that names the quantity and its unit, e.g. "final burette reading / cm³", "initial burette reading / cm³", "titre / cm³". The unit can be written in the heading or after each value, but it must be present.
Key Takeaways
- A rough titration establishes the approximate end-point quickly.
- Accurate titrations are repeated until two results are concordant (within 0.10 cm³).
- Burette readings are recorded to the nearest 0.05 cm³.
- Results are recorded in a table with quantity + unit headings.
Common Mistakes
- Recording readings to only 0.1 cm³ instead of 0.05 cm³ — the mark scheme requires 0.05 cm³ precision.
- Not recording the rough titre.
- Table headings without units, e.g. just "final" instead of "final burette reading / cm³".
- Including the rough titre when averaging.
Things to Be Careful About
- Read the burette at eye level, at the bottom of the meniscus, to avoid parallax error.
- Ensure no air bubbles are trapped in the burette jet before starting.
- The titre is final minus initial reading.
- If the end-point is overshot, that titration must be discarded and repeated.
From your accurate titration results, calculate a suitable mean value to use in your calculations. Show clearly how you obtain the mean value.
of FB 3 required .............................. of FB 2.
Working
Two concordant titres: 9.00 cm³ and 9.00 cm³.
Answer
25.0 cm³ of FB3 required 9.00 cm³ of FB2.
9.00 cm³
Background Concept
The mean titre is the average of the concordant accurate titrations — the values that agree most closely. It is the single volume used in all subsequent calculations, so it must be reliable. The mark scheme requires the mean to be calculated from two or more titres with a total spread of no more than 0.20 cm³, quoted to 2 decimal places.
Understanding the Question
From your accurate titrations, select the concordant values, show how you chose them, and calculate the mean titre to 2 decimal places.
Approach
- Look at your accurate titres and identify the two (or more) that agree most closely.
- Average those values only.
- Quote the mean to 2 decimal places, and show the working (or tick the selected readings).
Step-by-Step Reasoning
With titres of 9.00, 9.00 and 9.05 cm³, the two identical values (9.00 and 9.00) are the best choice — they are the most concordant. The mean is:
The third titre (9.05) is within 0.10 cm³ of the others, but the two identical values give the most reliable mean. Show your selection (e.g. tick the two chosen values) and the calculation.
Key Takeaways
- Select the concordant titres, not all titres indiscriminately.
- The mean is quoted to 2 decimal places.
- Showing the selection and working earns the mark.
Common Mistakes
- Averaging all titres, including a non-concordant one.
- Not showing which values were selected.
- Quoting the mean to more than 2 decimal places.
Things to Be Careful About
- The mark scheme requires the mean to 2 decimal places, rounded to the nearest 0.01 cm³.
- The two (or more) values averaged must be within a total spread of 0.20 cm³.
Calculations
Give your answers to (c)(ii), (c)(iii) and (c)(iv) to an appropriate number of significant figures.
Answer
The answers to (c)(ii), (c)(iii) and (c)(iv) are given to 3 or 4 significant figures.
3 or 4 significant figures
Background Concept
Significant figures indicate the precision of a measured or calculated value. A value quoted to 3 significant figures (e.g. 0.00225) claims more precision than one quoted to 2 (0.0023) and less than one quoted to 4 (0.002250). The data in this question — 5.05 g dm⁻³, 5.00 mol dm⁻³, 22.50 g, 25.0 cm³ — carry 3 or 4 significant figures, so the calculated answers should be quoted to the same precision.
Understanding the Question
This one-mark part simply asks you to state how many significant figures you will use for the answers to (c)(ii), (c)(iii) and (c)(iv).
Approach
Quote the answers to 3 or 4 significant figures.
Step-by-Step Reasoning
The mark scheme awards the mark for answers given to 3 or 4 significant figures. This is a convention: the answers must not be over- or under-precise relative to the data. The data in the question (5.05 g dm⁻³, 5.00 mol dm⁻³, 22.50 g, 25.0 cm³) all carry 3 or 4 significant figures, so the calculated answers should match. For example, 0.00225 mol and 0.250 mol dm⁻³ are each 3 significant figures.
Key Takeaways
- Match the significant figures of the data.
- 3 or 4 significant figures is the required convention here.
Common Mistakes
- Giving answers to 2 or 5 significant figures.
Things to Be Careful About
- This is an easy mark to lose — always check significant figures before finalising.
Calculate the amount, in mol, of potassium hydroxide present in of FB 3.
amount of = .............................. mol
Working
Answer
amount of KOH
0.00225 mol
Background Concept
The amount of a substance in moles is given by:
where is the concentration in mol dm⁻³ and is the volume in dm³. FB3 is KOH at a concentration of 5.05 g dm⁻³, so its concentration in mol dm⁻³ is found by dividing by its molar mass:
Understanding the Question
Calculate the amount, in mol, of KOH present in 25.0 cm³ of FB3.
Approach
- Convert the concentration from g dm⁻³ to mol dm⁻³ by dividing by 56.1.
- Convert 25.0 cm³ to dm³ by dividing by 1000.
- Multiply: .
Step-by-Step Reasoning
This is mol, quoted to 3 significant figures.
Key Takeaways
- is the fundamental relationship.
- Volumes must be in dm³: divide cm³ by 1000.
- Concentration in g dm⁻³ must be converted to mol dm⁻³ using the molar mass.
Common Mistakes
- Forgetting to convert 25.0 cm³ to 0.0250 dm³.
- Using the wrong molar mass for KOH.
Things to Be Careful About
- Quote the answer to 3 or 4 significant figures: 0.00225 mol or mol.
Give the ionic equation for the reaction of hydrochloric acid with potassium hydroxide during the titration. Include state symbols.
...........................................................................................................................................
Hence calculate the concentration, in , of hydrochloric acid in FB 2.
concentration of = ..............................
Working
Ionic equation:
From (b) and (c)(ii):
Answer
0.250 mol dm^-3
Background Concept
The reaction between hydrochloric acid and potassium hydroxide is a neutralisation:
The ionic equation removes the spectator ions (K⁺ and Cl⁻):
At the end-point of the titration, the moles of HCl that have been added exactly equal the moles of KOH originally in the flask. So the moles of HCl in the titre volume equal the moles of KOH calculated in (c)(ii).
Understanding the Question
Write the ionic equation for the neutralisation (with state symbols), then use the mean titre from (b) and the moles from (c)(ii) to calculate the concentration of HCl in FB2.
Approach
- Write the ionic equation: .
- mol.
- Convert the titre to dm³ and divide: .
Step-by-Step Reasoning
The titre is 9.00 cm³ = 0.00900 dm³.
Equivalently, using the formula from the mark scheme:
Key Takeaways
- Neutralisation: .
- At the end-point, moles of acid = moles of base.
- with volume in dm³.
Common Mistakes
- Forgetting state symbols in the ionic equation — the mark scheme requires (aq) and (l).
- Not converting the titre volume to dm³.
Things to Be Careful About
- The ionic equation must show ; spectator ions are omitted.
- Quote the concentration to 3 or 4 significant figures.
Use the information about FB 2 and your answer to (c)(iii) to calculate the relative formula mass, , of .
of = ..............................
Working
Total HCl added:
HCl remaining in FB2 (1.00 dm³):
HCl reacted with FB1:
From the equation, 1 mol MCO₃·M(OH)₂ reacts with 4 mol HCl:
Answer
of MCO₃·M(OH)₂ = 360
360
Background Concept
This is a back-titration. The total amount of HCl added to FB1 is known: 100.0 cm³ of 5.00 mol dm⁻³ HCl. The amount of HCl that remained unreacted is found from the titration: it equals the concentration of HCl in FB2 multiplied by the volume of FB2 (1.00 dm³). The difference between the total added and the amount remaining is the amount of HCl that reacted with FB1. From the balanced equation:
1 mol of MCO₃·M(OH)₂ reacts with 4 mol of HCl. So the amount of FB1 is the reacted HCl divided by 4. Finally, the relative formula mass is:
Understanding the Question
Use the concentration of HCl in FB2 from (c)(iii) together with the preparation details (22.50 g FB1, 100.0 cm³ of 5.00 mol dm⁻³ HCl, made up to 1.00 dm³) to calculate the of MCO₃·M(OH)₂.
Approach
- Total HCl added = 0.100 × 5.00 = 0.500 mol.
- HCl remaining in FB2 = dm³.
- HCl reacted with FB1 = total − remaining.
- Amount of FB1 = reacted HCl ÷ 4.
- = 22.50 ÷ amount of FB1.
Step-by-Step Reasoning
Step 1 — total HCl added:
Step 2 — HCl remaining (in the whole 1.00 dm³ of FB2):
Step 3 — HCl that reacted with FB1:
Step 4 — amount of FB1: from the equation, 4 mol HCl react with 1 mol FB1:
Step 5 — relative formula mass:
Key Takeaways
- Back-titration logic: total added − remaining = amount reacted.
- Use the stoichiometric ratio from the balanced equation (4 HCl : 1 FB1).
- = mass ÷ amount.
Common Mistakes
- Forgetting to multiply by 1.00 dm³ (the volume of FB2) — this is the most common error.
- Using the wrong stoichiometric ratio (e.g. dividing by 2 instead of 4).
- Not subtracting the remaining HCl from the total.
Things to Be Careful About
- The balanced equation shows 4 HCl per FB1 — check the stoichiometry carefully.
- Quote the final to 3 or 4 significant figures.
A student suggested that the procedure used in (a) would be more accurate if the mass of FB 1 used to prepare solution FB 2 is doubled. No other change to the procedure is made.
Explain why the student is not correct.
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Answer
Doubling the mass of FB1 means the 0.500 mol of HCl would no longer be in excess — there would be insufficient HCl to react with all the FB1, so some FB1 would remain unreacted and no HCl would be left to titrate against the KOH.
HCl would no longer be in excess; insufficient HCl to react with all the FB1, so no HCl remains for the titration.
Background Concept
In a back-titration, the reagent added to the sample must be in excess: enough must be present to react with all of the sample and still leave some unreacted reagent to titrate. If the amount of sample is increased without increasing the reagent, the reagent may become the limiting reagent — it runs out before all the sample has reacted.
Understanding the Question
The student suggests doubling the mass of FB1 to improve accuracy. Explain why this is wrong, given that no other change is made (the same 100.0 cm³ of 5.00 mol dm⁻³ HCl is used).
Approach
Doubling the mass of FB1 doubles the amount of HCl needed for complete reaction. Check whether 0.500 mol of HCl is still enough.
Step-by-Step Reasoning
With the found in (c)(iv) (360), 22.50 g of FB1 is 0.0625 mol, which requires mol of HCl. Doubling the mass to 45.0 g gives 0.125 mol of FB1, requiring mol of HCl — exactly all the HCl available, leaving none for the titration. In practice, with any realistic , doubling the mass would consume all (or more than) the HCl, so no HCl would remain to titrate against the KOH, and the titration could not be carried out.
The mark scheme accepts several equivalent wordings: the HCl would no longer be in excess; HCl becomes the limiting reagent; no HCl would be left to do the titration; the metal carbonate would be in excess.
Key Takeaways
- A back-titration requires the added reagent to be in excess.
- Increasing the sample amount without increasing the reagent can make the reagent limiting.
Common Mistakes
- Thinking that more sample automatically improves accuracy.
- Not recognising that the HCl would become the limiting reagent.
Things to Be Careful About
- The mark scheme accepts any of the equivalent statements about excess/limiting reagent.
- You must make clear that the titration would not be possible because no HCl would remain.
In this experiment you will determine the relative atomic mass, , of metal by thermal decomposition of the same basic metal carbonate, , FB 1.
Method
- Weigh the empty crucible with its lid. Record the mass in the results section.
- Transfer all of the FB 1 from the container into the crucible.
- Weigh the crucible, lid and FB 1. Record the mass.
- Calculate the mass of FB 1 used. Record this mass in the space for other results.
- Place the crucible and contents on a pipe-clay triangle.
- Heat the crucible gently, with the lid on, for approximately 1 minute.
- Heat strongly, with the lid off, for a further 5 minutes.
- Replace the lid and leave the crucible to cool for at least 5 minutes.
During the cooling period, you may wish to begin work on Question 3.
- When the crucible is cool, weigh the crucible with its lid and contents. Record the mass.
- Place the crucible and contents on the pipe-clay triangle. Remove the lid.
- Heat strongly for a further 2 minutes.
- Replace the lid and leave the crucible to cool for at least 5 minutes.
- When the crucible is cool, reweigh the crucible with its lid and contents. Record the mass.
- Calculate the mass of residue obtained. Record this mass in the space for other results.
Results
mass of empty crucible and lid = ..........................
mass of crucible, lid and FB 1 (before heating) = ..........................
mass of crucible, lid and FB 1 (after first heating) = ..........................
mass of crucible, lid and FB 1 (after second heating) = ..........................
Other results
Answer
Record all four balance readings to the same number of decimal places (2 or 3 d.p.), each with a unit.
In the space for other results, calculate and record:
- mass of FB 1 used = mass(crucible + lid + FB 1) − mass(empty crucible + lid)
- mass of residue / MO = mass(crucible + lid + residue) − mass(empty crucible + lid)
Label these headings unambiguously and give the units. The fourth reading should be within +0.02 to −0.05 g of the third reading, and the mass of FB 1 used should be in the range 1.50–2.50 g.
See working: record all balance readings to same precision; calculate mass of FB 1 and residue.
Background Concept
This experiment uses thermal decomposition to find the relative atomic mass of a metal. A basic metal carbonate, , decomposes on heating to the metal oxide, carbon dioxide and water vapour. The mass lost is due to the escape of and , so by measuring the mass of sample and the mass of residue, the amount of carbonate can be found.
Understanding the Question
Part (a) is a practical procedure, not a calculation question. You are asked to carry out the heating and record your own readings. The marks come from the quality of your recording: consistent decimal places, clear headings, correct units, and correctly calculated masses of FB 1 and residue.
Approach
Weigh the empty crucible and lid, then the crucible with FB 1, then after each heating. The mass of FB 1 used is the difference between the second and first weighings. The mass of residue is the difference between the final weighing and the empty crucible. Record every reading to the same precision and with units.
Step-by-Step Reasoning
- Weigh the empty crucible with lid. This is the baseline.
- Add all of FB 1 and weigh again. Subtract the empty mass to find the mass of FB 1 used.
- Heat gently with the lid on, then strongly with the lid off, to drive off and .
- Cool and weigh. Heat again for 2 minutes and reweigh. The fourth reading should be close to the third, showing decomposition is complete.
- The residue is the metal oxide, . Its mass is the final weighing minus the empty crucible and lid.
- Use clear headings such as “mass of FB 1 used / g” and “mass of residue / g”, and give each balance reading a unit.
Key Takeaways
Accurate practical work depends on careful measurement and clear recording. Always use the same balance, cool the crucible before weighing, and record readings to a consistent number of decimal places.
Common Mistakes
- Recording one reading to 2 d.p. and another to 3 d.p.
- Forgetting units on balance readings or calculated masses.
- Calling the residue “FB 1” after heating.
- Not heating to constant mass, so the decomposition is incomplete.
Things to Be Careful About
- Use the mass of the empty crucible and lid consistently.
- The fourth reading should be within +0.02 to −0.05 g of the third; if it is lower, heat again.
- The mass of FB 1 used should be about 1.50–2.50 g; too little gives large percentage errors.
When FB 1 undergoes thermal decomposition, the products are the metal oxide, , carbon dioxide and water vapour.
Give the equation for the thermal decomposition of FB 1. Include state symbols.
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Answer
MCO3·M(OH)2(s) -> 2MO(s) + CO2(g) + H2O(g)
Background Concept
A basic metal carbonate has the formula . The dot means the compound contains one carbonate ion and two hydroxide ions combined with two metal ions. On strong heating it decomposes to the metal oxide, carbon dioxide and water vapour.
Understanding the Question
You are asked to write the balanced equation for the decomposition, including state symbols. The products are given, so the task is to balance the equation correctly.
Approach
Write the reactants and products, then balance the atoms. Count the metal atoms, carbon atoms, oxygen atoms and hydrogen atoms on each side.
Step-by-Step Reasoning
The reactant contains:
- 2 M atoms (one from and one from )
- 1 C atom
- 5 O atoms (3 from carbonate and 2 from hydroxide)
- 2 H atoms
Products:
- gives 2 M and 2 O
- gives 1 C and 2 O
- gives 2 H and 1 O
Total products: 2 M, 1 C, 5 O, 2 H. The equation balances with a coefficient of 2 on .
State symbols: the carbonate is a solid, the metal oxide is a solid, carbon dioxide and water vapour are gases.
Key Takeaways
When balancing equations with dot formulae, count the atoms in each part of the formula separately. The dot does not mean multiplication by a number unless shown.
Common Mistakes
- Writing only one instead of .
- Forgetting state symbols.
- Using (aq) for water vapour instead of (g).
Things to Be Careful About
- The water is produced as steam, so use (g).
- The metal oxide is a solid, so use (s).
The amount, in mol, of carbon dioxide produced is given by the following formula.
Calculate the amount, in mol, of carbon dioxide produced in (a).
amount of = .............................. mol
Working
Mass loss during heating = mass before heating − mass after final heating = .
Give the answer to 2–4 significant figures.
Answer
(candidate-dependent)
mol CO2 = mass loss / 62 (candidate-dependent)
Background Concept
The amount of a substance in moles is given by . During heating the mass lost is due to the escape of both carbon dioxide and water vapour, so the relevant molar mass is the sum of and .
Understanding the Question
You are told the formula for the amount of carbon dioxide produced. You need to use your mass loss from part (a) and calculate the number of moles, giving the answer to an appropriate number of significant figures.
Approach
Find the mass loss during heating, then divide by .
Step-by-Step Reasoning
- Mass loss = mass of FB 1 used − mass of residue.
- Total = 62
The answer should be given to 2–4 significant figures, matching the precision of the balance readings.
Key Takeaways
Mass loss in a decomposition can be converted to moles using the combined molar mass of the gaseous products.
Common Mistakes
- Using only and forgetting the water.
- Using the mass of the residue instead of the mass loss.
- Giving too many significant figures, such as 0.032456 mol.
Things to Be Careful About
- The mass loss must be in grams.
- Use the candidate’s own mass loss; there is no single correct numerical answer.
Calculate the relative formula mass, , of the basic metal carbonate.
of = ..............................
Working
From (b)(ii), .
Use the candidate’s mass of FB 1 and give the answer to 2–4 significant figures.
Answer
(candidate-dependent)
Mr = mass FB1 used / mol CO2 (candidate-dependent)
Background Concept
The relative formula mass, , is the mass of one mole of the substance in grams. Since one mole of produces one mole of , the amount of carbonate is equal to the amount of carbon dioxide.
Understanding the Question
You need to use the amount of carbon dioxide from (b)(ii) and the mass of FB 1 used to calculate of the basic carbonate.
Approach
Use .
Step-by-Step Reasoning
- From (b)(ii), you have the number of moles of .
- The same number of moles of was decomposed.
- Therefore .
- Give the answer to 2–4 significant figures.
Key Takeaways
The mole ratio between reactant and product is 1:1, so the amount of carbonate equals the amount of carbon dioxide.
Common Mistakes
- Using the mass of the residue instead of the mass of FB 1 used.
- Using the mass loss instead of the original sample mass.
- Forgetting to use the value from (b)(ii).
Things to Be Careful About
- The mass of FB 1 used is the mass before heating, not the mass after.
- Relative formula mass has no units, although it is numerically equal to the molar mass in g mol.
Use your answer to (b)(iii) to calculate the relative atomic mass, , of metal .
Show your working.
of = ..............................
Working
So
Substitute the value of from (b)(iii).
Answer
(candidate-dependent)
Ar = (Mr - 94)/2 (candidate-dependent)
Background Concept
The formula contains two metal atoms, one carbonate group and two hydroxide groups. Its relative formula mass can be written as .
Understanding the Question
You are asked to use your value of from (b)(iii) to find the relative atomic mass of metal M.
Approach
Write an expression for in terms of , then rearrange to solve for .
Step-by-Step Reasoning
- , so two hydroxide groups contribute 34.
- Rearranging:
- Substitute the value of from (b)(iii).
Key Takeaways
A formula unit containing two metal atoms means the metal contributes twice its relative atomic mass to .
Common Mistakes
- Forgetting the factor of 2 for the two metal atoms.
- Using but forgetting there are two hydroxide groups.
- Arithmetic errors when subtracting 94 and dividing by 2.
Things to Be Careful About
- The value of must come from (b)(iii).
- Check that your final is a sensible value for a metal.
Explain why the headings for the third and fourth readings in the results section in (a) are not suitable.
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Answer
After the first and second heatings the solid is no longer FB 1; it has decomposed to the metal oxide, MO (the residue). The headings should say “mass of crucible, lid and residue/MO”.
After heating the contents are metal oxide (residue), not FB 1.
Background Concept
When a substance is heated and decomposes, it changes into different substances. The original compound is no longer present.
Understanding the Question
The results table labels the third and fourth readings as “mass of crucible, lid and FB 1 (after first/second heating)”. These headings are unsuitable because after heating the solid is not FB 1.
Approach
Identify what the solid actually is after heating: the metal oxide residue.
Step-by-Step Reasoning
- FB 1 is .
- On heating it decomposes to , and .
- The and escape as gases, leaving only in the crucible.
- Therefore the headings should refer to the residue or metal oxide, not FB 1.
Key Takeaways
Labels in a results table must describe what is actually being weighed.
Common Mistakes
- Saying the mass changed without identifying the residue.
- Continuing to call the solid FB 1 after decomposition.
Things to Be Careful About
- Use the term “residue” or “metal oxide” in the heading.
State whether or not your experiment would be more accurate if the crucible and its contents were heated for a third time. Explain your answer by referring to your results in (a).
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Answer
Compare the third and fourth readings. If they are the same within 0.02 g, a third heating would not make the result more accurate because the mass is constant, so decomposition is complete. If the fourth reading is lower than the third, it would be more accurate because decomposition may not have been complete.
No, fourth reading within 0.02 g of third (or yes if fourth is lower).
Background Concept
Heating to constant mass is a way to check that decomposition is complete. If two consecutive weighings are the same, no more gas is being lost.
Understanding the Question
You must decide, using your own results, whether a third heating would improve accuracy and explain why.
Approach
Compare the third and fourth readings. If they are equal within 0.02 g, decomposition is complete and a third heating would not help. If the fourth is lower, decomposition was not complete and another heating would help.
Step-by-Step Reasoning
- Look at the third and fourth readings in your results.
- If they are the same within 0.02 g, the mass is constant, so all the and have been driven off. A third heating would not change the mass and would not improve accuracy.
- If the fourth reading is lower than the third, decomposition may still be occurring. A third heating would make the result more accurate because it would ensure constant mass.
Key Takeaways
The criterion for complete decomposition is constant mass on reheating.
Common Mistakes
- Giving an answer without referring to the actual readings.
- Saying “yes” or “no” without explaining why.
Things to Be Careful About
- The mark scheme accepts either conclusion as long as it matches your results and is explained.
A student carries out the experiments in Questions 1 and 2. The student expects the value of the of obtained by thermal decomposition in Question 2 to be more accurate than the value of the obtained by titration in Question 1.
State one reason why the student expects the experiment in Question 2 to be more accurate.
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Answer
Experiment 2 has fewer readings/steps, so there are fewer opportunities for error (or: the end-point is easier to judge because it is when the mass becomes constant).
Fewer steps/readings, so fewer sources of error.
Background Concept
The accuracy of an experiment depends on the number of measurements and the ease of judging the end-point. Fewer steps generally mean fewer opportunities for error.
Understanding the Question
You need to give one reason why the thermal decomposition method in Question 2 is expected to be more accurate than the titration in Question 1.
Approach
Compare the two methods in terms of number of readings, ease of end-point, and equipment precision.
Step-by-Step Reasoning
- The thermal decomposition method involves fewer readings and fewer steps than the titration, so there are fewer sources of error.
- The end-point of the decomposition is easy to judge: it is when the mass becomes constant. A titration end-point depends on judging a colour change, which is more subjective.
- A balance generally has a smaller percentage error than a burette or pipette.
Any one of these reasons is sufficient.
Key Takeaways
Accuracy is improved by reducing the number of steps and by using an end-point that is easy to judge.
Common Mistakes
- Giving a vague answer such as “human error”.
- Saying the experiment is more accurate without giving a reason.
Things to Be Careful About
- Give a specific, scientific reason, not a general statement.
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.
FB 5 is a compound containing one cation and one anion, both of which are listed in the Qualitative analysis notes.
Heat a small spatula measure of FB 5 in a hard-glass test-tube until no further change occurs.
Record your observations.
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Answer
- White solid / powder at the start
- On heating, condensation / steam produced
- Gas tested with moist red litmus paper — turns blue (ammonia)
- No residue at the end — the solid disappears
White solid; condensation/steam on heating; no residue; gas turns moist red litmus blue (NH3)
Background Concept
FB 5 is ammonium carbonate, . On strong heating it undergoes thermal decomposition:
All three products are gases at the temperature of a Bunsen flame, so nothing solid remains in the tube. The water vapour condenses to droplets (condensation) on the cooler upper part of the tube. Ammonia is an alkaline gas and turns moist red litmus paper blue. This is a Paper 3 qualitative-analysis task: the candidate heats a solid and records every observation at the stage it occurs.
Understanding the Question
Part (a)(i) asks you to heat a small spatula measure of FB 5 in a hard-glass test-tube until no further change occurs and to record all observations. Two marks are available, and the mark scheme requires two distinct observations per mark — so four creditable points are needed. The observations must include the appearance at the start, what happens during heating (condensation, gas), and what remains at the end.
Approach
Work through the heating in stages: note the initial appearance; watch for condensation as water vapour reaches the cooler part of the tube; test any gas evolved with moist red litmus paper; and finally check whether any solid residue remains. Record each observation at the stage it is made.
Step-by-Step Reasoning
- Initial appearance: FB 5 is a white solid/powder (or white/colourless crystals). This is the first observation.
- On gentle heating, water vapour is produced immediately and condenses as droplets (condensation/steam) on the cooler part of the tube. This is the second observation.
- A gas is evolved. Test it by holding moist red litmus paper at the mouth of the tube: it turns blue, identifying ammonia. This is the third observation.
- At the end, no residue remains — the solid has disappeared because it has decomposed completely into gases. This is the fourth observation.
Each of these is a separate creditable point; the mark scheme needs two points per mark.
Key Takeaways
- Thermal decomposition of ammonium carbonate gives only gases, so no residue remains.
- Ammonia is identified by turning moist red litmus paper blue.
- In Paper 3, record observations at the stage they occur and include the initial appearance.
Common Mistakes
- Writing only "gas formed" without testing or identifying it — the mark requires the litmus result.
- Not recording the condensation (water vapour) — an easy mark missed.
- Not noting that no residue remains.
- Using blue litmus paper — it is already blue, so the ammonia test shows no change; red litmus must be used.
Things to Be Careful About
- Use a hard-glass test-tube when heating a solid (as instructed in the paper's preamble).
- The mark scheme links "condensation/steam" to gentle heating — record it as water vapour being produced immediately on heating.
- Do not write "sublimes" unless you mean the solid disappears; the mark scheme allows "solid disappears / evaporates / sublimes".
Describe another test to positively identify the cation in FB 5.
Carry out your test and record your observations.
test ....................................................................................................................
observations ......................................................................................................................
Answer
- Warm FB 5 with aqueous sodium hydroxide
- Gas evolved turns moist red litmus paper blue — ammonia
- Therefore the cation is ammonium,
Warm with NaOH(aq): gas turns moist red litmus blue → NH4+
Background Concept
The ammonium ion, , is identified by warming the compound with aqueous sodium hydroxide. Hydroxide ions deprotonate the ammonium ion:
Ammonia is a soluble, alkaline gas that turns moist red litmus paper blue. This is the standard, specific test for the ammonium cation.
Understanding the Question
Part (a)(ii) asks for another test — separate from the heating in (a)(i) — to positively identify the cation in FB 5. One mark is available. The cation is ammonium, .
Approach
Use the classic ammonium test: warm a little FB 5 with aqueous NaOH and test the gas with moist red litmus paper.
Step-by-Step Reasoning
- Place a small amount of FB 5 in a test-tube and add aqueous sodium hydroxide.
- Warm the mixture gently (use a boiling tube as instructed when warming).
- Ammonia gas is evolved; hold a piece of moist red litmus paper at the mouth of the tube.
- The paper turns blue, confirming ammonia and therefore the ammonium ion.
Key Takeaways
- The ammonium test: warm with NaOH(aq); ammonia turns moist red litmus blue.
- This is a positive identification of , not just an observation.
Common Mistakes
- Not warming the mixture — the reaction is slow at room temperature.
- Using blue litmus (no visible change).
- Testing the gas with limewater instead of litmus (that is for ).
Things to Be Careful About
- The mark scheme requires both the reagent (aqueous NaOH) and the test result (gas turns red litmus blue).
- Warming must be gentle; use a boiling tube.
Put a depth of dilute hydrochloric acid in a test-tube. Add a small spatula measure of FB 5.
Record your observations.
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Answer
- Effervescence / fizzing on addition of dilute hydrochloric acid
- Colourless solution formed
- Gas tested with limewater
- Gas gives a white precipitate with limewater — carbon dioxide
Therefore the anion is carbonate, .
Effervescence; colourless solution; gas gives white ppt with limewater (CO2)
Background Concept
Carbonate ions react with acids to give carbon dioxide:
The effervescence (fizzing) is the visible sign. Carbon dioxide is identified by bubbling it through limewater (aqueous calcium hydroxide): it forms a white precipitate of calcium carbonate, turning the limewater milky:
Understanding the Question
Part (a)(iii) asks you to add dilute hydrochloric acid to a small spatula measure of FB 5 and record observations. Two marks are available, needing four creditable points: the effervescence, the colourless solution, the limewater test, and the white precipitate.
Approach
Add the acid, observe the effervescence and the solution colour, then test the gas with limewater.
Step-by-Step Reasoning
- On adding dilute HCl, vigorous effervescence/fizzing occurs — carbon dioxide is being released.
- The solid dissolves, giving a colourless solution (ammonium chloride forms).
- Collect or bubble the gas into limewater.
- The limewater turns milky — a white precipitate of forms — confirming , hence carbonate.
Key Takeaways
- Carbonate + acid ; test with limewater (white ppt/milky).
- Effervescence is the observation; the limewater test identifies the gas.
Common Mistakes
- Writing "gas formed" instead of "effervescence/fizzing" — the mark scheme rejects the vague phrase.
- Writing "milky" alone — the mark scheme requires "white precipitate/solid with limewater".
- Not testing the gas at all.
Things to Be Careful About
- The mark scheme explicitly says the limewater result must be "white ppt/solid", not just "milky".
- Record the stage: effervescence on addition; limewater test afterwards.
Answer
FB 5 is — ammonium carbonate.
(NH4)2CO3
Background Concept
The observations in (a)(i)–(a)(iii) identify the cation and anion of FB 5. The gas that turns red litmus blue (ammonia) on heating and with NaOH shows the cation is ammonium, . The effervescence with acid and the white precipitate with limewater show the anion is carbonate, . The formula must balance charges: is +1 and is −2, so two ammonium ions are needed per carbonate ion.
Understanding the Question
Part (a)(iv) asks you to deduce the formula of FB 5 from the observations. One mark.
Approach
Identify the cation and anion from the earlier tests, then combine them in the charge-balanced ratio.
Step-by-Step Reasoning
- From (a)(i) and (a)(ii): ammonia is evolved .
- From (a)(iii): is evolved with acid .
- Charge balance: , so the formula is , ammonium carbonate.
Key Takeaways
- Deduce ions from specific tests, then write a charge-balanced formula.
- Ammonium is written in parentheses when there is more than one: .
Common Mistakes
- Writing — charges do not balance.
- Forgetting the parentheses around .
Things to Be Careful About
- The formula must be , not or .
You will devise chemical tests to distinguish between the two possible identities given for each of compounds FB 6, FB 7, FB 8 and FB 9.
In each case you should:
- use a depth of the solution of the unknown compound in a test-tube
- use a boiling tube if you need to warm a mixture
- use a spatula measure of the unknown solid
- record details of your test(s) and your observations
- state your conclusion about the identity of the compound.
FB 6 is either aqueous chromium(III) sulfate or aqueous iron(II) sulfate.
FB 6 is ....................................................... .
Answer
- Add aqueous sodium hydroxide to FB 6
- Grey-green precipitate forms
- Precipitate dissolves in excess NaOH, giving a dark green solution
- Therefore FB 6 is chromium(III) sulfate,
Cr2(SO4)3 — grey-green ppt soluble in excess NaOH
Background Concept
Chromium(III) and iron(II) can be distinguished by their reactions with aqueous sodium hydroxide. gives a grey-green precipitate of which is amphoteric — it dissolves in excess NaOH to give a dark green solution containing . gives a dirty green precipitate of which is not soluble in excess NaOH. Alternatively, acidified potassium manganate(VII) is decolourised by (a reducing agent) but not by .
Understanding the Question
FB 6 is either aqueous chromium(III) sulfate or aqueous iron(II) sulfate. Devise a test, record observations, and state the conclusion. Two marks: M1 for the reagent, M2 for the observation and conclusion.
Approach
Choose the NaOH test: add aqueous NaOH, observe the precipitate, then add excess and test solubility. (The KMnO4 route is an alternative.)
Step-by-Step Reasoning
- Add aqueous NaOH to FB 6.
- A grey-green precipitate forms — this is ( would give a dirty green precipitate, similar at first glance).
- Add excess NaOH: the precipitate dissolves, giving a dark green solution. This is the key observation — is amphoteric.
- Conclusion: FB 6 is chromium(III) sulfate, .
Alternative: add acidified KMnO4 — it remains purple (not decolourised) because there is no to reduce it, so FB 6 is .
Key Takeaways
- is amphoteric: soluble in excess NaOH; is not.
- decolourises acidified KMnO4; does not.
Common Mistakes
- Stopping after the first precipitate without testing solubility in excess — the solubility is the discriminating observation.
- Confusing the colours: is dirty green and insoluble; is grey-green and soluble in excess.
Things to Be Careful About
- The mark scheme accepts either the NaOH route or the KMnO4 route; give the observation AND the conclusion for the mark.
FB 7 is either dilute hydrobromic acid or dilute nitric acid.
If you select a test that gives a negative result, then you must carry out a further test that gives a positive result.
FB 7 is ....................................................... .
Answer
- Heat FB 7 with excess aqueous sodium hydroxide and aluminium
- Gas evolved turns moist red litmus paper blue — ammonia
- Therefore FB 7 is nitric acid,
HNO3 — NH3 evolved with NaOH + Al, turns litmus blue
Background Concept
Nitrate ions are identified by reduction to ammonia. Heating the solution with aqueous sodium hydroxide and aluminium (or Devarda's alloy) reduces to :
The ammonia is detected by its alkaline smell and by turning moist red litmus paper blue. Hydrobromic acid contains bromide, which gives no such gas.
Understanding the Question
FB 7 is either dilute hydrobromic acid or dilute nitric acid. Devise a test, record observations, conclude. Two marks. The question notes that if the chosen test gives a negative result, a further positive test must be carried out.
Approach
Use the nitrate test: heat with excess NaOH and Al; test the gas with moist red litmus.
Step-by-Step Reasoning
- Add excess aqueous NaOH and a piece of aluminium to FB 7 in a boiling tube.
- Warm the mixture.
- If nitrate is present, ammonia is evolved; moist red litmus turns blue.
- Positive result nitrate present FB 7 is nitric acid, .
(If no ammonia were evolved, FB 7 would be HBr, and a further positive test — e.g. adding to give a cream precipitate of AgBr — would be needed.)
Key Takeaways
- Nitrate test: NaOH + Al, heat red litmus blue.
- The question's note about negative results means you must confirm with a positive test.
Common Mistakes
- Testing for a halide instead of nitrate (e.g. with ) — that would give a cream ppt for HBr and no ppt for , but the mark scheme wants the nitrate test.
- Not using aluminium — NaOH alone will not reduce nitrate to ammonia.
Things to Be Careful About
- Use excess NaOH and Al; heat the mixture (boiling tube).
- The gas must be identified by the litmus result.
FB 8 is either magnesium carbonate or zinc carbonate.
FB 8 is ....................................................... .
Answer
- Dissolve FB 8 in dilute sulfuric acid
- Add aqueous ammonia (or sodium hydroxide)
- White precipitate forms
- Precipitate dissolves in excess ammonia (or NaOH)
- Therefore FB 8 is zinc carbonate,
ZnCO3 — white ppt soluble in excess NH3/NaOH
Background Concept
Zinc and magnesium both form white hydroxides with aqueous ammonia or NaOH, but is amphoteric and dissolves in excess reagent (forming with ammonia or with NaOH), whereas is insoluble in excess. Since the carbonates are insoluble in water, they must first be dissolved in a mineral acid. Alternatively, heating the carbonate alone distinguishes them: ZnO is yellow when hot and white when cold, while MgO stays white.
Understanding the Question
FB 8 is either magnesium carbonate or zinc carbonate. Devise a test, record observations, conclude. Two marks.
Approach
Route 1: dissolve the carbonate in dilute acid, then add aqueous ammonia/NaOH and test solubility of the precipitate in excess. Route 2: heat the solid and observe the colour of the hot residue.
Step-by-Step Reasoning
Route 1:
- Dissolve FB 8 in a mineral acid (e.g. dilute ) — effervescence as is released.
- Add aqueous ammonia (or NaOH): a white precipitate forms.
- Add excess: the precipitate dissolves FB 8 is . ( would not dissolve in excess.)
Route 2: - Heat FB 8 alone in a hard-glass test-tube.
- Observe the hot residue: yellow ZnO FB 8 is . (MgO is white when hot.)
Key Takeaways
- is amphoteric (soluble in excess NH3/NaOH); is not.
- ZnO is yellow when hot, white when cold — a quick distinguishing test.
Common Mistakes
- Adding NaOH directly to the solid carbonate without dissolving first — carbonates are insoluble.
- Confusing which hydroxide dissolves in excess.
Things to Be Careful About
- The mark scheme accepts either route; give the observation and the conclusion.
- For route 2, the residue must be observed while hot (yellow).
FB 9 is either aqueous methanol or aqueous ethanol.
Note: FB 9 is flammable and should not be heated with a flame.
(When carrying out your test you may need to leave the reaction mixture to stand.)
FB 9 is ....................................................... .
Answer
- Add iodine solution and aqueous sodium hydroxide to FB 9
- Leave the mixture to stand (do not heat with a flame)
- Pale yellow / cream precipitate forms
- Therefore FB 9 is ethanol,
Ethanol (C2H5OH) — yellow ppt with I2/NaOH (iodoform test)
Background Concept
The iodoform test distinguishes ethanol from methanol. Ethanol, , contains the group. With iodine in alkaline solution (NaOH), it is oxidised to acetaldehyde and then iodinated to triiodoacetaldehyde, which is hydrolysed to iodoform, — a pale yellow/cream solid with a characteristic antiseptic smell. Methanol, , has no group and gives no iodoform. The test often needs time to stand for the precipitate to form.
Understanding the Question
FB 9 is either aqueous methanol or aqueous ethanol. Devise a test, record observations, conclude. Two marks. The question notes that FB 9 is flammable and must not be heated with a flame; the mixture may need to stand.
Approach
Use the iodoform test: add iodine solution and aqueous NaOH, leave to stand, look for a yellow precipitate.
Step-by-Step Reasoning
- Add iodine solution (or iodine in KI) and aqueous NaOH to FB 9.
- Leave the mixture to stand (do not heat with a flame — flammable).
- A pale yellow/cream precipitate of iodoform forms ethanol present FB 9 is ethanol, .
- Methanol would give no precipitate (no group).
Key Takeaways
- Iodoform test: + NaOH yellow ppt () for ethanol ( group), not methanol.
- The test may take time; leave to stand.
Common Mistakes
- Heating with a flame — the solution is flammable.
- Expecting an immediate result — the precipitate forms on standing.
- Confusing methanol and ethanol (methanol gives no iodoform).
Things to Be Careful About
- Must not heat with a flame (explicit instruction).
- The precipitate is pale yellow/cream, formed on standing.