Chemistry 9701/36 — October/November 2025
Cambridge AS Level · Advanced Practical Skills · worked solutions for every part, with the mark scheme
Topics Manipulation, Measurement and Observation · Analysis, Conclusions and Evaluation · Presentation of Data and Observations · Qualitative Analysis
Quantitative analysis
Read through the whole method before starting any practical work. Where appropriate, prepare a table for your results in the space provided.
Show the precision of the apparatus you used in the data you record.
Show your working and appropriate significant figures in the final answer to each step of your calculations.
Many hydrated salts decompose when heated, losing water of crystallisation.
The number of molecules of water of crystallisation, , in hydrated aluminium sulfate can be determined by heating until it becomes anhydrous: is an integer.
FB 1 is hydrated aluminium sulfate, .
Method
- Weigh the crucible with its lid. Record the mass.
- Add between 1.80 and 2.00 g of FB 1 to the crucible.
- Weigh the crucible, lid and FB 1. 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 5 minutes.
- Replace the lid and leave the crucible and residue to cool for at least 5 minutes.
While the crucible is cooling, you should begin work on Questions 2 or 3.
- Reweigh the crucible and contents with the lid on. Record the mass.
- Remove the lid. Heat the crucible and contents strongly for a further 2 minutes.
- Replace the lid and leave the crucible and residue to cool for at least 5 minutes.
- Reweigh the crucible and residue with the lid on. Record the mass.
- Calculate and record the mass of FB 1 used, the mass of residue obtained and the mass lost during heating.
Results
Answer
Results Table
| Measurement | Mass / g |
|---|---|
| Mass of empty crucible + lid | [e.g. 25.40] |
| Mass of crucible + lid + FB 1 | [e.g. 27.30] |
| Mass of crucible + lid + residue (after 1st heating) | [e.g. 26.50] |
| Mass of crucible + lid + residue (after 2nd heating) | [e.g. 26.48] |
| Mass of FB 1 used | [e.g. 1.90] |
| Mass of residue obtained | [e.g. 1.08] |
| Mass of water lost | [e.g. 0.82] |
Note: All mass readings must be recorded to the same number of decimal places (2 or 3). The mass after the 2nd heating should be within g and g of the mass after the 1st heating to indicate constant mass has been reached. The mass of FB 1 used should be between g and g.
See working
Background Concept
Gravimetric analysis relies on precise mass measurements to determine the composition of a substance. When determining the formula of a hydrated salt, the salt is heated to drive off water of crystallisation. The process must continue until the mass of the anhydrous residue is constant, indicating that all water has been removed. This is achieved by heating, cooling, and weighing repeatedly until successive weighings agree within a small tolerance.
Understanding the Question
This part asks you to record the data obtained from the practical method described. The method involves weighing the crucible, adding the hydrated salt, heating to remove water, and re-weighing. You need to present this data clearly in a table, showing the raw readings and the calculated differences (mass of salt, mass of residue, mass of water lost).
Approach
- Table Structure: Create a table with two columns: 'Measurement' and 'Mass / g'.
- Raw Readings: Record four specific mass readings:
- Empty crucible + lid.
- Crucible + lid + hydrated salt (FB 1).
- Crucible + lid + residue (after 1st heating).
- Crucible + lid + residue (after 2nd heating).
- Precision: Ensure all readings are recorded to the same number of decimal places (typically 2 or 3, depending on the balance used).
- Calculations: Subtract the raw readings to find:
- Mass of FB 1 = (Crucible + FB 1) - (Empty Crucible).
- Mass of residue = (Crucible + residue after 2nd heating) - (Empty Crucible).
- Mass of water lost = (Mass of FB 1) - (Mass of residue).
- Validity Check: Ensure the mass of FB 1 is within the required range ( g) and that the two residue weighings are close enough to suggest constant mass.
Step-by-Step Reasoning
- Recording Readings: The mark scheme requires seven unambiguous headings. This includes the four raw weighings and the three calculated masses. Units must be clearly displayed (e.g., 'Mass / g').
- Precision: If the balance reads to g, record all masses to two decimal places (e.g., g, not g). This demonstrates awareness of apparatus precision.
- Constant Mass: The difference between the 1st and 2nd heating weighings should be small. The mark scheme specifies the 2nd reading should be within g and g of the 1st. This tolerance accounts for minor experimental variations while ensuring decomposition is complete.
- Calculated Masses:
- Mass of FB 1: Subtract the empty crucible mass from the crucible + FB 1 mass. This value must be between g and g as per the method instructions.
- Mass of Residue: Subtract the empty crucible mass from the final crucible + residue mass.
- Mass of Water: Subtract the mass of the residue from the mass of FB 1.
Key Takeaways
- Always record raw data before calculating derived values.
- Maintain consistent decimal places throughout a set of measurements to reflect the precision of the instrument.
- 'Heating to constant mass' is verified by comparing successive weighings; a small difference confirms completion of the reaction.
Common Mistakes
- Inconsistent decimal places (e.g., and in the same column).
- Failing to include units in the table headings.
- Using the mass after the first heating to calculate the final results instead of the mass after the second heating (which confirms constant mass).
- Mass of FB 1 falling outside the g range.
Things to Be Careful About
- Ensure the 'Mass of residue' calculation uses the reading after the second heating.
- Check that the calculated mass of water is positive.
- The accuracy marks (IV and V) depend on the ratio of Mass FB 1 / Mass Residue being within specific ranges ( and respectively). This ratio is essentially determined by the value of in the formula, so accurate measurement is crucial for high marks.
Calculations
Calculate the amount, in mol, of water of crystallisation lost during the thermal decomposition of FB 1.
amount of lost = .............................. mol
Working
Using the example values from part (a):
Answer
0.0455 mol
0.0455 mol
Background Concept
The amount of substance in moles is calculated by dividing the mass of the substance by its molar mass (). For water (), the molar mass is approximately (). In this experiment, the mass of water lost during heating corresponds directly to the water of crystallisation in the hydrated salt.
Understanding the Question
You need to calculate the number of moles of water that evaporated from the sample. This is derived from the 'Mass of water lost' calculated in part (a).
Approach
- Identify the mass of water lost from your results in part (a).
- Divide this mass by the molar mass of water ( or ).
- Report the answer to 2-4 significant figures.
Step-by-Step Reasoning
- Mass of Water: From part (a), the mass of water lost is the difference between the initial mass of FB 1 and the final mass of the anhydrous residue. In the example, this was g.
- Molar Mass: .
- Calculation:
- Significant Figures: The input mass ( g) has 2 significant figures, so the answer should ideally be given to 2 or 3 significant figures. mol is appropriate.
Key Takeaways
- Always use the correct molar mass for the substance being converted to moles.
- The mass lost in this specific experiment is purely water.
Common Mistakes
- Using the mass of the residue instead of the mass of water lost.
- Using the molar mass of the hydrated salt instead of water.
- Incorrect significant figures (e.g., too many or too few).
Things to Be Careful About
- Ensure you are using the mass of water lost, not the mass of the salt.
- Check the molar mass of water used ( vs ) is consistent with the rest of the calculation.
Calculate the amount, in mol, of anhydrous residue produced by the thermal decomposition. Show your working.
amount of produced = .............................. mol
Working
Using the example values from part (a):
Answer
0.00316 mol
0.00316 mol
Background Concept
The anhydrous residue left after heating is aluminium sulfate, . To find the moles of this substance, we divide its mass by its molar mass. The molar mass is calculated by summing the atomic masses of all atoms in the formula unit.
Understanding the Question
Calculate the moles of anhydrous aluminium sulfate produced. This requires the mass of the residue from part (a) and the molar mass of .
Approach
- Identify the mass of the residue from part (a).
- Calculate the molar mass of .
- Divide the mass of the residue by the molar mass.
- Report the answer to 2-4 significant figures.
Step-by-Step Reasoning
- Mass of Residue: From part (a), the mass of the anhydrous residue is g in the example.
- Molar Mass Calculation:
- Al:
- S:
- O:
- Total . The mark scheme uses .
- Calculation:
- Significant Figures: mol (3 s.f.) is appropriate.
Key Takeaways
- Accurate calculation of molar mass is essential for stoichiometric problems.
- The residue is the anhydrous salt, not the hydrated form.
Common Mistakes
- Using the initial mass of FB 1 instead of the residue mass.
- Incorrect molar mass calculation (e.g., forgetting there are 12 oxygen atoms).
- Arithmetic errors in division.
Things to Be Careful About
- Ensure the molar mass used matches the atomic masses provided in the question data booklet or standard values ( is the standard value here).
- Keep sufficient precision in intermediate steps to avoid rounding errors in the final ratio calculation.
Calculate the number of molecules of water of crystallisation in the formula of hydrated aluminium sulfate, .
= ..............................
Working
Using the example values from (b)(i) and (b)(ii):
Rounding to the nearest integer:
Answer
14
14
Background Concept
The formula of a hydrated salt indicates the ratio of moles of water to moles of anhydrous salt. By calculating the moles of water lost and the moles of anhydrous salt remaining, we can determine this ratio. The value of must be an integer, so we round the calculated ratio to the nearest whole number.
Understanding the Question
Determine the value of in . This is done by dividing the moles of water (from b.i) by the moles of anhydrous salt (from b.ii).
Approach
- Take the mole values calculated in parts (b)(i) and (b)(ii).
- Divide the moles of water by the moles of anhydrous salt.
- Round the result to the nearest integer.
Step-by-Step Reasoning
- Moles of Water: mol (from b.i).
- Moles of Anhydrous Salt: mol (from b.ii).
- Ratio Calculation:
- Rounding: The question states is an integer. is closest to . (Note: Actual hydrated aluminium sulfate is often or , but experimental error or specific hydrate forms can lead to other values. Based on the example data provided, 14 is the result. In a real exam, your value depends on your specific measurements. The mark scheme expects the calculation from your numbers).
Key Takeaways
- The coefficient in a chemical formula represents a mole ratio.
- Experimental data often yields a non-integer ratio due to errors; rounding to the nearest integer is the standard procedure.
Common Mistakes
- Dividing moles of salt by moles of water (inverting the ratio).
- Failing to round to the nearest integer.
- Using masses directly instead of converting to moles first.
Things to Be Careful About
- Ensure you use the unrounded mole values from the previous steps to minimize rounding errors.
- Check if the result is reasonably close to a known hydrate (e.g., 16, 18) to validate your experimental technique, though you must report the calculated value rounded to the nearest integer.
State how the appearance of the residue compares with the appearance of the hydrated solid before heating.
Answer
The hydrated solid (FB 1) is crystalline / finely divided powder, whereas the residue is lumpy / has a 'crusty' surface / has a 'skin'.
Hydrated solid is crystalline/powder; residue is lumpy/crusty
Background Concept
Hydrated salts typically form well-defined crystals or fine powders due to the ordered lattice structure incorporating water molecules. When heated, the loss of water can disrupt this structure, causing the remaining anhydrous salt to sinter or fuse into a harder, less defined mass, often described as lumpy or having a crust.
Understanding the Question
Compare the visual appearance of the starting material (FB 1) with the final residue after heating.
Approach
Describe the texture/form of the initial solid and contrast it with the final solid.
Step-by-Step Reasoning
- FB 1 (Hydrated): Usually appears as a white, crystalline solid or a fine powder.
- Residue (Anhydrous): After strong heating, the structure collapses or fuses. It often appears as a white, lumpy solid, sometimes with a 'crusty' top layer or 'skin' formed by the melting and resolidifying of surface particles.
Key Takeaways
- Physical appearance changes can indicate chemical or structural changes during heating.
Common Mistakes
- Stating only that the color changes (both are typically white).
- Failing to mention the texture difference (powder vs. lump/crust).
Things to Be Careful About
- Use descriptive terms like 'crystalline', 'powder', 'lumpy', 'crusty', or 'skin' as these are the key observation points.
Suggest why the crucible and contents are heated with the crucible lid on for the first two minutes of the experiment.
Answer
To prevent the solid (or solution formed during initial heating) from spitting / frothing out of the crucible.
To prevent spitting/frothing out
Background Concept
When hydrated salts are heated, they often dissolve in their own water of crystallisation before the water evaporates. This can cause vigorous boiling or 'spitting', where droplets of the solution are ejected from the crucible. This leads to a loss of sample mass that is not due to water evaporation, causing experimental error.
Understanding the Question
Explain why the crucible is heated with the lid on for the first two minutes.
Approach
Identify the physical phenomenon occurring during gentle heating (dissolution/spitting) and the consequence of not using a lid (loss of solid).
Step-by-Step Reasoning
- Initial Heating: Gentle heating causes the hydrated salt to melt/dissolve in its water of crystallisation.
- Risk: This liquid can bubble or spit, throwing solid material out of the crucible.
- Function of Lid: The lid acts as a barrier, keeping the solid inside the crucible even if spitting occurs.
- Subsequent Heating: Once the water has largely evaporated and the solid is dry, the lid is removed to allow remaining water vapor to escape freely during strong heating.
Key Takeaways
- Experimental steps are designed to minimize systematic errors (like loss of sample).
- 'Spitting' is a common issue when heating hydrated salts.
Common Mistakes
- Saying it prevents heat loss (the lid is removed later, so this isn't the primary reason for the initial gentle heating phase).
- Saying it prevents contamination from the air (less relevant than sample loss).
Things to Be Careful About
- Focus on the loss of solid material, not just water vapor.
A student carries out the experiment in (a), but obtains a value for that is higher than expected. The student suggests that this could be because the hydrated aluminium sulfate is contaminated with some anhydrous aluminium sulfate.
State whether the student's suggestion is correct.
Explain your answer.
Answer
The student's suggestion is not correct.
If the sample contains anhydrous aluminium sulfate, the mass of water lost will be lower (or the mass of residue higher) than expected for pure hydrated salt. This results in a lower mole ratio of water to salt (), not a higher one.
Not correct
Background Concept
The value of is calculated as . Contamination affects the numerator and denominator differently depending on the nature of the contaminant. Anhydrous salt contributes to the 'residue' mass but adds no 'water' mass.
Understanding the Question
A student claims that contamination with anhydrous salt causes an overestimation of . We must verify if this logic holds.
Approach
- Assume the sample is a mix of hydrated salt and anhydrous salt.
- Determine how this affects the measured 'Mass of water lost'.
- Determine how this affects the measured 'Mass of residue'.
- Analyze the effect on the ratio .
Step-by-Step Reasoning
- Effect on Water Mass: Anhydrous salt contains no water. Therefore, a contaminated sample will release less water per gram of sample than pure hydrated salt. The measured 'Mass of water lost' will be lower than expected for the mass of FB 1 taken.
- Effect on Residue Mass: The anhydrous contaminant remains as residue. This means the 'Mass of residue' will be higher than expected for the amount of water lost.
- Effect on Moles:
- will be lower.
- (calculated from residue mass) will be higher.
- Effect on Ratio : Since the numerator decreases and the denominator increases, the value of will decrease.
- Conclusion: The student obtained a higher . Contamination with anhydrous salt causes a lower . Therefore, the student's suggestion is incorrect. (A higher would be caused by contamination with a more hydrated salt or incomplete drying of the residue, or loss of salt during heating).
Key Takeaways
- Always trace the effect of an error through the calculation steps.
- Contamination with the anhydrous form reduces the water content of the sample.
Common Mistakes
- Assuming any contamination increases the residue mass and therefore increases (forgetting the water mass also changes).
- Confusing the direction of the error (thinking anhydrous contamination leads to higher ).
Things to Be Careful About
- Clearly state whether the suggestion is correct or incorrect.
- Provide the reasoning linking the contamination to the change in measured masses and the final ratio.
The number of molecules of water of crystallisation, , in hydrated iron(II) sulfate can be determined by titration with acidified potassium manganate(VII): is an integer.
FB 2 is aqueous iron(II) sulfate, containing of .
FB 3 is aqueous potassium manganate(VII), containing of .
FB 4 is sulfuric acid, .
Method
- Fill the burette with FB 3.
- Pipette of FB 2 into a conical flask.
- Use the measuring cylinder to transfer approximately 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 below, all your burette readings and the volume of FB 3 added in each accurate titration.
Answer
Rough titre = 24.60 cm3.
Accurate titration results:
| Trial 1 | Trial 2 | |
|---|---|---|
| initial burette reading / cm3 | 0.00 | 24.50 |
| final burette reading / cm3 | 24.50 | 49.00 |
| titre / cm3 | 24.50 | 24.50 |
Both accurate titres are within 0.10 cm3 of each other, so they are concordant.
See table: accurate titres 24.50 cm3 and 24.50 cm3
Background Concept
This is a redox titration. The burette delivers FB 3 (), the pipette measures a fixed of FB 2 into the flask, and FB 4 () provides the acidic conditions needed for manganate(VII) to act as an oxidising agent. The end point is the first permanent pink colour caused by a tiny excess of manganate(VII). The candidate does not need to know the exact chemistry to perform the titration, but should record readings sensibly and repeat until results agree.
Understanding the Question
The part has no calculation. It asks the candidate to fill the burette, do a rough titration, then carry out as many accurate titrations as necessary and record all burette readings and titres in a suitable table. The table must show initial/final readings and the volume added, each with units, and the readings must show the precision of the burette.
Approach
Use the rough titre to know roughly where the end point is. Then repeat the titration, adding FB 3 dropwise near the end point, until two accurate titres agree to within . For each accurate titration, record the initial and final burette readings, then subtract: titre = final reading initial reading.
Step-by-Step Reasoning
- Fill the burette with FB 3 and remove any air bubble from the jet.
- Run a rough titration and record the rough titre, e.g. .
- Refill the burette and carry out accurate titrations.
- For each accurate titration, record:
- initial burette reading, e.g. cm3;
- final burette reading, e.g. cm3;
- titre cm3.
- Repeat until two accurate titres are concordant. In the example, the two accurate titres are both cm3, which are well within cm3 of each other.
- Include headings and units in the table. The rough titre is not included in the mean.
Key Takeaways
Always record the quantity and unit in every table heading. Estimate burette readings to the nearest cm3 and repeat titrations until two agree closely. Concordance is the key to a reliable mean titre.
Common Mistakes
- Recording only the titre and not the initial and final burette readings.
- Omitting units from table headings.
- Using the rough titre as an accurate result.
- Making only one accurate titration when the instructions ask for consistent results.
- Writing burette readings to inconsistent numbers of decimal places.
Things to Be Careful About
Read the bottom of the meniscus. A burette can be read to the nearest cm3, so readings such as cm3 are appropriate. Check that every titre is calculated correctly from the recorded readings and that the two concordant values are clearly identifiable.
From your accurate titration results, calculate a suitable mean value to be used in your calculations.
Show clearly how you obtained this value.
of FB 2 required .............................. of FB 3.
Working
Using the two concordant accurate titres:
mean titre cm3
Answer
Mean titre = 24.50 cm3.
24.50 cm3
Background Concept
A mean should only be calculated from accurate titrations that agree closely with one another. The rough titre is ignored because it was not performed carefully enough. The mean titre is then used in all later calculations.
Understanding the Question
Part (b) asks for one representative mean value from the accurate results, with working shown. The mean must be based on two or more accurate titrations whose total spread is no more than cm3, and it should be quoted to 2 decimal places.
Approach
Look at the accurate titrations only. If there are more than two, select the two closest values that are concordant. Add the selected titres and divide by the number used. Show the sum, division, and final value to 2 d.p.
Step-by-Step Reasoning
- The accurate titres from part (a) are cm3 and cm3.
- They are within cm3 of each other, so both can be used.
- Mean cm3.
- The answer is already to 2 d.p.
Key Takeaways
The mean titre is a processing step, not an experimental result. Only concordant accurate titrations should be averaged, and the selected readings should be clearly identified in the answer.
Common Mistakes
- Including the rough titre in the mean.
- Averaging titres that are not concordant, e.g. values more than cm3 apart.
- Quoting the mean to only 1 decimal place.
- Not showing any working, so the mark cannot be credited.
Things to Be Careful About
The final mean must be rounded to the nearest cm3. If three titrations are done and two are concordant but the third is not, ignore the outlier and average the two concordant values.
Calculations
Calculate the amount, in mol, of potassium manganate(VII) present in the volume of FB 3 in (b). Show your working.
amount of = .............................. mol
Working
Amount of used:
Answer
Amount of mol (3 s.f.)
5.40 x 10^-4 mol
Background Concept
The concentration of FB 3 is given as a mass concentration in . To find the amount in mol, first divide by the molar mass to get a concentration in , then multiply by the volume used in dm3.
Understanding the Question
Part (c)(i) asks for the amount of in the volume found in part (b). The only extra information needed is the molar mass of , which can be calculated from .
Approach
- Calculate .
- Convert to by dividing by .
- Convert the mean titre from cm3 to dm3 by dividing by 1000.
- Multiply the molar concentration by the volume in dm3.
Step-by-Step Reasoning
.
Concentration of :
Volume used: .
Amount:
A suitable final answer is mol to 3 s.f. or mol to 4 s.f.
Key Takeaways
Whenever a solute concentration is given in , convert it to using molar mass before finding . Volumes in cm3 must be divided by 1000 before using .
Common Mistakes
- Using as the concentration in without dividing by .
- Leaving the titre in cm3 instead of converting to dm3.
- Using the rough titre rather than the mean titre from part (b).
- Quoting too many or too few significant figures.
Things to Be Careful About
Use consistently. Keep more significant figures during the calculation and only round at the final answer. The mark scheme accepts 3 or 4 significant figures for the final value.
An incomplete equation for the reaction of iron(II) ions with manganate(VII) ions is shown. The mole ratio of and is given correctly.
Complete the equation.
Answer
5Fe2+(aq) + MnO4-(aq) + 8H+(aq) -> 5Fe3+(aq) + Mn2+(aq) + 4H2O(l)
Background Concept
In acidified manganate(VII), the oxidising agent in this titration is . It is reduced to , while iron(II) is oxidised to iron(III). The equation must balance for atoms and charge.
Understanding the Question
The mole ratio of to is already given as . The task is to complete the coefficients in front of , , and .
Approach
Write the two half-equations, balance electrons, then combine them. The oxidation half-equation releases one electron per ; the reduction half-equation needs five electrons, so five iron(II) ions are oxidised.
Step-by-Step Reasoning
Oxidation:
Reduction:
Multiply the oxidation half-equation by 5:
Add the two half-equations, cancelling 5 electrons:
Check: on the left, total charge is . On the right, . Atoms are also balanced.
Key Takeaways
The redox equation is the basis of the mole ratio used in (c)(iii): 5 mol react with 1 mol . Balancing redox equations always requires equal numbers of electrons transferred.
Common Mistakes
- Writing instead of .
- Forgetting .
- Balancing atoms but not charge.
- Confusing the oxidation and reduction half-equations.
Things to Be Careful About
Make sure the coefficient of is 5, not 1. The equation needs both atom balance and charge balance.
Calculate the concentration of iron(II) sulfate, in , in FB 2.
concentration of = ..............................
Working
Amount of in cm3 of FB 2:
Volume of FB 2 = .
Concentration of :
Answer
Concentration of mol dm3 (3 s.f.)
0.108 mol dm^-3
Background Concept
The balanced equation shows that 5 mol of react with 1 mol of . Therefore the amount of iron(II) in the 25.0 cm3 sample is five times the amount of manganate(VII) that reacted. Concentration is then moles divided by volume in dm3.
Understanding the Question
Part (c)(iii) asks for the concentration of iron(II) sulfate in FB 2 in . The volume used in the titration was cm3, and the amount of was found in (c)(i).
Approach
- Multiply the amount of by 5.
- Divide by dm3.
Step-by-Step Reasoning
From (c)(i), the amount of used is mol.
Amount of :
This amount was present in cm3, i.e. dm3.
Concentration:
A suitable final answer is mol dm3 to 3 s.f. or mol dm3 to 4 s.f. The unrounded value is used in the next part.
Key Takeaways
The mole ratio comes directly from the balanced redox equation. Always convert a pipette volume in cm3 to dm3 before dividing to find concentration.
Common Mistakes
- Forgetting to multiply the amount by 5.
- Dividing by instead of .
- Quoting the volume as dm3 without conversion.
- Rounding to 1 or 6 significant figures.
Things to Be Careful About
Use the unrounded amount from (c)(i) in the calculation. If the rounded value is used, the concentration becomes mol dm3, which is still acceptable for part (c)(iv).
Working
Answer
7
Background Concept
FB 2 contains of . Dividing a mass concentration in by a molar concentration in gives the molar mass in . The hydrated salt has molar mass , where is the of anhydrous and is the of one water molecule.
Understanding the Question
The aim of the experiment is to determine the integer value of . We now know the molar concentration of hydrated iron(II) sulfate from part (c)(iii) and the mass concentration from the original data. This gives of the hydrate, from which can be solved.
Approach
- Use .
- Subtract from this value to find the total molar mass of water in one mole of hydrate.
- Divide by 18.0.
- Give the answer as the nearest integer.
Step-by-Step Reasoning
Using the unrounded concentration from (c)(iii), mol dm3:
Mass of water per mole of hydrate:
Moles of water per mole of hydrate:
So . This is consistent because has .
Key Takeaways
The value of is found indirectly: titration gives the molar concentration, and the known mass concentration gives the molar mass. The final answer must be reported as an integer.
Common Mistakes
- Using the amount of instead of the concentration of when finding .
- Substituting as the hydrated instead of the anhydrous .
- Rounding the concentration to only 1 or 2 significant figures before calculating .
- Leaving as or instead of giving the integer 7.
Things to Be Careful About
Use the most precise value available from part (c)(iii). The mark scheme allows up to 4 significant figures in intermediate answers, and requires the final to be an integer.
A student suggests that the experiment is more accurate if FB 4 is measured with a pipette.
State whether you agree with the student.
Explain your answer.
Answer
Disagree. The is used in excess, so it is not the limiting reagent. The exact volume of acid added does not affect the titre, provided enough is present.
Disagree: H2SO4 is in excess, so exact volume does not matter.
Background Concept
In a titration, the amount of the limiting reagent determines the volume of titrant needed. Here FB 4, sulfuric acid, provides the acidic medium but is not consumed stoichiometrically in the same way as iron(II). It must simply be present in excess so that all the iron(II) reacts completely with manganate(VII) under acidic conditions.
Understanding the Question
The student proposes that using a pipette to measure FB 4 would make the experiment more accurate. The question asks whether this is correct and why. The answer depends on whether the exact volume of FB 4 affects the titre.
Approach
Determine the role of FB 4. Because the acid is in excess, a small variation in its volume changes the amount of acid present but not the amount of iron(II) titrated. Therefore pipetting it does not improve the result.
Step-by-Step Reasoning
- The endpoint depends on the amount of in the 25.0 cm3 sample.
- The amount of needed depends only on the amount of , provided enough is present.
- FB 4 is deliberately added in excess, so its exact volume is not important.
- Using a measuring cylinder rather than a pipette introduces no error into the determination.
- Therefore the student is incorrect.
Key Takeaways
Only the limiting reagent needs to be measured accurately in a titration. A reagent added in excess affects neither the stoichiometry nor the endpoint, as long as it is genuinely in excess.
Common Mistakes
- Agreeing with the statement and suggesting the acid volume needs to be exact.
- Saying the acid affects the colour at the endpoint instead of addressing the excess.
- Giving an answer such as “it would be more accurate” without explaining why the acid volume is not limiting.
Things to Be Careful About
Make clear that the acid is not the limiting reagent. The mark scheme explicitly accepts “used in excess” but not vague comments about accuracy alone.
Aqueous solutions of iron(II) sulfate are slowly oxidised by air.
State what effect this oxidation would have on the value of calculated in (c)(iv).
Explain your answer.
Answer
The calculated value of would be greater than the true value.
Some is oxidised to by air. This lowers the amount of available, so less is needed and the titre is lower than expected. The calculation then gives a lower apparent concentration of , a larger apparent , and hence a larger value of .
y would be greater.
Background Concept
Iron(II) is slowly oxidised to iron(III) by oxygen in the air:
Only iron(II) is oxidised by manganate(VII) in this titration. Any iron(III) present does not react, so the amount of manganate(VII) needed is reduced.
Understanding the Question
If the iron(II) sulfate solution has been partially oxidised before titration, the experiment will not give the true concentration of as initially prepared. The question asks whether the calculated value of in (c)(iv) will be too high or too low, and why.
Approach
Trace the effect through every part of the calculation:
- Oxidation lowers the amount of in the sample.
- The titre of is therefore lower.
- Part (c)(iii) gives a lower calculated concentration of .
- Part (c)(iv) divides the fixed mass concentration by this lower concentration, giving a larger apparent .
- A larger means a larger value of .
Step-by-Step Reasoning
The original solution was made from of hydrated iron(II) sulfate. If some iron(II) oxidises, the number of moles of reacting with is less than expected, so the calculated is larger. Since is obtained from:
a larger gives a larger . Thus the effect is that is greater than the true value.
Key Takeaways
Air oxidation of iron(II) is a real source of systematic error. Any error that lowers the titre leads to a lower apparent concentration and therefore a higher apparent molar mass of the analyte. Always trace an experimental error through the full calculation to decide its effect on the final answer.
Common Mistakes
- Saying would be smaller, because it is easy to confuse a lower titre with a lower .
- Saying the titre would be higher because “more oxidation increases the value”.
- Giving only “the titre is lower” without linking it to the final value of .
Things to Be Careful About
The answer must state that does not react with under these conditions, so the measured amount of reducible iron is lower. The mark scheme accepts any one linked consequence such as “lower titre” or “fewer moles of KMnO4,” but the final direction must be that is greater.
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.
Use very small quantities of solid FB 5 and carry out each of the tests described in Table 3.1.
Identify any gases produced.
Table 3.1
| test | observations |
|---|---|
| Test 1 Pour a 1 cm depth of aqueous iron(III) chloride into a test-tube. Add a small spatula measure of FB 5. Leave the test-tube to stand for about 3 minutes, then pour off some of the solution into another test-tube and add aqueous sodium hydroxide. | |
| Test 2 Pour a 1 cm depth of aqueous copper(II) sulfate into a test-tube. Add a small quantity of FB 5. Leave the test-tube to stand for about 3 minutes. | |
| Test 3 Pour a 1 cm depth of dilute sulfuric acid into a test-tube and add 2 drops of aqueous copper(II) sulfate. Then add a small quantity of FB 5. |
Answer
Test 1 ()
- Solution becomes colourless / paler yellow / pale green
- Fizzing / effervescence
- Adding gives a (pale) green / green-white precipitate
- Precipitate is insoluble in excess / precipitate turns brown at the surface
Test 2 ()
- Pink-brown solid / precipitate / residue forms
- Solution gets paler (blue) / turns colourless
- Mixture gets hotter
Test 3 ( + )
- Fizzing / effervescence
- Gas pops with a lighted splint
- Gas is hydrogen
See working — observations recorded for Tests 1, 2 and 3
Background Concept
This is a qualitative analysis exercise. The unknown solid FB 5 is zinc metal (), though you must deduce this from your observations. The key chemistry is the reactivity series: zinc sits above both iron and copper, so it displaces them from their salt solutions. Zinc also reacts with dilute acids to liberate hydrogen gas. The three tests probe these properties through visible changes — colour changes in solution, formation of precipitates, evolution of gas, and temperature changes.
Understanding the Question
You are asked to perform three tests on a small quantity of FB 5 and record all observations in Table 3.1. Test 1 uses iron(III) chloride solution, Test 2 uses copper(II) sulfate solution, and Test 3 uses dilute sulfuric acid with two drops of copper(II) sulfate. The general instructions emphasise recording the stage at which each observation is made — e.g. "on adding FB 5" versus "on adding " — and to write "no change" where nothing happens.
Approach
Work through each test using the reactivity series. Predict what zinc does in each solution: displacement of iron, displacement of copper, and reaction with acid. Then translate each chemical change into observable signs: colour changes, precipitates, gas bubbles, temperature rise. For Test 1, remember the second stage — pouring off some solution and adding — tests for the cation left in solution.
Step-by-Step Reasoning
Test 1: Zinc is more reactive than iron, so . The yellow ions are removed from solution, so the solution becomes paler or colourless. Some fizzing may occur as zinc reacts with any trace acid in the solution. When is added to the poured-off solution (which contains and possibly ), a pale green or green-white precipitate of forms; this is insoluble in excess . The precipitate may turn brown at the surface as is oxidised to by air.
Test 2: Zinc displaces copper: . A pink-brown solid (copper metal) forms. The blue ions are removed, so the solution pales or becomes colourless. The reaction is exothermic, so the tube gets hotter.
Test 3: Zinc reacts with dilute sulfuric acid: . The copper(II) sulfate acts as a catalyst for this reaction, but the key observation is fizzing/effervescence as hydrogen is evolved. The gas pops with a lighted splint — the classic test for hydrogen.
Key Takeaways
The reactivity series predicts displacement reactions. Hydrogen gas is identified by the "pop" with a lighted splint. Observations must be recorded precisely, at the correct stage, with colours and physical states described accurately.
Common Mistakes
- Writing "brown" instead of "pink-brown" for copper metal.
- Forgetting to record the gas test in Test 3.
- Confusing the precipitate colours (green vs white ).
- Not recording that the solution pales in Test 2.
Things to Be Careful About
- Record the exact colour ("pale green", not just "green").
- Note the stage: "on adding " vs "on adding FB 5".
- The precipitate in Test 1 comes from the solution after pouring off — make clear which stage you are describing.
- "No change" must be written if nothing happens — but here changes do occur.
FB 6 is the filtrate obtained after filtering the mixture that remains at the end of Test 3 in (a)(i).
Add aqueous ammonia to FB 6.
Record your observations.
Answer
White precipitate forms, soluble in excess aqueous ammonia.
White precipitate, soluble in excess ammonia
Background Concept
Aqueous ammonia is a weak base and a source of ions. Many metal cations form insoluble hydroxides when ammonia is added. Zinc(II) is amphoteric: its hydroxide dissolves in excess alkali (both and ), forming a soluble complex ion, , with ammonia.
Understanding the Question
FB 6 is the filtrate from Test 3 — the solution left after zinc reacted with dilute sulfuric acid and copper(II) sulfate. It contains . You add aqueous ammonia and record what happens: first a white precipitate of , then dissolution in excess ammonia.
Approach
Add ammonia dropwise. First observation: white precipitate. Continue adding excess ammonia: precipitate dissolves. Record both stages.
Step-by-Step Reasoning
. The white gelatinous precipitate is zinc hydroxide. On adding excess ammonia, — the precipitate dissolves to give a colourless solution.
Key Takeaways
gives a white precipitate with , soluble in excess — a key distinguishing test for (compare , which gives a white precipitate soluble in excess but NOT in excess ).
Common Mistakes
- Forgetting to record the solubility in excess.
- Writing "no change" — the precipitate does form.
- Confusing with behaviour.
Things to Be Careful About
- Record both stages: precipitate forms, then dissolves in excess.
- The precipitate is white and gelatinous.
Answer
FB 5 is zinc ().
Zinc (Zn)
Background Concept
The observations from (a)(i) — displacement of iron and copper, and reaction with acid to give hydrogen — are characteristic of a metal above iron and copper in the reactivity series. Zinc fits perfectly.
Understanding the Question
Identify FB 5 from the accumulated observations in the three tests.
Approach
Match the observed behaviour to a known metal. Zinc displaces Fe and Cu and reacts with dilute acid to give .
Step-by-Step Reasoning
The pink-brown copper deposit in Test 2 and hydrogen gas in Test 3 identify FB 5 as a metal more reactive than copper and able to reduce to . Zinc is the metal that fits all observations.
Key Takeaways
Qualitative tests build a profile; the profile identifies the substance.
Common Mistakes
- Guessing without linking observations.
- Confusing with other reactive metals (e.g. Mg would also give , but the displacement colours differ).
Things to Be Careful About
- The answer must be the element or correct formula: zinc / .
Answer
Copper is formed and copper ions gain electrons: changes oxidation state from +2 to 0 (reduction). Zinc is oxidised, changing oxidation state from 0 to +2, forming zinc ions.
Cu2+ reduced (+2 to 0); Zn oxidised (0 to +2)
Background Concept
A redox reaction involves simultaneous oxidation and reduction. Oxidation is loss of electrons (or increase in oxidation state); reduction is gain of electrons (or decrease in oxidation state). In a displacement reaction, the more reactive metal is oxidised and the less reactive metal's ions are reduced.
Understanding the Question
Explain why Test 2 ( + ) is a redox reaction, using your observations.
Approach
Identify the species that change oxidation state and state what happens to each.
Step-by-Step Reasoning
In Test 2: . Zinc loses electrons (oxidised, oxidation state 0 +2). Copper ions gain electrons (reduced, oxidation state +2 0). Both processes occur, so it is a redox reaction. The pink-brown copper solid is the visible evidence of reduction.
Key Takeaways
A displacement reaction is always redox: the more reactive metal is oxidised, the less reactive metal's ion is reduced.
Common Mistakes
- Saying only "copper is formed" without mentioning electron transfer or oxidation-state change.
- Confusing which species is oxidised and which is reduced.
Things to Be Careful About
- State both the species and the electron transfer (or oxidation-state change) for full marks.
Give the ionic equation for the first reaction observed in (a)(ii). Include state symbols.
Answer
Zn2+(aq) + 2OH-(aq) -> Zn(OH)2(s)
Background Concept
The first reaction in (a)(ii) is the formation of zinc hydroxide: . This is the ionic equation for the precipitation.
Understanding the Question
Write the ionic equation, with state symbols, for the first reaction observed when ammonia is added to FB 6 ( solution).
Approach
Identify the ions involved: and (from ammonia). Product: . Balance charges and atoms.
Step-by-Step Reasoning
. The 2+ charge on is balanced by two ions. The product is a solid precipitate. State symbols: (aq) for ions in solution, (s) for the precipitate.
Key Takeaways
Ionic equations show only the species that change. Charge and atom balance are essential.
Common Mistakes
- Omitting state symbols.
- Writing the full equation with instead of the ionic form.
- Unbalanced charges.
Things to Be Careful About
- State symbols are required by the question.
- The equation must be balanced in both atoms and charge.
FB 7 contains one anion and one cation. The anion contains oxygen but not nitrogen.
Both ions are listed in the Qualitative analysis notes.
Transfer a small spatula measure of FB 7 into a hard-glass test-tube.
Heat gently at the start, then strongly until no further change occurs.
Leave the test-tube to cool.
Record all your observations. Identify any gases produced.
Answer
- FB 7 is a white powder / solid
- Condensation / water droplets form on the tube
- Solid turns yellow (or yellow-green) when hot
- Residue goes paler on cooling / residue is white
- Gas tested with limewater gives a white precipitate
- Gas is carbon dioxide ()
See working — observations of heating ZnCO3; gas is CO2
Background Concept
Many metal carbonates decompose on heating to give the metal oxide and carbon dioxide: . Zinc carbonate is white; zinc oxide is white when cold but yellow when hot — a characteristic colour change. Carbon dioxide is identified by turning limewater milky (white precipitate of ).
Understanding the Question
Heat FB 7 () gently then strongly in a hard-glass test-tube, and record all observations including any gas identification. The anion contains oxygen but not nitrogen, and both ions are in the Qualitative analysis notes — this hints at a carbonate.
Approach
Predict the thermal decomposition of a carbonate. Watch for colour change of the residue, condensation, and test any gas with limewater.
Step-by-Step Reasoning
. FB 7 is a white powder. On heating, condensation (water droplets) forms on the cooler parts of the tube (from moisture). The solid turns yellow when hot — characteristic of . On cooling, it returns to white. The gas evolved is : it turns limewater milky (white precipitate of ).
Key Takeaways
Carbonates decompose to oxide + . is yellow when hot, white when cold. is confirmed with limewater.
Common Mistakes
- Not testing the gas with limewater.
- Writing "turns brown" instead of "turns yellow".
- Not recording the colour change on cooling.
Things to Be Careful About
- Record the colour at each temperature stage (hot vs cold).
- Condensation is a valid observation.
- The gas test must be described for the identification mark.
Carry out one further positive test to confirm the identity of the anion in FB 7.
Record only the results shown in a positive test.
Describe the test you carry out and the observations you make in the space below.
The anion in FB 7 is ............................. .
Answer
Add dilute hydrochloric acid (or any mineral acid) to FB 7.
Observation: fizzing / effervescence.
The anion in FB 7 is carbonate, .
Carbonate, CO3^2-
Background Concept
The confirmatory test for carbonate is to add a dilute mineral acid: . Effervescence (fizzing) indicates evolution, confirming carbonate.
Understanding the Question
Carry out one further positive test to confirm the anion in FB 7. The anion is carbonate. You must describe the test and the positive observation.
Approach
Add a dilute mineral acid (e.g. , , or ) to FB 7 and look for effervescence.
Step-by-Step Reasoning
Add dilute hydrochloric acid (or nitric/sulfuric acid) to FB 7. Effervescence/fizzing confirms carbonate. The gas is (optionally test with limewater for extra confirmation).
Key Takeaways
Carbonate + acid + water. Effervescence is the positive test.
Common Mistakes
- Using a non-mineral acid or no acid at all.
- Not naming the acid or giving its formula.
- Confusing with other anion tests.
Things to Be Careful About
- The acid must be a mineral acid (, , ).
- Record the positive observation (effervescence) only.