Chemistry 9701/31 — October/November 2010
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
You are to determine the concentration of hydrochloric acid, which supplies the ions in the following reaction.
In the presence of an excess of ions and an excess of ions, the amount of liberated is directly proportional to the amount of ions present and can be determined by titration with sodium thiosulfate, .
You are provided with the following reactants.
- FA 1 hydrochloric acid
- FA 2 containing sodium thiosulfate,
- aqueous potassium iodate(V),
- aqueous potassium iodide,
Method
- Fill a burette with FA 2.
- Pipette of FA 1 into the conical flask.
- Use a measuring cylinder to add to the flask of aqueous potassium iodate(V) and of aqueous potassium iodide. There is an excess of each of these reagents.
- Place the flask on a white tile.
- Titrate the liberated iodine with FA 2.
- During the titration the colour of the iodine in the solution will fade from red-brown to orange to yellow. The end-point occurs when the solution just goes colourless with the addition of a single drop of FA 2.
- You should perform a rough titration.
In the space below record your burette readings for this rough titration.
The rough titre is .................................
- Carry out as many accurate titrations as you think necessary to obtain consistent results.
- Record in a suitable form below all of your burette readings and the volume of FA 2 added in each accurate titration.
- Make certain any recorded results show the precision of your practical work.
Answer
Rough titre: 25.60 cm^3
Accurate titrations (all readings to the nearest 0.05 cm^3):
| Titration | Initial reading / cm^3 | Final reading / cm^3 | Volume of FA 2 / cm^3 |
|---|---|---|---|
| 1 | 0.00 | 25.05 | 25.05 |
| 2 | 25.05 | 50.00 | 24.95 |
| 3 | 0.00 | 25.00 | 25.00 |
[Example data — your own readings will differ. Two accurate titres must agree within 0.10 cm^3; record initial and final readings for every titration.]
See working — candidate-dependent readings (representative: rough 25.60 cm^3; accurate titres 25.05, 24.95, 25.00 cm^3)
Background Concept
This is an iodometric (redox) titration. The hydrochloric acid is not titrated directly; instead it supplies the H+ ions that drive the reaction between iodate(V) and iodide ions, liberating iodine:
With iodate and iodide in excess, the amount of iodine produced is directly proportional to the amount of H+ (hence HCl) present. The iodine is then titrated against sodium thiosulfate:
The end-point is the disappearance of the iodine colour. A burette is read to the nearest 0.05 cm^3 (half a graduation, since the scale is marked every 0.1 cm^3). A rough titration locates the approximate end-point quickly; accurate titrations are then performed carefully until two results agree within 0.10 cm^3 — these are concordant.
Understanding the Question
Part (a) asks you to record your practical readings: the rough titre, and a table of accurate titrations showing the initial reading, final reading and volume of FA 2 added. The marks reward correct technique (concordant titres, readings to 0.05 cm^3) and clear recording (proper headings and units). There is no single correct value — the examiner compares your titre with the Supervisor's value.
Approach
- Fill the burette with FA 2, ensuring the jet is full and there are no air bubbles.
- Pipette 25.0 cm^3 of FA 1 into the conical flask; add 10 cm^3 of aqueous KIO3 and 10 cm^3 of aqueous KI (both in excess).
- Place the flask on a white tile so the colour change is easy to judge.
- Run the rough titration, adding FA 2 fairly quickly while swirling, until the solution just goes colourless. Record the rough titre.
- For accurate titrations, add FA 2 dropwise near the end-point, swirling after each addition. Record the initial and final readings for every titration.
- Repeat until two accurate titres agree within 0.10 cm^3.
Step-by-Step Reasoning
The white tile gives a white background against which the red-brown → orange → yellow → colourless transition is clearly visible. The end-point is sharp: a single drop of thiosulfate removes the last of the iodine colour, and the solution becomes permanently colourless. For each accurate titration, record the initial burette reading (e.g. 0.00 cm^3) and the final reading (e.g. 25.05 cm^3); the volume added is the difference. Readings must be to the nearest 0.05 cm^3. Two accurate titres within 0.10 cm^3 are concordant and give confidence in the result. A representative set of results is shown in the solution; your own readings will differ but should follow the same pattern.
Key Takeaways
- Burette readings are recorded to the nearest 0.05 cm^3.
- A rough titration is followed by accurate titrations.
- Two accurate titres within 0.10 cm^3 are concordant.
- A clear table with headings and units is essential for full marks.
Common Mistakes
- Using 50.00 cm^3 as the initial burette reading — the mark scheme explicitly rejects this.
- Having more than one final reading of 50.00 cm^3.
- Recording any burette reading greater than 50.00 cm^3.
- Not recording initial and final readings separately for each accurate titration.
- Giving readings to only 0.1 cm^3 (or to 0.01 cm^3, which implies false precision).
Things to Be Careful About
- Headings in the table must match the readings recorded (e.g. "Initial reading / cm^3").
- All accurate readings to the nearest 0.05 cm^3.
- Ensure the burette jet is full before taking the initial reading.
- Swirl the flask after each addition; the end-point is the first drop that makes the solution permanently colourless.
From your titration results obtain a suitable value to be used in your calculation. Show clearly how you have obtained this value.
of FA 1 require .............. of FA 2.
Working
Mean titre = (25.05 + 24.95 + 25.00)/3 = 25.00 cm^3
Answer
25.0 cm^3 of FA 1 require 25.00 cm^3 of FA 2.
25.00 cm^3
Background Concept
When several accurate titrations have been performed, the mean of the concordant titres is used in the calculation. Only titres within 0.20 cm^3 of each other should be averaged; an outlier is discarded. The mean is quoted to two decimal places.
Understanding the Question
Part (b) asks you to select a suitable value (the mean titre) from your accurate results and show clearly how you obtained it. The value is then used in the calculation in part (c).
Approach
Identify the accurate titres that agree within 0.20 cm^3, add them together, and divide by the number of titres used. Show the expression so the examiner can see exactly which titres were used.
Step-by-Step Reasoning
With titres of 25.05, 24.95 and 25.00 cm^3, all three lie within 0.10 cm^3 of each other, so all are used:
The mean is quoted to two decimal places. If the titres had been, for example, 24.3 and 24.4, the mean would be 24.35 cm^3 (not 24.4, which would be incorrect rounding).
Key Takeaways
- Only concordant titres (within 0.20 cm^3) are averaged.
- The mean is quoted to two decimal places.
- The working must be shown clearly (the titres used must be identifiable).
Common Mistakes
- Averaging titres that are not concordant (more than 0.20 cm^3 apart).
- Rounding the mean incorrectly, e.g. writing 24.4 for the mean of 24.3 and 24.4 instead of 24.35.
- Not showing which titres were used in the mean.
Things to Be Careful About
- The mean must be correct to two decimal places.
- If all burette readings are given to one decimal place, the mean may be quoted to one decimal place if numerically correct.
- Tick the titres used or write the expression so the examiner can follow your selection.
Calculations
Show your working and appropriate significant figures in the final answer to each step of your calculations.
Calculate the concentration, in , of the sodium thiosulfate in FA 2.
FA 2 contains .
[: H, 1.0; O, 16.0; Na, 23.0; S, 32.1]
The concentration of sodium thiosulfate in FA 2 is ............................ .
Working
Answer
0.0604 mol dm^-3
0.0604 mol dm^-3
Background Concept
The sodium thiosulfate is provided as the hydrated salt Na2S2O3·5H2O, so its molar mass includes the five water molecules of crystallisation. The molar concentration is found by dividing the mass concentration (in g dm^-3) by the molar mass (in g mol^-1):
Understanding the Question
FA 2 contains 15.0 g dm^-3 of Na2S2O3·5H2O. You must calculate the concentration in mol dm^-3. The Ar values are given: H, 1.0; O, 16.0; Na, 23.0; S, 32.1.
Approach
- Calculate Mr of Na2S2O3·5H2O, remembering to include the 5H2O.
- Divide 15.0 by Mr to get the molar concentration.
- Give the answer to 3 significant figures.
Step-by-Step Reasoning
Mr = 2(23.0) + 2(32.1) + 3(16.0) + 5(18.0) = 46.0 + 64.2 + 48.0 + 90.0 = 248.2.
Note that 5H2O contributes 5 × 18.0 = 90.0 to the molar mass. Then:
The answer is given to 3 significant figures (0.0604), consistent with the 15.0 g dm^-3 given.
Key Takeaways
- The molar mass of a hydrated salt includes its water of crystallisation.
- Molar concentration = mass concentration ÷ Mr.
- Final answers should carry 3–5 significant figures.
Common Mistakes
- Forgetting the water of crystallisation and using Mr = 158.1 instead of 248.2 — this gives a wrong answer (0.0949 instead of 0.0604).
- Giving the answer to too few significant figures (e.g. 0.06).
Things to Be Careful About
- Include 5H2O in the Mr calculation.
- The mark scheme accepts 0.060, 0.0604 or 0.06044 — all are fine, but 3 significant figures is the cleanest.
- No additional factor or expression is allowed in this step — use exactly 15.0/248.2.
Calculate how many moles of are contained in the volume of FA 2 recorded in (b).
.............. mol of
Working
Moles of mol
Answer
0.00151 mol
0.00151 mol
Background Concept
The number of moles of a solute is the product of its molar concentration and the volume of solution used, with the volume expressed in dm^3:
Since 1 dm^3 = 1000 cm^3, a volume in cm^3 is converted to dm^3 by dividing by 1000.
Understanding the Question
From part (b), 25.00 cm^3 of FA 2 was used (the mean titre). Using the concentration from part (c)(i), calculate the moles of Na2S2O3 in that volume.
Approach
Multiply the concentration (0.0604 mol dm^-3) by the volume in dm^3 (25.00/1000 = 0.02500 dm^3).
Step-by-Step Reasoning
The answer is given to 3 significant figures (0.00151).
Key Takeaways
- moles = concentration × volume (volume in dm^3).
- Convert cm^3 to dm^3 by dividing by 1000.
- Keep the same number of significant figures as the input data.
Common Mistakes
- Forgetting to divide the volume by 1000 (giving 1.51 mol instead of 0.00151 mol).
- Using the rough titre instead of the mean titre.
Things to Be Careful About
- Use the mean titre from part (b), not the rough titre.
- The mark scheme requires this step to use answer (i) × (candidate's average titre)/1000.
Calculate how many moles of iodine, reacted with the in (ii).
............................ mol of iodine reacted with the sodium thiosulfate.
Working
From , moles of mol
Answer
0.000755 mol
0.000755 mol
Background Concept
The titration reaction between sodium thiosulfate and iodine is:
The stoichiometric ratio is 2 mol thiosulfate : 1 mol iodine. Therefore, the moles of iodine that reacted equal half the moles of thiosulfate used.
Understanding the Question
Using the moles of Na2S2O3 from part (c)(ii), calculate the moles of I2 that reacted with it.
Approach
Read the ratio from the balanced equation (2:1) and divide the moles of thiosulfate by 2.
Step-by-Step Reasoning
The answer is 0.000755 mol (3 significant figures).
Key Takeaways
- The stoichiometric ratio comes directly from the coefficients in the balanced equation.
- 2 mol S2O3^2- ≡ 1 mol I2, so moles I2 = ½ moles S2O3^2-.
Common Mistakes
- Using a 1:1 ratio and writing 0.00151 mol.
- Multiplying by 2 instead of dividing (confusing the direction of the ratio).
Things to Be Careful About
- The mark scheme requires you to show the ×½ (or ÷2) step explicitly.
- Keep 3 significant figures in the final answer.
Calculate how many moles of hydrochloric acid, , reacted with an excess of potassium iodate(V) and an excess of potassium iodide to produce the amount of iodine calculated in (iii).
............................ mol of produced the amount of iodine calculated in (iii).
Working
From (i.e. ), moles of mol
Answer
0.00151 mol
0.00151 mol
Background Concept
The reaction that liberates iodine is:
The stoichiometric ratio is 6 mol H+ : 3 mol I2, which simplifies to 2 mol H+ : 1 mol I2. Since each mole of HCl provides one mole of H+, the moles of HCl equal the moles of H+.
Understanding the Question
Using the moles of I2 from part (c)(iii), calculate the moles of HCl that produced that iodine. The iodate and iodide are in excess, so all the H+ comes from the HCl.
Approach
Read the ratio from the balanced equation (6H+ : 3I2 = 2:1) and multiply the moles of iodine by 2.
Step-by-Step Reasoning
The answer is 0.00151 mol (3 significant figures). Notice that this equals the moles of thiosulfate — a useful cross-check: the overall stoichiometry from HCl to thiosulfate is 1:1 because 6H+ produce 3I2 and each I2 consumes 2S2O3^2-, so 6H+ ≡ 6S2O3^2-.
Key Takeaways
- The H+ : I2 ratio is 2:1 (from 6:3 in the equation).
- Each mole of HCl supplies one mole of H+.
- Moles of HCl = 2 × moles of I2.
Common Mistakes
- Using a 6:3 ratio but applying it wrongly (e.g. dividing by 2 instead of multiplying).
- Forgetting that the ratio simplifies to 2:1.
- Confusing the direction: more H+ than I2, so moles HCl > moles I2.
Things to Be Careful About
- The mark scheme requires you to show multiplication or division by 6, 1.2 or 2 in this step.
- The overall chain HCl → H+ → I2 → S2O3^2- is 1:1, so the final moles of HCl should equal the moles of thiosulfate — a good check.
Calculate the concentration, in , of in FA 1.
The concentration of in FA 1 is ....................... .
Working
Answer
0.0604 mol dm^-3
0.0604 mol dm^-3
Background Concept
The concentration of a solution is the number of moles of solute per cubic decimetre of solution:
The 25.0 cm^3 of FA 1 pipetted into the flask contained the 0.00151 mol of HCl calculated in part (c)(iv).
Understanding the Question
Using the moles of HCl from part (c)(iv) and the 25.0 cm^3 volume of FA 1, calculate the concentration of HCl in FA 1.
Approach
- Convert 25.0 cm^3 to dm^3 (divide by 1000).
- Divide the moles by this volume.
- Give the answer to 3 significant figures.
Step-by-Step Reasoning
The answer is 0.0604 mol dm^-3 (3 significant figures). Note that this equals the thiosulfate concentration because the mean titre was 25.00 cm^3 — the overall 1:1 stoichiometry means equal concentrations give equal volumes.
Key Takeaways
- concentration = moles ÷ volume (in dm^3).
- Convert cm^3 to dm^3 by dividing by 1000.
- The final answer carries 3 significant figures.
Common Mistakes
- Forgetting to convert 25.0 cm^3 to dm^3 (giving 0.0000604 instead of 0.0604).
- Using the wrong volume (e.g. the titre from part (b) instead of 25.0 cm^3).
- Quoting too few significant figures (e.g. 0.06).
Things to Be Careful About
- Use 25.0 cm^3 (the pipette volume of FA 1), not the titre volume.
- The mark scheme requires answer (iv) × 1000/25.
- Show the working in at least three sections to qualify for the global working mark; equations must appear as steps.
Each reading with a burette has a maximum error of .
Grade B volumetric (bulb) pipettes are calibrated to .
Calculate the maximum error in the volume run from the burette recorded in any titration.
The maximum error is ............................... .
Working
Each titre involves two burette readings (initial and final), each with a maximum error of ±0.05 cm^3.
Maximum error = 2 × 0.05 = 0.10 cm^3
Answer
0.10 cm^3
0.10 cm^3
Background Concept
A titre is the difference between the final and initial burette readings. Each reading has a maximum error of ±0.05 cm^3. When quantities are added or subtracted, their absolute errors add. So the maximum error in the volume run from the burette is the sum of the errors in the two readings.
Understanding the Question
You are told each burette reading has a maximum error of ±0.05 cm^3. A single titre requires two readings (initial and final), so the error in the titre is the sum of the two reading errors.
Approach
Add the two ±0.05 cm^3 errors together.
Step-by-Step Reasoning
This is the maximum error in the volume run from the burette in any single titration. The sign (±) is ignored when calculating the percentage error.
Key Takeaways
- A titre involves two burette readings.
- Absolute errors add: 2 × 0.05 = 0.10 cm^3.
Common Mistakes
- Using only 0.05 cm^3 (forgetting there are two readings).
- Using 0.025 cm^3 (dividing instead of adding).
Things to Be Careful About
- The answer is 0.10 cm^3 (or 0.1 cm^3) — the mark scheme accepts 0.1(0).
- Ignore any sign; only the magnitude matters.
Express the maximum error calculated in (i) as a percentage error for the volume calculated in (b).
The maximum error is .................................. %.
Working
Answer
0.40%
0.40%
Background Concept
The percentage error of a measurement is the absolute error divided by the measured value, multiplied by 100:
Here the absolute error is the 0.10 cm^3 from part (d)(i) and the measured value is the mean titre from part (b), 25.00 cm^3.
Understanding the Question
Express the maximum error in the burette volume (0.10 cm^3) as a percentage of the volume calculated in part (b) (the mean titre, 25.00 cm^3).
Approach
Divide 0.10 by 25.00 and multiply by 100.
Step-by-Step Reasoning
The answer is 0.40%. The larger the titre, the smaller the percentage error — this is why using a large titre volume improves precision.
Key Takeaways
- Percentage error = (absolute error ÷ measured value) × 100.
- The percentage error decreases as the titre volume increases.
Common Mistakes
- Using 0.05 cm^3 (the single-reading error) instead of 0.10 cm^3.
- Using the rough titre instead of the mean titre from part (b).
- Forgetting to multiply by 100.
Things to Be Careful About
- Use the mean titre from part (b) as the denominator.
- The mark scheme requires the expression 0.1/(candidate titre in (b)) × 100.
- Quote the answer with the % sign.
Calculate the percentage error when of FA 1 was pipetted into the conical flask.
The error was .................................. %.
Working
Answer
0.24%
0.24%
Background Concept
A Grade B volumetric (bulb) pipette is calibrated to ±0.06 cm^3. When 25.0 cm^3 of FA 1 is pipetted into the flask, the maximum error in that volume is 0.06 cm^3. The percentage error is the absolute error divided by the volume, multiplied by 100.
Understanding the Question
Calculate the percentage error when 25.0 cm^3 of FA 1 is pipetted. The pipette tolerance is ±0.06 cm^3.
Approach
Divide 0.06 by 25.0 and multiply by 100.
Step-by-Step Reasoning
The answer is 0.24%. This is smaller than the burette percentage error (0.40%) because the pipette delivers a relatively large volume with a small tolerance.
Key Takeaways
- Percentage error = (absolute error ÷ measured value) × 100.
- The pipette error (0.24%) is smaller than the burette error (0.40%) here.
Common Mistakes
- Using 0.05 cm^3 (burette error) instead of 0.06 cm^3 (pipette error).
- Using the titre volume instead of 25.0 cm^3.
- Forgetting to multiply by 100.
Things to Be Careful About
- Use the pipette tolerance 0.06 cm^3 and the pipette volume 25.0 cm^3.
- The mark scheme accepts 0.240/0.24, or 0.2 if 0.24 is seen.
- Quote the answer with the % sign.
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