Chemistry 9701/36 — October/November 2024
Cambridge AS Level · Advanced Practical Skills · worked solutions for every part, with the mark scheme
Topics Presentation of Data and Observations · Analysis, Conclusions and Evaluation · Manipulation, Measurement and Observation · Qualitative Analysis
Sodium carbonate reacts with hydrochloric acid to release carbon dioxide as shown.
You will find the percentage purity in a sample of impure sodium carbonate by reacting it with excess hydrochloric acid and measuring the volume of carbon dioxide formed. You may assume that the impurity does not react with acid to produce a gas.
FB 1 is impure sodium carbonate, .
FB 2 is hydrochloric acid, .
Method
- Weigh the container with FB 1. Record the mass.
- Fill the tub with water to a depth of approximately .
- Fill the measuring cylinder completely with water. Holding a piece of paper towel firmly over the top, invert the measuring cylinder and place it in the water in the tub.
- Remove the paper towel and clamp the inverted measuring cylinder so the open end is in the water just above the base of the tub.
- Use the measuring cylinder to transfer of FB 2 into the flask labelled X. Check the bung fits tightly into the neck of flask X, clamp flask X and place the delivery tube into the inverted measuring cylinder.
- Remove the bung from the neck of the flask. Tip all the FB 1 into the acid in the flask and replace the bung immediately. Remove the flask from the clamp and swirl it to mix the contents.
- Replace the flask in the clamp and leave until the fizzing has stopped.
- Remove the flask from the clamp occasionally, swirl it and replace the flask in the clamp.
- Weigh the empty container that held FB 1. Record the mass.
- Calculate and record the mass of FB 1 added.
- When no more gas is collected, record the final volume of gas produced.
You may wish to start Question 2 while the gas is being produced.
Results
Answer
Results table (representative values):
| Measurement | Value |
|---|---|
| Mass of container + FB 1 / g | 22.45 |
| Mass of empty container / g | 21.75 |
| Mass of FB 1 / g | 0.70 |
| Volume of gas / cm³ | 150 |
- All balance readings recorded to 2 decimal places.
- Mass of FB 1 = 22.45 − 21.75 = 0.70 g
- Volume of gas recorded to the nearest 1 cm³ and within the range 50–250 cm³.
See working: results table with headings and units, balance readings to 2 dp, volume to 1 cm³
Background Concept
This is a gas-collection experiment to determine the percentage purity of an impure sample of sodium carbonate. The key idea is that the volume of carbon dioxide produced is directly proportional to the amount of pure sodium carbonate present, because the impurity does not produce gas. Recording data correctly is essential in practical work: every measurement must be associated with a clear heading and unit, and readings must be taken to an appropriate precision.
Understanding the Question
Part (a) is about recording the results of the experiment. The marks are awarded for the structure and quality of the results table, not for the actual values (which depend on the candidate's own readings). You need to record: the mass of the container with FB 1, the mass of the empty container, the calculated mass of FB 1, and the final volume of gas produced.
Approach
Set up a table with clear headings, each with its unit. Record balance readings to 2 or 3 decimal places. Calculate the mass of FB 1 by subtraction. Record the gas volume to the nearest 1 cm³. Check the volume is between 50 and 250 cm³.
Step-by-Step Reasoning
- Headings: "Mass of container + FB 1 / g", "Mass of empty container / g", "Mass of FB 1 / g", "Volume of gas / cm³" (or "Volume of CO2 / cm³"). Each heading must have its unit.
- Balance readings: record to 2 dp or 3 dp (e.g., 22.45 g, not 22.4 g). The mass of FB 1 is the difference: 22.45 − 21.75 = 0.70 g.
- Volume: read the measuring cylinder to the nearest 1 cm³ (e.g., 150 cm³, not 150.2 cm³).
- Range check: the volume must be between 50 and 250 cm³. If it is outside this range, the experiment may need repeating with a different mass of FB 1.
Key Takeaways
- Results tables need clear headings with units.
- Balance readings to 2 or 3 dp.
- Gas volumes to nearest 1 cm³.
- The mass of FB 1 is found by difference.
Common Mistakes
- Missing units in headings.
- Recording balance readings to 1 dp.
- Recording gas volume to more precision than the measuring cylinder allows.
- Writing "Mass of FB 1" without showing the subtraction.
Things to Be Careful About
- The volume of gas must be within 50–250 cm³; if not, the experiment is invalid.
- Keep the same decimal places for both balance readings.
- The mass of FB 1 is a calculated value, so it may have fewer decimal places than the raw readings (e.g., 0.70 g from 22.45 − 21.75).
Calculations
Give your answers to each part of (b)(ii), (b)(iii) and (b)(iv) to an appropriate number of significant figures.
Answer
Give the answers to parts (b)(ii), (b)(iii) and (b)(iv) to 2–4 significant figures.
Answers to 2–4 significant figures
Background Concept
Significant figures indicate the precision of a measurement or calculation. In calculations, the result should not be quoted to more significant figures than the least precise input value justifies. The practical guidance here is to give answers to 2–4 significant figures.
Understanding the Question
This is a one-mark instruction: give your answers to parts (ii), (iii) and (iv) to an appropriate number of significant figures. The mark is awarded for actually doing so — the examiner checks that the answers you present are to 2–4 sf.
Approach
When you calculate each value, round the final answer to 2–4 significant figures. Do not carry excessive decimal places.
Step-by-Step Reasoning
The mark is awarded holistically: if all three answers ((ii), (iii), (iv)) are given to 2–4 sf, the mark is scored. For example, 0.00625 mol (3 sf), 0.6625 g (4 sf), 94.6% (3 sf) all fall within the 2–4 sf range.
Key Takeaways
- Always round final answers to a sensible number of significant figures in practical calculations.
Common Mistakes
- Quoting too many significant figures (e.g., 0.006250000 mol).
- Quoting too few (e.g., 0.006 mol is 1 sf — not acceptable).
Things to Be Careful About
- The mark scheme accepts 2–4 sf — anything outside this range loses the mark.
Working
Using the representative gas volume of 150 cm³:
Answer
0.00625 mol
0.00625 mol (representative)
Background Concept
At room temperature and pressure (r.t.p.), one mole of any gas occupies approximately 24 dm³ = 24000 cm³. This is the molar gas volume. The amount of gas collected can be calculated from its volume using:
Understanding the Question
You measured the volume of CO2 collected in the measuring cylinder. Use the molar gas volume to convert that volume into an amount in moles.
Approach
Divide the volume of gas (in cm³) by 24000.
Step-by-Step Reasoning
Using the representative value of 150 cm³:
The answer is given to 3 sf, which satisfies part (b)(i).
Key Takeaways
- Molar gas volume at r.t.p. is 24000 cm³ mol⁻¹.
- amount = volume / molar gas volume.
Common Mistakes
- Using 24000 dm³ instead of 24000 cm³.
- Forgetting to convert cm³ to dm³ first (dividing by 24000 works directly if volume is in cm³).
Things to Be Careful About
- The volume must be in cm³ for the 24000 factor to work.
Use your answer to (b)(ii) to deduce the amount, in mol, of the sodium carbonate present in the FB 1 you used in your experiment.
Use your answer to calculate the mass, in g, of sodium carbonate in your sample of FB 1.
Working
From the balanced equation, 1 mol produces 1 mol , so:
Answer
0.6625 g
0.6625 g (representative)
Background Concept
The balanced equation shows a 1:1 molar ratio between Na2CO3 and CO2:
So the amount of Na2CO3 that reacted equals the amount of CO2 produced. The molar mass of Na2CO3 is 2(23.0) + 12.0 + 3(16.0) = 106 g mol⁻¹.
Understanding the Question
Use the amount of CO2 from (b)(ii) to find the amount of Na2CO3, then convert to a mass using the molar mass.
Approach
- Amount of Na2CO3 = amount of CO2 (1:1 ratio).
- Mass = amount × molar mass (106).
Step-by-Step Reasoning
Amount of Na2CO3 = 0.00625 mol.
Mass = 0.00625 × 106 = 0.6625 g.
Key Takeaways
- Stoichiometric ratio from the balanced equation.
- mass = amount × molar mass.
Common Mistakes
- Using the wrong ratio (e.g., 2:1 because of the 2HCl).
- Using the wrong molar mass (e.g., 84 for NaHCO3).
Things to Be Careful About
- The ratio Na2CO3:CO2 is 1:1, not 1:2.
Working
Using the representative values:
Answer
94.6%
94.6% (representative)
Background Concept
Percentage purity is the fraction of the sample that is actually the desired substance, expressed as a percentage:
Understanding the Question
The mass of pure Na2CO3 was found in (b)(iii). The mass of the impure sample (FB 1) was recorded in (a). Divide and multiply by 100.
Approach
Step-by-Step Reasoning
Using representative values: mass from (iii) = 0.6625 g, mass of FB 1 = 0.70 g.
Key Takeaways
- Percentage purity = (pure mass / sample mass) × 100.
Common Mistakes
- Swapping numerator and denominator.
- Forgetting to multiply by 100.
Things to Be Careful About
- Use the mass of the impure sample (FB 1), not the mass of the container.
Even though the bung was replaced quickly, some carbon dioxide was lost. Suggest a change you could make to minimise gas loss at this stage.
Answer
Place the solid FB 1 in a small tube or container suspended above the acid inside the flask, so that the solid and acid only mix after the bung has been replaced.
Suspend the solid in a small tube above the acid so it mixes only after the bung is replaced
Background Concept
In this experiment, the solid and acid are mixed by tipping FB 1 into the acid, then replacing the bung. During the brief moment when the bung is off, any gas produced escapes. To minimise this loss, the solid and acid should only mix after the bung is sealed.
Understanding the Question
Suggest a change to the apparatus or method so that the solid and acid mix only after the flask is sealed.
Approach
Think of a way to keep the solid separate from the acid until the bung is firmly in place.
Step-by-Step Reasoning
The mark scheme accepts: a small tube or container holding FB 1 suspended above the acid inside the flask, a flask with a shelf, or a divided flask. When the flask is sealed, the solid is tipped or shaken into the acid.
Key Takeaways
- Gas-loss minimisation: mix reagents only after sealing.
Common Mistakes
- Suggesting "be quicker" — not a design change.
- Suggesting something that doesn't keep the solid separate.
Things to Be Careful About
- The change must be practical and specific.
Some carbon dioxide is not collected because it is slightly soluble in water. State a change you could make to reduce the solubility of the gas.
Do not suggest using a liquid other than water in your tub or changing the volume of water used.
Answer
Use hot water in the tub (or saturate the water with CO2 before the experiment).
Use hot water, or saturate the water with CO2
Background Concept
Gases are more soluble in cold water than in hot water. CO2 is slightly soluble in water, so some of the gas dissolves in the water in the tub and is not collected. Heating the water reduces its solubility.
Understanding the Question
State a change to reduce the solubility of CO2 in the water, without changing the liquid or its volume.
Approach
Use hot water, or saturate the water with CO2 beforehand so no more can dissolve.
Step-by-Step Reasoning
Hot water dissolves less gas than cold water, so using hot water in the tub reduces the amount of CO2 lost by dissolution. Alternatively, saturating the water with CO2 before the experiment means it cannot absorb more.
Key Takeaways
- Solubility of gases decreases with increasing temperature.
Common Mistakes
- Suggesting a different liquid (explicitly disallowed).
- Changing the volume of water (disallowed).
Things to Be Careful About
- Read the question carefully: it restricts the options.
State the uncertainty in a single reading of your balance.
Calculate the maximum percentage error in the mass of FB 1 used in (a).
Working
For a 2 dp balance, the uncertainty in a single reading is .
The mass of FB 1 is found by difference, so the total uncertainty is .
Using the representative mass of FB 1 = 0.70 g:
Answer
; maximum percentage error = 2.9%
U = 0.01 g; maximum percentage error = 2.9%
Background Concept
A balance with 2 decimal places has an uncertainty of ±0.01 g (or ±0.005 g depending on convention). When two readings are subtracted (container + FB1 minus empty container), the uncertainties add, giving a total uncertainty of 2 × U.
Understanding the Question
State the uncertainty in a single balance reading, then calculate the maximum percentage error in the mass of FB 1.
Approach
- State U (e.g., 0.01 g for a 2 dp balance).
- Maximum percentage error = (2U / mass of FB 1) × 100.
Step-by-Step Reasoning
For a 2 dp balance, U = 0.01 g. The mass of FB 1 is found by difference, so the total uncertainty is 2 × 0.01 = 0.02 g.
Key Takeaways
- Uncertainty in a difference is the sum of the individual uncertainties.
- Percentage error = (uncertainty / value) × 100.
Common Mistakes
- Using U instead of 2U (forgetting the subtraction).
- Using the wrong U for the balance precision.
Things to Be Careful About
- The mark scheme accepts U = 0.01 g or 0.005 g for a 2 dp balance, and U = 0.001 g or 0.0005 g for a 3 dp balance.
Many metal carbonates, such as magnesium carbonate, decompose to form the metal oxide when heated.
Other metal carbonates, such as sodium carbonate, , do not decompose at the temperature produced by a Bunsen burner.
FB 3 is a mixture that contains only sodium carbonate, , and magnesium carbonate.
You will carry out an experiment involving thermal decomposition to find the percentage of each of these metal carbonates in this mixture.
Method
- Weigh the empty crucible with its lid. Record the mass.
- Transfer all the FB 3 from the container into the crucible.
- Weigh the crucible, lid and FB 3. Record the mass.
- Calculate and record the mass of FB 3 used.
- Place the crucible and contents on the 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.
- Leave the crucible with its contents until it is cool.
While the crucible is cooling, 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.
- Heat the crucible strongly, with the lid off, for approximately 4 minutes.
- Allow the crucible and contents to cool.
- When the crucible is cool, weigh the crucible with its lid and contents. Record the mass.
- Calculate and record the mass of residue.
- Calculate and record the mass of carbon dioxide produced.
Leave the crucible and contents to become completely cool for use in Question 2(c).
Results
Answer
Use a results table with these headings (include units):
- mass of crucible + lid / g
- mass of crucible + lid + FB 3 / g
- mass of FB 3 added / g
- mass of crucible + lid + contents after 1st heating / g
- mass of crucible + lid + contents after 2nd heating / g
- mass of residue / g
- mass of / g
Record all balance readings to the same number of decimal places (2 dp or 3 dp). The two post-heating readings should agree closely to show decomposition is complete.
Example using representative readings:
| Reading | Mass / g |
|---|---|
| crucible + lid | 15.00 |
| crucible + lid + FB 3 | 17.50 |
| FB 3 added | 2.50 |
| after 1st heating | 16.88 |
| after 2nd heating | 16.86 |
| residue | 1.86 |
| produced | 0.64 |
Calculations:
- mass of FB 3 = 17.50 - 15.00 = 2.50 g
- mass of residue = 16.86 - 15.00 = 1.86 g
- mass of = 2.50 - 1.86 = 0.64 g
See working: completed results table with headings and example values (FB 3 2.50 g, residue 1.86 g, CO2 0.64 g); candidate-dependent.
Background Concept
Thermal decomposition of a metal carbonate produces the metal oxide and carbon dioxide. Magnesium carbonate decomposes at Bunsen-burner temperature:
Sodium carbonate is much more stable and does not decompose under these conditions. Therefore, when a mixture of the two is heated, only the MgCO loses mass. The mass lost is exactly the mass of CO released, because CO is the only gaseous product. Heating to constant mass (reweighing after further heating and getting the same mass) ensures decomposition is complete.
Understanding the Question
This part asks you to carry out the heating procedure and record your results in a clear table. You need to record the masses needed to find the mass of FB 3, the mass of residue, and the mass of CO produced. The mark scheme rewards correct headings with units, consistent decimal places, and correct calculations.
Approach
Weigh the empty crucible with its lid, then weigh it again after adding FB 3. Heat, cool, and reweigh. Repeat heating until the mass is constant. Use mass differences to calculate the required quantities.
Step-by-Step Reasoning
- Record the mass of the crucible and lid.
- Record the mass of the crucible, lid and FB 3.
- Mass of FB 3 = (mass of crucible + lid + FB 3) - (mass of crucible + lid).
- After heating and cooling, record the mass of the crucible, lid and contents.
- Heat again and reweigh. If the two post-heating masses agree closely, decomposition is complete.
- Mass of residue = (mass of crucible + lid + contents after final heating) - (mass of crucible + lid).
- Mass of CO = mass of FB 3 - mass of residue (or mass loss on heating).
In the example, FB 3 = 2.50 g, residue = 1.86 g, and CO = 0.64 g.
Key Takeaways
- Mass loss on heating a carbonate equals mass of CO released.
- Heating to constant mass confirms complete decomposition.
- A results table must have clear headings with units and consistent decimal places.
Common Mistakes
- Forgetting units in headings.
- Using different numbers of decimal places for different readings.
- Calculating mass of CO incorrectly (it is mass lost, not mass of residue).
- Weighing before the crucible is cool, giving inaccurate readings.
Things to Be Careful About
- Always cool the crucible before weighing.
- Use the same balance and same precision throughout.
- The two post-heating masses should differ by no more than about 0.02 g (allowing a small range) to show constant mass.
Working
From (a): mass of = 0.64 g
g mol
Answer
1.45 x 10^-2 mol (using example mass CO2 = 0.64 g; use your own value)
1.45 x 10^-2 mol (example)
Background Concept
The amount of a substance in moles is found using:
where is mass in g and is molar mass in g mol. For CO, g mol.
Understanding the Question
You are asked to calculate the amount, in mol, of CO produced in the decomposition. The mass of CO comes from your results in part (a).
Approach
Divide the mass of CO by its molar mass.
Step-by-Step Reasoning
Using the example mass of CO = 0.64 g:
Give the answer to 2-4 significant figures.
Key Takeaways
- is the central conversion between mass and moles.
- Molar mass of CO is 44.0 g mol.
Common Mistakes
- Using 44 instead of 44.0 (minor but avoid).
- Forgetting to divide mass by molar mass.
- Giving too few or too many significant figures.
Things to Be Careful About
- Use the mass of CO from your own results, not the example.
- Include the unit mol.
Working
From the equation, 1 mol produces 1 mol , so:
g mol
Answer
1.22 g (example)
1.22 g (example)
Background Concept
From the decomposition equation, 1 mol MgCO produces 1 mol CO. So amount of MgCO = amount of CO. Mass = amount × molar mass. g mol.
Understanding the Question
Use the moles of CO from (b)(i) to calculate the mass of MgCO in FB 3.
Approach
Apply the 1:1 stoichiometric ratio, then multiply by molar mass.
Step-by-Step Reasoning
mol.
Key Takeaways
- Stoichiometry from the balanced equation is 1:1 here.
- mass = n × M.
Common Mistakes
- Using wrong molar mass for MgCO.
- Forgetting to convert moles to mass.
Things to Be Careful About
- Use the same significant figures as in (b)(i).
- Include unit g.
Calculate the percentages by mass of magnesium carbonate and sodium carbonate in FB 3.
Working
Answer
MgCO3 48.8%; Na2CO3 51.2% (example)
MgCO3 48.8%; Na2CO3 51.2% (example)
Background Concept
Percentage by mass = (mass of component / total mass of mixture) × 100. Since the mixture contains only MgCO and NaCO, the percentage of NaCO is 100 - percentage of MgCO.
Understanding the Question
Calculate percentages by mass of both carbonates in FB 3 using mass of MgCO from (b)(ii) and total mass of FB 3 from (a).
Approach
Divide mass of MgCO by mass of FB 3, multiply by 100, then subtract from 100 for NaCO.
Step-by-Step Reasoning
Using example values:
Key Takeaways
- Percentages of all components in a two-component mixture sum to 100%.
- Use the total mass of FB 3, not the residue mass.
Common Mistakes
- Using residue mass instead of original FB 3 mass.
- Forgetting to subtract from 100 for NaCO.
- Not including the % sign.
Things to Be Careful About
- Use your own data.
- Give answer to 2-4 significant figures.
Add a few drops of water to the cool residue in the crucible.
Use universal indicator to test the pH of the solution formed.
Tick () one box to show the direction of the temperature change.
| temperature goes up | temperature goes down |
|---|---|
| [ ] | [ ] |
Answer
- (alkaline; pH )
Tick: temperature goes up
pH >= 9; temperature goes up
Background Concept
Magnesium oxide is a basic oxide. When added to water, it reacts to form magnesium hydroxide, which dissolves slightly and gives an alkaline solution:
The reaction is exothermic, so the temperature rises.
Understanding the Question
After adding water to the cooled residue, you test the pH with universal indicator and note whether the temperature goes up or down. The residue contains MgO (and NaCO if it did not decompose).
Approach
Observe the colour of universal indicator to estimate pH, and feel/touch the crucible or use a thermometer to detect temperature change.
Step-by-Step Reasoning
MgO reacts with water to form Mg(OH), an alkali. Universal indicator gives a blue/purple colour, pH . Because the reaction is exothermic, the temperature goes up.
Key Takeaways
- Basic oxides form alkaline solutions with water.
- Dissolution/hydration of MgO is exothermic.
Common Mistakes
- Saying pH is acidic or neutral.
- Ticking temperature goes down.
Things to Be Careful About
- Universal indicator measures pH, not a precise value.
- The temperature change is small but noticeable.
Use these observations and the information about the thermal decomposition of magnesium carbonate to write an equation for the reaction in (c)(i). Include state symbols and the sign of .
Answer
is negative (-ve).
MgO(s) + H2O(l) -> Mg(OH)2(s), Delta H negative
Background Concept
Metal oxides react with water to form metal hydroxides. The enthalpy change of reaction is negative if the reaction releases heat (exothermic). The sign of follows the observed temperature change: temperature increase means is negative.
Understanding the Question
Write the equation for the reaction in (c)(i), i.e. MgO with water, including state symbols and the sign of .
Approach
Identify reactants and products, balance, add state symbols, then use the temperature change to assign the sign.
Step-by-Step Reasoning
MgO(s) + HO(l) → Mg(OH)(s) (or aq). The equation is already balanced with one Mg, two O and two H on each side. State symbols: MgO is solid, HO is liquid, Mg(OH) is solid (or aqueous). Since the temperature went up, the reaction is exothermic, so is negative.
Key Takeaways
- Balanced equation for oxide + water → hydroxide.
- Exothermic reaction has negative .
Common Mistakes
- Missing state symbols.
- Writing MgOH instead of Mg(OH).
- Giving positive.
Things to Be Careful About
- Mark scheme allows Mg(OH)(s) or Mg(OH)(aq).
- The sign must match the observed temperature rise.
Suggest how you would show that sodium carbonate had not decomposed during the reaction in (a). State the reagent(s) and observations.
Do not carry out your test.
Answer
Add dilute hydrochloric acid (or dilute nitric acid) to a sample of the residue.
Observation: effervescence/fizzing (bubbles) is seen.
The gas evolved turns limewater milky, showing CO is produced, so carbonate is still present and NaCO has not decomposed.
Add dilute HCl to residue; effervescence; gas turns limewater milky (CO2).
Background Concept
Carbonates react with acids to produce carbon dioxide gas, which can be identified by turning limewater milky. If sodium carbonate had not decomposed, carbonate ions would still be present in the residue. Adding acid to the residue would produce CO.
Understanding the Question
Suggest a test to show that NaCO had not decomposed during heating. You must state the reagent(s) and observations, but not carry out the test.
Approach
Use the standard carbonate test: add a dilute acid and test any gas evolved with limewater.
Step-by-Step Reasoning
- Add dilute hydrochloric acid (or dilute nitric acid) to a small sample of the residue.
- If carbonate is present, effervescence/fizzing occurs as CO is released.
- Bubble the gas through limewater; it turns milky/cloudy, confirming CO.
This shows carbonate is still present, so NaCO has not decomposed.
Key Takeaways
- Carbonate + acid → salt + water + CO.
- CO turns limewater milky.
Common Mistakes
- Testing for sodium ions instead of carbonate.
- Forgetting to name the acid.
- Saying 'bubbles' without identifying CO with limewater.
Things to Be Careful About
- The residue also contains MgO, which reacts with acid but produces no gas.
- Use a named dilute acid and state the observation clearly.
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 4 is a mixture of two salts that each contain one cation and one anion.
All the ions present are in the Qualitative analysis notes.
Place a small spatula measure of FB 4 into a hard-glass test-tube. Heat the tube gently at first and then more strongly.
Record all your observations and identify any gas given off.
Answer
On gentle heating:
- Condensation/steam forms on the cooler part of the tube (water of crystallisation driven off)
- A gas is given off that turns damp red litmus paper blue — ammonia,
- A white solid sublimes onto the cooler part of the tube
- The solid dissolves/melts in its own water of crystallisation and the liquid bubbles
On stronger heating:
- White smoke is produced
- The gas now turns damp blue litmus paper red — hydrogen chloride,
- A white/grey residue remains on cooling
Gases identified: ammonia () and hydrogen chloride ()
Ammonia (NH₃) and hydrogen chloride (HCl) identified from litmus tests; observations recorded in order (condensation, sublimation, white smoke, litmus colour changes, white/grey residue)
Background Concept
When a solid mixture is heated in a test-tube, several types of change can occur: loss of water of crystallisation (dehydration of a hydrated salt), thermal decomposition, and sublimation. Hydrated salts such as lose their water of crystallisation on heating, producing steam which condenses on the cooler parts of the tube. Ammonium chloride () is unusual: it sublimes, and at the same time undergoes reversible thermal decomposition into ammonia () and hydrogen chloride ():
Ammonia is a basic gas — it turns damp red litmus paper blue. Hydrogen chloride is an acidic gas — it turns damp blue litmus paper red. Because ammonia is the lighter gas and is released first as the salt begins to decompose, the litmus test often shows blue first, then red as more accumulates.
Understanding the Question
FB 4 is a mixture of zinc sulfate heptahydrate () and ammonium chloride (). The question asks you to heat a spatula measure in a hard-glass test-tube, gently at first and then more strongly, recording all observations and identifying any gas given off. The instruction to heat gently first then strongly is deliberate: gentle heating drives off water of crystallisation and begins the decomposition of , while stronger heating completes decomposition and may cause further changes. The marking scheme explicitly rewards observations "in the expected order" — gentle heating towards stronger heating.
Approach
Work through the heating in stages. First, gentle heating: expect water loss (steam/condensation) and the start of decomposition ( released, litmus blue). Then stronger heating: more complete decomposition, released (litmus red), white smoke from and recombining in the air, and a residue of anhydrous . Test any gas with damp litmus paper and record observations in the order they occur.
Step-by-Step Reasoning
- Gentle heating: loses its seven waters of crystallisation. Steam is produced and condenses as droplets on the cooler upper part of the tube — this is the "condensation / steam produced" observation.
- As heating continues, begins to decompose: . Ammonia is released and turns damp red litmus blue — the first gas identification.
- The and recombine on cooler surfaces, depositing white solid — this appears as sublimation (solid on the colder tube) and as white smoke where the gases meet the air.
- The solid may appear to melt/dissolve in its own water of crystallisation, and the liquid bubbles as gases escape.
- Stronger heating: more is released; the atmosphere in the tube becomes acidic and damp blue litmus turns red.
- On cooling, the residue (anhydrous ) is white/grey.
Gas identification: ammonia () — turns damp red litmus blue; hydrogen chloride () — turns damp blue litmus red.
Key Takeaways
- Heating a solid mixture can produce multiple gases; test each with damp litmus.
- sublimes and decomposes reversibly to .
- Damp red litmus → blue = basic gas (); damp blue litmus → red = acidic gas ().
- Hydrated salts lose water on heating → steam condenses on cooler surfaces.
- Record observations in the order they occur, distinguishing gentle vs strong heating.
Common Mistakes
- Not recording observations in the order seen (the mark scheme requires this).
- Missing the condensation/steam observation.
- Confusing which gas turns litmus which colour ( = blue, = red).
- Not identifying the gases by name or formula.
- Using a soft-glass test-tube instead of hard-glass for heating a solid.
Things to Be Careful About
- Use a hard-glass test-tube when heating a solid.
- Use damp litmus paper, not dry.
- Write "no change" if nothing happens at a stage.
- The white smoke is recombining — record it as a separate observation.
To a depth of distilled water in a boiling tube, add a spatula measure of FB 4. Shake the tube to dissolve the FB 4.
Carry out the following tests using a depth of this FB 4 solution in a test-tube for each test. Record your observations in Table 3.1.
Table 3.1
| test | observations |
|---|---|
| Test 1 Add aqueous sodium hydroxide, then transfer the mixture into a boiling tube, add a piece of aluminium foil and heat gently. | |
| Test 2 Add an equal volume of dilute nitric acid, then add a few drops of aqueous silver nitrate. | |
| Test 3 Add aqueous barium chloride or barium nitrate, then add dilute nitric acid. | |
| Test 4 Add aqueous sodium carbonate dropwise with shaking until in excess. |
Answer
Test 1 (NaOH, then Al foil + heat):
- White precipitate forms
- Precipitate dissolves in excess NaOH
- On adding Al and warming: effervescence/fizzing
- Gas evolved turns damp red litmus paper blue — ammonia ( present)
- Aluminium turns black/dark grey
Test 2 (dilute nitric acid, then silver nitrate):
- No change on adding nitric acid
- White precipitate on adding silver nitrate
Test 3 (barium chloride/nitrate, then dilute nitric acid):
- White precipitate on adding barium chloride
- No change on adding dilute nitric acid
Test 4 (sodium carbonate dropwise):
- White precipitate forms
Observations recorded for all four tests (see working)
Background Concept
Qualitative analysis uses characteristic reactions to identify ions in solution:
- : forms a white gelatinous precipitate of with NaOH; the hydroxide is amphoteric, so it dissolves in excess NaOH (forming zincate, ). With it forms white .
- : with warm NaOH releases ammonia gas, , which turns damp red litmus blue. Adding aluminium foil and warming helps drive off the ammonia (and would also reduce any nitrate to ammonia, but here it simply assists release).
- : with in dilute nitric acid gives a white precipitate of , insoluble in the acid.
- : with or gives a white precipitate of , insoluble in dilute nitric acid.
Understanding the Question
Four tests are carried out on separate 1 cm depths of FB 4 solution:
- NaOH, then transfer to boiling tube, add Al foil, heat gently.
- Dilute nitric acid, then a few drops of aqueous silver nitrate.
- Aqueous barium chloride or barium nitrate, then dilute nitric acid.
- Aqueous sodium carbonate dropwise until in excess.
Record all observations in Table 3.1. The marking scheme awards 2 observations per mark (round down).
Approach
For each test, predict the observation from the known composition (, , , ). Record the colour of any precipitate, its solubility in excess reagent, and any gas evolved with its test result.
Step-by-Step Reasoning
Test 1: NaOH added to FB 4 solution → white ppt of (insoluble in water, but the hydroxide is amphoteric). On adding excess NaOH the ppt dissolves (zincate ion). Then Al + heat: the aluminium reacts with NaOH producing hydrogen (fizzing/bubbling/effervescence) and the releases which turns damp red litmus blue. The aluminium surface turns black/dark grey as it reacts.
Test 2: Dilute nitric acid added first — no change (no carbonate present to produce ). Then → white ppt of (chloride confirmed).
Test 3: / → white ppt of . Adding dilute nitric acid → no change ( is insoluble in acid).
Test 4: → white ppt of (zinc carbonate is insoluble).
Key Takeaways
- : white ppt with NaOH, soluble in excess; white ppt with .
- : with NaOH + heat (turns damp red litmus blue).
- : white ppt with in dilute nitric acid.
- : white ppt with / , insoluble in dilute nitric acid.
Common Mistakes
- Saying "white precipitate" without noting solubility in excess reagent (this is a separate observation).
- Missing the ammonia test result in Test 1.
- Not recording "no change" for the nitric acid additions.
- Confusing (white) with (cream) or (yellow).
Things to Be Careful About
- Use dilute nitric acid (not sulfuric) before — sulfuric would precipitate and interfere.
- Record at what stage each observation occurs (e.g. "on adding NaOH" vs "on adding excess").
- Write "no change" where appropriate — it is a valid observation.
- Use a boiling tube when warming solutions.
Use your observations in Table 3.1 to identify two anions which must be present in FB 4.
Answer
The two anions present in FB 4 are:
- Chloride, — white precipitate with silver nitrate in dilute nitric acid ()
- Sulfate, — white precipitate with barium chloride/nitrate, insoluble in dilute nitric acid ()
Chloride, Cl⁻ and sulfate, SO₄²⁻
Background Concept
From the observations in Table 3.1:
- Test 2: white ppt with after acidification → ( is white and insoluble in dilute nitric acid).
- Test 3: white ppt with / , insoluble in dilute nitric acid → ( is white and insoluble in acid).
Understanding the Question
Use the observations from part (i) to identify the two anions present in FB 4. Each observation must be matched to the characteristic test. The question gives 2 marks — one per anion.
Approach
Match each observation to the known anion test:
- in acid → halide test; white ppt = chloride.
- / → sulfate test; white ppt insoluble in acid = sulfate.
Step-by-Step Reasoning
- The white precipitate formed with silver nitrate in dilute nitric acid is — chloride, , present.
- The white precipitate formed with barium chloride/nitrate, which does not dissolve on adding dilute nitric acid, is — sulfate, , present.
Key Takeaways
- test distinguishes halides: (white), (cream), (yellow).
- / test confirms sulfate: white insoluble in acid.
Common Mistakes
- Confusing chloride with bromide or iodide (colour of ppt differs).
- Saying "sulfate" without the acid-insolubility evidence.
Things to Be Careful About
- Both anions must be stated with correct formulae (, ).
Carry out further tests to confirm or identify which two cations are present in FB 4.
Record the reagents and conditions needed, your observations and your conclusions in a suitable table.
Answer
| Test | Observation | Conclusion |
|---|---|---|
| Add aqueous ammonia dropwise to FB 4 solution, then in excess | White precipitate forms; precipitate dissolves in excess ammonia giving a colourless solution | present |
| Add aqueous sodium hydroxide and warm (no aluminium foil) | Gas evolved that turns damp red litmus paper blue (ammonia) | present |
Zn²⁺ confirmed by white ppt soluble in excess NH₃; NH₄⁺ confirmed by NH₃ gas with warm NaOH
Background Concept
Cation confirmatory tests:
- : with aqueous ammonia forms a white gelatinous precipitate of ; this dissolves in excess ammonia forming the colourless complex . This distinguishes from (whose hydroxide does NOT dissolve in excess ammonia) and from other cations.
- : with warm aqueous NaOH (no aluminium) releases ammonia gas, , which turns damp red litmus blue.
Understanding the Question
Design further tests to confirm the two cations in FB 4. Record the reagents and conditions, observations, and conclusions in a suitable table. The marking scheme requires a table with at least 2 tests, with Test/Observation headings and a Conclusion column.
Approach
Use aqueous ammonia to confirm (white ppt soluble in excess). Use aqueous NaOH + warm (without aluminium) to confirm (ammonia gas, litmus blue). Present both in a table with clear headings.
Step-by-Step Reasoning
- : add aqueous ammonia dropwise to FB 4 solution → white ppt; add excess ammonia → ppt dissolves giving a colourless solution. This behaviour is characteristic of (amphoteric hydroxide forming a soluble ammine complex).
- : add aqueous NaOH and warm (no aluminium foil — aluminium is only needed if nitrate is suspected) → gas evolved that turns damp red litmus blue = ammonia. This confirms .
Key Takeaways
- : white ppt with , soluble in excess (forms ).
- : ammonia gas with warm NaOH, litmus blue.
- A results table must have clear headings: Test, Observation, Conclusion.
Common Mistakes
- Using aluminium foil in the confirmation (that's the nitrate test).
- Not warming the NaOH for the test (ammonia release is too slow cold).
- Not presenting results in a table with proper headings.
Things to Be Careful About
- Table must have "Test" and "Observation" headings, plus a "Conclusion" column.
- Record reagents and conditions precisely (e.g. "aqueous ammonia, dropwise then excess").
- Zinc hydroxide dissolves in excess — this is the key distinguishing observation.