EUNOIA JUNIOR COLLEGE

JC2 Preliminary Examination 2024

General Certificate of Education Advanced Level
Higher 2

CANDIDATE
NAME

CIVICS INDEX
GROUP 2 3 – NUMBER

CHEMISTRY 9729/04
Paper 4 Practical
15 August 2024
2 hour 30 minutes

Candidates answer on the Question Paper.

Additional Materials: As listed in the Confidental Instructions

READ THESE INSTRUCTIONS FIRST

Write your name, civics group and registration number on the work you hand in.
Give details of the practical shift and laboratory, where appropriate, in the boxes provided.
Write in dark blue or black pen.
You may use an HB pencil for any diagrams or graphs.
Do not use paper clips, highlighters, glue or correction fluid.

Answer all questions in the spaces provided on the Question paper. Shift
The use of an approved scientific calculator is expected, where appropriate.
You may lose marks if you do not show your working or if you do not use
appropriate units. Laboratory

At the end of the examination, fasten all your work securely together.
The number of marks is given in brackets [ ] at the end of each question or
For Examiner’s Use
part question.
1 / 9

2 / 11

3 / 22

4 / 13

Total / 55

This document consists of 19 printed pages and 1 blank page.

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Answer all the questions in the spaces provided. For

Examiner’s
Use
1 Investigation of some reactions of ascorbic acid

Ascorbic acid, more commonly known as vitamin C, is a water-soluble vitamin with

molecular formula, C6H8O6. Ascorbic acid is a well-known antioxidant that is reasonably
stable in the solid form but oxidised quite rapidly by oxygen in air once dissolved in water.

FA 1 is a solution of ascorbic acid, C6H8O6.

FA 2 is a solution of copper(II) sulfate, CuSO4
FA 6 is 1.0 mol dm–3 hydrochloric acid, HCl

Carry out the following test. Carefully record your observations in Tables 1.1 and 1.2.

Unless otherwise stated, the volumes given below are approximate and should be
estimated rather than measured.
Table 1.1

test observations

(a) Add 2 cm depth of aqueous silver

nitrate to a clean dry boiling tube.

Add 1 cm depth of aqueous sodium

hydroxide slowly to the same tube.

Add aqueous ammonia slowly, with

shaking until the precipitate just
dissolves. You may use a clean glass
rod to help dissolve the precipitate.

Add 1 cm depth of FA 1 to this mixture

and shake the tube.

Place the boiling tube in the test-tube

rack and leave it for 3 minutes.
Important: After about 3 minutes, pour the mixture down the sink and wash
out the boiling tube several times with tap water. [2]

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Table 1.2 For

Examiner’s
Use
test observations

(b) (i) Add 2 cm depth of FA 2 to a clean

dry boiling tube.

Add 1 cm depth of FA 1 to the same

tube and shake the tube.

Gently heat the boiling tube until the

liquid boils. Place the boiling tube in
the test-tube rack and leave it to
stand.

(ii) Add 2 cm depth of FA 2 to a clean

dry boiling tube.

Add 10 drops of FA 6 to the same

tube.

Add 1 cm depth of FA 1 to the same

tube and shake the tube.

Gently heat the boiling tube until the

liquid boils. Place the boiling tube in
the test-tube rack and leave it to
stand.
[3]

(c) In (a), an organic product with molecular formula C6H6O6 is obtained from ascorbic
acid.

(i) Name the type of reaction that ascorbic acid undergoes in (a).

......................................................................................................................... [1]

(ii) State and explain the chemical change the reagent undergoes during the reaction
in (a).

.............................................................................................................................

......................................................................................................................... [1]

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(iii) Explain why ascorbic acid is not expected to react with the reagent in (a). For
Examiner’s
Use
.............................................................................................................................

.............................................................................................................................

......................................................................................................................... [1]

(d) The Cu2+ in (b) undergoes the same chemical change identified in (c)(ii).

From the appearance of the copper-containing product, state

• the oxidation state of copper in the copper-containing product in (b)(i) ...................

• the oxidation state of copper in the copper-containing product in (b)(ii) ..................

[1]

[Total : 9]

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BLANK PAGE

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2 Determination of the percentage by mass of ascorbic acid in a tablet For

Examiner’s
Use
As ascorbic acid is readily oxidised, it is easier to analyse ascorbic acid using a redox
titration rather than an acid-base titration.

–
When iodate ions, IO3, are added to an acidic solution containing iodide ions, I–, a redox
reaction occurs to produce iodine, I2.

–
equation 1 IO3 + 5I– + 6H+ → 3I2 + 3H2O

The I2 formed by this reaction is able to oxidise ascorbic acid to dehydroascorbic acid.

equation 2 C6H8O6 + I2 → 2I– + 2H+ + C6H6O6

Due to this reaction the I2 formed is immediately reduced to I– as long as there is any
ascorbic acid present. Once all the ascorbic acid has reacted, the excess I2 is free to react
with the starch indicator, forming the dark blue starch-iodine complex. This is the end-point
of the titration.

In 2(a), you will perform titrations to determine the percentage by mass of ascorbic acid
present in a vitamin C tablet.

FA 3 is a powdered vitamin C tablet, C6H8O6

FA 4 is 0.0020 mol dm–3 potassium iodate, KIO3
FA 5 is 0.200 mol dm–3 potassium iodide, KI
FA 6 is 1.0 mol dm–3 hydrochloric acid, HCl
Solution S is starch indicator

(a) (i) Preparation of standard solution of FA 3

1. Weigh the capped bottle containing solid FA 3. Record the mass in Table 2.1
on page 7.

2. Transfer all the solid FA 3* into a 250 cm3 beaker.

3. Reweigh the empty capped container. Record this mass in Table 2.1 on
page 7.

4. Dissolve the solid in about 70 cm3 of deionised water.

5. Transfer all the solution into a 250 cm3 volumetric flask.

6. Make up the solution to 250 cm3 with deionised water and mix thoroughly. You
need FA 3 solution for use in 3(a) as well. Do not pour away after the titration.

* Gently tap the capped bottle on the benchtop to loosen the solid in the bottle before
transfer and ensure that as much of solid FA 3 is transferred into the beaker as possible
without using any other aids.

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Table 2.1 For

Examiner’s
Use
mass of capped container and solid FA 3 / g

mass of emptied capped container / g

(ii) Titration of FA 3 solution against FA 4

1. Fill the burette with FA 4.

2. Use the pipette to transfer 25.0 cm3 of FA 3 solution into a 250 cm3 conical
flask.

3. Use a measuring cylinder to add 15.0 cm3 of FA 5 to the conical flask.

4. Use a measuring cylinder to add 5.0 cm3 of FA 6 to the conical flask.

5. Use a measuring cylinder to add 5.0 cm3 of solution S to the conical flask.

6. Run FA 4 from the burette into the flask. The end-point is reached when the
first permanent trace of a dark blue colour is seen.

7. Record your titration results, to an appropriate level of precision, in Table 2.2.

8. Repeat points 2 to 8 until consistent titre values are obtained.

Table 2.2

final burette reading / cm3

initial burette reading / cm3

volume of FA 4 used / cm3

[2]

(iii) From your titration results, obtain a suitable volume of FA 4 to be used in your
calculations. Show clearly how you obtained this volume.

volume of FA 4 = .................................................. cm3 [3]

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–
(b) (i) Calculate the amount of IO3 ions present in the volume of FA 4 calculated in (a)(iii). For
Examiner’s
Use

–
amount of IO3 ions = .......................................................... [1]

–
(ii) Calculate the amount of I2 formed from the amount of IO3 ions in (b)(i).

amount of I2 formed = .......................................................... [1]

(iii) Calculate the concentration of ascorbic acid in FA 3 solution.

[ascorbic acid] in FA 3 solution = .......................................................... [2]

(iv) Hence, calculate the percentage by mass of ascorbic acid, C6H8O6, in the tablet.
[Ar: H, 1.0; C, 12.0; O, 16.0]

percentage by mass of ascorbic acid in tablet = ......................................................... [2]

[Total: 11]

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3 Determination of the kinetics of the reaction between peroxodisulfate and iodide For
ions Examiner’s
Use

FA 3 solution is the standard solution of vitamin C tablet prepared in 2(a)(i)

FA 5 is 0.200 mol dm–3 potassium iodide, KI
FA 7 is 0.100 mol dm–3 ammonium peroxodisulfate, (NH4)2S2O8
Solution S is starch indicator

2–
Peroxodisulfate ions, S2O8 , in FA 7 oxidise iodide ions, I–, in FA 5 as shown below.

S2O8 (aq) + 2I–(aq) → I2(aq) + 2SO4 (aq)

2– 2–
equation 3

The iodine, I2, produced in equation 3 reacts immediately with ascorbic acid, from FA 3, as
shown in equation 2.

equation 2 C6H8O6 + I2 → 2I– + 2H+ + C6H6O6

Once all the ascorbic acid have reacted, the concentration of iodine rapidly increases and,
due to the presence of starch in the reaction mixture, the dark blue colouration of the starch-
iodine complex is formed.

The reaction in equation 3 is first order with respect to the iodide ion concentration, [I–].

You are to perform a series of experiments to determine the rate order for the reaction in
2–
equation 3 with respect to the peroxodisulfate ion concentration, [S2O8 ].

(a) Experiments

You will attempt five experiments.

• In Experiment 1, Solution A will be prepared as described on page 10.
• In the remaining experiments you will repeat the procedure from Experiment 1,
but using volumes of FA 7 of your choice.

For each experiment, you note the time taken, t, for the solution to turn dark blue.

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(i) Experiment 1 For

Examiner’s
Use
Fill the burette labelled E3 with FA 7.

• Transfer 25.00 cm3 of FA 7 to a conical flask.

Solution A

• Using a 10 cm3 measuring cylinder, add 5.0 cm3 of FA 3 solution to the beaker
labelled Solution A.

• Using a 25 cm3 measuring cylinder, add 20.0 cm3 of FA 5 to the same beaker.

• Using a 10 cm3 measuring cylinder, add 5.0 cm3 of solution S to the same
beaker.

• Mix the contents thoroughly by swirling the beaker.

1. Pour Solution A rapidly into the conical flask containing FA 7. Start the
stopwatch when you have added about half of Solution A.
2. Mix the contents thoroughly by swirling the flask.
3. Stop the stopwatch when the dark blue colour first appears.
4. Note the time elapsed, t, to the nearest second.
5. Wash the conical flask and beaker thoroughly with water and allow to drain.

(ii) Experiments 2 to 5

You are now to perform four other experiments in order to determine the rate order
2–
with respect to [S2O8 ] for equation 3. You should number these experiments 2 to 5.

In each experiment, the volumes of FA 3, FA 5 and solution S are the same as

those used in Experiment 1.

Select suitable volumes of FA 7, VFA 7, ensuring that your chosen volumes:

• allow you to obtain sufficient data to determine the order through the plotting
of a graph,
• are not larger than the volume used in Experiment 1,
• are not less than 15.00 cm3.

In each case, the total volume of the reaction mixture must be kept the same as
that used in Experiment 1, by adding deionised water as required.

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(b) Results For

Examiner’s
Use
The volumes of FA 3, FA 5 and solution S are not changed in these experiments, and
do not need to be recorded.

Prepare a table in the space provided below in which to record, for each experiment:
• all volumes apart from those of FA 3, FA 5 and solution S,
• the value of t,
• calculated values for the experimental rate of reaction.

Record your results in the table.

(i) Table of results

[5]

(ii) Use your answer to 2(b)(iii), calculate the amount of ascorbic acid used in each
experiment in 3(a).

amount of ascorbic acid = .......................................................... [1]

(iii) Use your answer to 3(b)(ii), and the equations for the reactions involved, to
2–
calculate the amount of peroxodisulfate ions, S2O8 , that reacted in each
experiment in 3(a).

2–
amount of S2O8 = .......................................................... [1]

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2–
(iv) Use your answer to 3(b)(iii) to calculate the change in concentration of S2O8 , For
2– Examiner’s
[S2O ], that occurred when enough iodine was produced to produce the dark blue
8 Use
colour in each experiment in 3(a).

2–
change in [S2O8 ] = .......................................................... [1]

(v) The expression below shows the experimental rate of this reaction as the change
2–
in concentration of S2O8 per unit time.

change in S2O82− 
experimental rate = −  106 mol dm−3 s −1
time, t
(1 mol = 10−6 mol)

Complete your table on page 11 by calculating the experimental rates of reaction

for all 5 experiments, taking into consideration the units.

2–
If you are unable to calculate a value for the change in [S2O8 ] in 3(b)(iv), use the
value −2.50  10−4 mol dm−3. (Note: this is not the actual value.) [5]

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(c) Plot a graph of experimental rate on the y-axis against VFA 7 on the x-axis. For
Examiner’s
Use
The scales of both axes must be chosen to provide an origin.

Draw the best-fit straight line through the origin, taking into account all of your plotted
points.

[3]

(d) By considering the shape of the graph in (c), state and explain the order of the reaction
2–
with respect to [S2O8 ].

....................................................................................................................................

....................................................................................................................................

....................................................................................................................................

................................................................................................................................ [2]

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(e) The order of reaction with respect to [I−] is one. With reference to experiment 1, state For
Examiner’s
and explain the expected time taken for the appearance of the dark blue colour when
Use
the experiment is carried out using a mixture comprising the following:

• 10.0 cm3 of FA 3
• 10.0 cm3 of FA 5
• 25.00 cm3 of FA 7
• 5.0 cm3 of deionised water
• 5 cm3 of solution S

....................................................................................................................................

....................................................................................................................................

....................................................................................................................................

....................................................................................................................................

....................................................................................................................................

....................................................................................................................................

................................................................................................................................ [2]

(f) A student suggested that a more accurate timing can be obtained when the volume of
FA 3 solution is measured with a burette rather than a measuring cylinder.

A teacher said that the student’s claim is incorrect. Explain why this is so.

....................................................................................................................................

....................................................................................................................................

....................................................................................................................................

................................................................................................................................ [2]

[Total: 22]

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4 Planning For
Examiner’s
Use
Ascorbic acid is a weak monobasic acid with a pKa of 4.17 at 25 ºC. Besides acid-base and
redox titration, the concentration of ascorbic acid in a standard solution of FA 3 prepared
in 2(a)(i) can also be determined by thermometrically.

This involves performing a series of experiments using different volumes of aqueous

sodium hydroxide and the standard solution of FA 3 which together give a total volume of
50 cm3. The temperature change, T, for each experiment will be determined and a graph
of T against the volume of NaOH used will then be plotted.

The volume of NaOH, Vneut, which gives the maximum temperature change, Tmax, are
obtained from the graph.

Vneut can be used to calculate the concentration of ascorbic acid in the standard solution.

Tmax can be used to calculate the heat change, q, for this experiment. Using q, a value for
the the enthalpy change of neutralisation, Hneut, of vitamin C can be determined
simultaneously.

(a) Plan an investigation to determine the concentration of vitamin C in a standard solution

of FA 3, as well as the enthalpy change of neutralisation of ascorbic acid,
thermometrically.

You may assume that you are provided with:

• a standard solution of FA 3,
• 0.100 mol dm–3 sodium hydroxide, NaOH,
• The equipment normally found in a school or college laboratory.

In your plan you should include brief details of:

• the apparatus you would use,
• the procedure you would follow,
• the measurements you would take,
• how the data measured would be used to determine values needed for the plotting
of the graph.

..................................................................................................................................

..................................................................................................................................

..................................................................................................................................

..................................................................................................................................

..................................................................................................................................

..................................................................................................................................

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For
.................................................................................................................................. Examiner’s
Use

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..................................................................................................................................

..................................................................................................................................

.............................................................................................................................. [5]

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(b) (i) Sketch the graph that you would expect to obtain on the axes in Fig. 4.1. For
Examiner’s
Use

T

0
0 volume of NaOH / cm3 50

Fig. 4.1
[2]

(ii) Explain how the maximum temperature change, Tmax. and the corresponding
volume of NaOH, Vneut, can be determined. You may find it useful to show how this
might be done on your graph in 4(b)(i).

.............................................................................................................................

.............................................................................................................................

.............................................................................................................................

.............................................................................................................................

.............................................................................................................................

......................................................................................................................... [2]

(c) (i) Derive an expression for the concentration of ascorbic acid in the standard solution
of FA 3, in terms of Vneut only.

.............................................................................................................................

.............................................................................................................................

.............................................................................................................................

.............................................................................................................................

......................................................................................................................... [2]

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(ii) Derive an expression for the enthalpy change of neutralisation of ascorbic acid, in For
terms of Tmax and Vneut only. Examiner’s
Use

Assume that the specific heat capacity of the solution is 4.2 J cm‒3 K‒1.

.............................................................................................................................

.............................................................................................................................

.............................................................................................................................

.............................................................................................................................

......................................................................................................................... [2]

[Total: 13]

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Qualitative Analysis Notes

[ppt. = precipitate]

(a) Reactions of aqueous cations

reaction with
cation
NaOH(aq) NH3(aq)
aluminium, white ppt. white ppt.
Al3+(aq) soluble in excess insoluble in excess
ammonium, ammonia produced on heating
–
NH+4 (aq)
barium, no ppt. no ppt.
Ba2+(aq) (if reagents are pure)
calcium, white. ppt. with high no ppt.
Ca2+(aq) [Ca2+(aq)]
grey-green ppt. grey-green ppt.
chromium(III),
soluble in excess insoluble in excess
Cr3+(aq)
giving dark green solution
pale blue ppt. blue ppt.
copper(II),
insoluble in excess soluble in excess
Cu2+(aq),
giving dark blue solution
green ppt., turning brown on contact green ppt., turning brown on contact
iron(II),
with air with air
Fe2+(aq)
insoluble in excess insoluble in excess
iron(III), red-brown ppt. red-brown ppt.
Fe3+(aq) insoluble in excess insoluble in excess
magnesium, white ppt. white ppt.
Mg2+(aq) insoluble in excess insoluble in excess
off-white ppt., rapidly turning brown on off-white ppt., rapidly turning brown on
manganese(II),
contact with air contact with air
Mn2+(aq)
insoluble in excess insoluble in excess
zinc, white ppt. white ppt.
Zn2+(aq) soluble in excess soluble in excess

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(b) Reactions of anions

anion reaction
carbonate, CO2 liberated by dilute acids
CO2–
3

chloride, gives white ppt. with Ag+(aq) (soluble in NH3(aq))

Cl –(aq)

bromide, gives pale cream ppt. with Ag+(aq) (partially soluble in NH3(aq))
Br–(aq)

iodide, gives yellow ppt. with Ag+(aq) (insoluble in NH3(aq))

I–(aq)
nitrate, NH3 liberated on heating with OH–(aq) and Al foil
NO–3(aq)
NH3 liberated on heating with OH–(aq) and Al foil;
nitrite,
NO liberated by dilute acids
NO–2(aq)
(colourless NO → (pale) brown NO2 in air)
sulfate, gives white ppt. with Ba2+(aq) (insoluble in excess dilute strong acids)
SO2–
4 (aq)

sulfite, SO2 liberated with dilute acids;

2– gives white ppt. with Ba2+(aq) (soluble in dilute strong acids)
SO3 (aq)

(c) Tests for gases

gas test and test result

ammonia, NH3 turns damp red litmus paper blue
carbon dioxide, CO2 gives a white ppt. with limewater
(ppt. dissolves with excess CO2)
chlorine, Cl2 bleaches damp litmus paper
hydrogen, H2 “pops” with a lighted splint
oxygen, O2 relights a glowing splint

sulfur dioxide, SO2 turns aqueous acidified potassium manganate(VII) from purple to colourless

(d) Colour of halogens

halogen colour of element colour in aqueous solution colour in hexane

chlorine, Cl2 greenish yellow gas pale yellow pale yellow
bromine, Br2 reddish brown gas / liquid orange orange-red
iodine, I2 black solid / purple gas brown purple

© EJC 9729/04/J2Prelim/24