1. EXM.1B.SL.TZ0.

A student investigated the effect of storage time on the iron (II) content of raw spinach
using a titration with 0.01M KMnO4 in acid medium.

The equation is:

5Fe+2 (aq) + MnO4− (aq) + 8H+ (aq) → 5Fe+3 (aq) + Mn2+ (aq) + 4H2O (l)

The student acquired the spinach and stored it in the dark in a sealed bag at room
temperature. She tested the initial Fe(II) content (Day 1) on 3 samples of 2.0 g each and
then each day until day 5. The spinach leaves were roughly torn in pieces and placed in a
flask with water for 5 minutes and titrated.

(a)

The student reported the volumes of titrant used per trial for samples collected each day in
the following table:

[[N/A]]

(a.i)

The candidate used a 25 cm3 burette with an uncertainty of ±0.05 cm3. Comment on the
uncertainty recorded for the titrant volumes.

[1]

Markscheme

Incorrect AND two readings, uncertainty is ±0.1 ✔

(a.ii)

1
Calculate the initial % content of Fe2+ in the raw spinach, showing your working.

[3]

Markscheme

«mol» MnO4− «=0.00339 × 0.01» = 3.38 × 10−5 «mol» ✓ «mol MnO4−:

mol Fe+2 = 1:5» «mol» Fe2+ = 1.95 × 10−4 ✓ % Fe2+ «= 1.95 × 10−4 × 55.8 ×
100/2.0»= 0.47«%» ✓ Must show working for the marks.

(a.iii)

The results calculated for the subsequent days are shown.

Comment on the significance of the difference in Fe2+ content measured for day 4 and 5.

[1]

Markscheme

no difference AND uncertainty larger than difference ✔ Accept other

explanations referred to overlapping.

(b.i)

Suggest two flaws in the design that could have contributed to the random error in the
investigation.

[2]

Markscheme

2
 dilute the titrant to use larger volumes «of titrant» ✔ ensure spinach leaf
fragments are the same size ✔

(b.ii)

The student did not standardise the KMnO4 solution used for titration. Suggest what type
of error this may have caused, giving your reasons.

[1]

Markscheme

systematic error AND all values «equally» inaccurate ✔

(c.i)

The titration of Fe(II) with MnO4 in acid medium is a redox reaction. State the oxidised
and reduced species, including their change in oxidation states.

Oxidised:
........................................................................................................................................

Reduced: ........................................................................................................................
................

[2]

Markscheme

Oxidised: Fe+2 → Fe+3 ✔ Reduced: Mn7+ → Mn2+ ✔

(c.ii)

Spinach contains a large amount of antioxidant compounds, including ascorbic acid and
oxalic acid. Predict how this will affect the accuracy of the results, mentioning the
type and direction of the error.

[2]

3
 Markscheme

systematic error AND lower accuracy ✔ overestimation of [Fe(II)] ✔

2. EXM.1B.SL.TZ0.2

Broccoli is a rich source of ascorbic acid (vitamin C). To investigate the importance of
storage temperature of ascorbic acid, a sample of broccoli was stored at different
temperatures, from 5 °C (refrigerator temperature) to 75 °C at 10 °C intervals. A simple
colourimetric method based on the reaction of colourless ascorbic acid, AA with a reagent,
R, that produces a coloured complex, AAR, was used to measure the ascorbic acid content.

AA (aq) + R (aq) → AAR (aq)

colourless purple

(a)

A calibration curve with pure ascorbic acid and appropriate amounts of the reagent, R, was
prepared by dilutions with water of an initial aqueous solution of 100 μg/cm−3
ascorbic acid in water, AA (aq)

[[N/A]]

(a.i)

Calculate the volumes of pure ascorbic acid solution required for each point of the
calibration curve; point 4 of the curve is shown as an example.

[2]

4
 Markscheme

1- 1.0 cm3 2- 4.0 cm3 ✔ 3- 8.0 cm3 5- 4.0 cm3 ✔ Award [1] for 2 correct
answers

(a.ii)

The resulting calibration curve is shown:

Suggest a range of absorbance values for which this curve can be used to calculate ascorbic
acid of broccoli accurately.

[1]

Markscheme

0.050−1.000 ✔

(a.iii)

Suggest what should be used as a blank for spectrophotometric reading.

[1]

5
 Markscheme

water AND all samples dissolved «in water» ✔

(a.iv)

Discuss why it is important to obtain a value of R2 close to 1 for a calibration curve.

[2]

Markscheme

ensures the line is best-fit ✔ line/equation of the line will be used for
quantitation ✔ Accept any other explanations referring to accuracy.

(b)

After 3 days, the broccoli samples were removed from storage and 1.0 g of each sample
was blended with 100.0 cm3 of water. The filtered solution was mixed with the
reactant in the same proportions as that used for the calibration curve in a cuvette and
measured.

The sample stored at 5 °C showed an absorbance of 0.600. Determine the concentration of

ascorbic acid in the sample solution by interpolation and using the line equation.

interpolation in graph:
..........................................................................................................................

using line
equation: .........................................................................................................................
....

[2]

Markscheme

6
 Interpolation: 9.8 μg cm−3 ✔ using equation: 0.600/0.06283 =
9.55 «μg cm−3» ✔

(c)

Suggest why water was chosen to extract ascorbic acid from the spinach leaves with
reference to its structure.

[2]

Markscheme

«ascorbic acid» has multiple −OH/hydroxyl groups ✔ can H-bond with

water ✔ Do not accept OH−/hydroxide for M1

(d)

The content of ascorbic acid in broccoli was calculated in mg per 100 g of broccoli for all
values of temperature and plotted.

[[N/A]]

(d.i)

7
Estimate the % change in ascorbic acid concentration when stored for 3 days storage at
5 °C and 20 °C.

[1]

Markscheme

Δ % = «95.5 - 50.0/95.5 × 100»= 47.6 % ✔ Accept calculations using line

equation

(d.ii)

Estimate how much ascorbic acid will remain after 6 days storage at 20 °C in the same
experimental conditions, stating any assumption made for the calculation.

[3]

Markscheme

assumption: linear decrease ✔ rate «mg 100 g−1 day−1 = 95.5 − 50.0 / 3 » =
15 «mg 100 g−1 day−1» ✔ «95.5 − 15 × 6 = 5.5 «mg 100 g−1 day−1» ✔

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