CANDIDATE

( ) CLASS 20S0
NAME

RAFFLES INSTITUTION
2020 YEAR 6 PRELIMINARY EXAMINATION

Higher 2

CHEMISTRY 9729/04
Paper 4 Practical 26 August 2020
2 hours 30 minutes

Do not turn over the Question Booklet until you are told to do so.

READ THESE INSTRUCTIONS FIRST.

Write your name and class on the space provided when instructed to do so.
Give details of the practical shift and laboratory where appropriate, in the space provided.
Write in dark blue or black pen.
You may use an HB pencil for any diagrams or graphs.
Do not use staples, paper clips, glue or correction fluid.

Answer all questions in the spaces provided on the Question Paper.

The number of marks is given in brackets [ ] at the end of each question or part question.

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.
Qualitative Analysis Notes are printed on pages 19 and 20.

Shift

Laboratory

Bench Number

For Examiner’s Use

Question Marks

1 / 17

2 / 15

3 / 12

4 / 11

Total / 55

This document consists of 18 printed pages and 2 blank pages.

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Answer all the questions in the spaces provided.

1 Determination of the concentration of hydrogen peroxide and the relative formula mass
of hydrated halotrichite

Halotrichite is a mineral which is formed by the weathering and decomposition of pyrite

commonly found near volcanic vents. Halotrichite contains Fe2+, one other cation and one
anion.

Both potassium manganate(VII) and hydrogen peroxide are oxidising agents which will oxidise
the Fe2+ in halotrichite to Fe3+ under acidic conditions.

equation 1 MnO4−(aq) + 5Fe2+(aq) + 8H+(aq) ⎯→ Mn2+(aq) + 5Fe3+(aq) + 4H2O(l)

equation 2 2Fe2+(aq) + H2O2(aq) + 2H+(aq) ⎯→ 2Fe3+(aq) + 2H2O(l)

You may assume that the other cation and the anion present in halotrichite do not react with
potassium manganate(VII) and hydrogen peroxide.

FA 1 is a solution formed by dissolving 22.26 g of hydrated halotrichite in 100 cm3 of water.

FA 2 is 0.0200 mol dm−3 potassium manganate(VII), KMnO4.
FA 3 is aqueous hydrogen peroxide, H2O2.
FA 4 is 0.800 mol dm–3 sulfuric acid, H2SO4.

Note: FA 1 and FA 4 are also used in questions 3 and 2 respectively.

In Experiment 1, you will perform the titration of FA 1 against potassium manganate(VII),

FA 2. Analysis of your titration results will enable you to determine the relative formula mass
of hydrated halotrichite.

In Experiment 2, you will add different volumes of hydrogen peroxide, FA 3, to identical

samples of FA 1. In each case, the amount of hydrogen peroxide you add will only partially
oxidise the Fe2+ ions present. You will then complete the redox reaction of each mixture by
titration with potassium manganate(VII), FA 2. Graphical analysis of your results will enable
you to determine the concentration of the hydrogen peroxide in FA 3.

(a) (i) Experiment 1

1. Fill a burette labelled ‘FA 2’ with FA 2.

2. Use a pipette to transfer 10.0 cm3 of FA 1 into a 100 cm3 conical flask.

3. Use a measuring cylinder to add 5 cm3 of FA 4 to the conical flask.

4. Run FA 2 from the burette into the flask. The end-point is reached when the
solution first becomes a permanent pale pink or orange colour.

5. Record your titration results, to an appropriate level of precision, in Table 1.1.

6. Repeat points 2 to 5 until consistent titre values are obtained.

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Table 1.1

final burette reading / cm3

initial burette reading / cm3

volume of FA 2 used / cm3

[2]

(ii) From your titration results, obtain a suitable volume of FA 2, V1, to be used in your
calculations. Show clearly how you obtained this volume.

V1 = ……………………………….. cm3 [2]

(b) (i) Use your value for V1 from (a)(ii) to calculate the concentration of iron(II) ions,
[Fe2+], in FA 1.

[Fe2+] = ……………………………….. mol dm−3 [2]

(ii) Each formula unit of the hydrated halotrichite contains only one Fe2+.

Calculate the relative formula mass of the hydrated halotrichite.

relative formula mass = ……………………………….. [1]

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(c) Experiment 2

Each titration is to be performed once only, so great care should be taken that you do
not overshoot the end-points.

1. Fill a second burette with FA 3.

2. Use a pipette to transfer 10.0 cm3 of FA 1 into a 100 cm3 conical flask.

3. Use a measuring cylinder to add 5 cm3 of FA 4 to the conical flask.

4. Add, from the second burette, 6.00 cm3 of FA 3 to the conical flask.

5. Run FA 2 from the burette into the flask. The end-point is reached when the solution
first becomes a permanent pale pink or orange colour.

6. Record your titration results, to an appropriate level of precision, in Table 1.2.

7. Repeat points 2 to 6 using two other suitable volumes of FA 3. Your selected volumes
of FA 3 must not exceed 20.00 cm3 and should differ by at least 6.00 cm3.

Table 1.2

volume of FA 3 added / cm3 0.00

final burette reading for FA 2 / cm3

initial burette reading for FA 2 / cm3

volume of FA 2 used / cm3

 [2]
enter your value for V1 from (a)(ii) in Experiment 1

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(d) Plot a graph of volume of FA 2 used, on the y-axis, against volume of FA 3 added, on the
x-axis, on the grid in Fig. 1.1.

Your scale on the x-axis should allow you to determine by extrapolation, V2, which is the
volume of FA 3 required to react completely with 10.0 cm3 of FA 1 in the absence of
FA 2.

Draw a best-fit straight line taking into account all of your plotted points.

Fig. 1.1
[3]

(e) (i) From your graph in (d), determine V2, which is the volume of FA 3 required to react
completely with the Fe2+ present in 10.0 cm3 of FA 1 in the absence of FA 2.

V2 = ……………………………….. cm3 [1]

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(ii) Calculate the concentration of hydrogen peroxide, [H2O2], in FA 3.

[H2O2] = ……………………………….. mol dm−3 [2]

(f) Sketch the graph which you plotted in (d) on the axes given below. Label the graph
as (d).

On the same axes, sketch the graph that would be obtained if the concentration of KMnO4
in FA 2 is higher than 0.0200 mol dm−3. Label the graph as (f).

volume of FA 2 used / cm3

0
volume of FA 3 added / cm3

Explain your answer.

……………………………………………………………………………..…..……………….…..

……………………………………………………………………………..…..……………….…..

……………………………………………………………………………..…..……………….…..

……………………………………………………………………………..…..……………….…..

……………………………………………………………………………..…..……………….…..

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

[Total: 17]

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BLANK PAGE

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2 Determination of the relative atomic mass, Ar, of M in a metal hydroxide, M(OH)x, and
the enthalpy change of neutralisation, Hneut, of the reaction between H2SO4 and M(OH)x

FA 4 is 0.800 mol dm–3 sulfuric acid, H2SO4.

FA 5 is 1.20 mol dm–3 metal hydroxide, M(OH)x.

You will carry out a series of experiments where different volumes of FA 4 and FA 5 are mixed
together while keeping the total volume of solution constant. You will determine the
temperature change, T, for each experiment and plot a graph of T against volume of FA 5
used.

Using the graph, you will determine the relative atomic mass, Ar, of M in M(OH)x and the
enthalpy change of neutralisation, Hneut, for the reaction between sulfuric acid and M(OH)x.

(a) Procedure
1. Place a clean and dry polystyrene cup inside a second polystyrene cup which is
placed in a 250 cm3 glass beaker to prevent the cups from tipping over. Use a
50 cm3 measuring cylinder to transfer 10.0 cm3 of FA 4 into the polystyrene cup and
put the lid on.
2. Insert a thermometer through the lid and ensure that the bulb of the thermometer is
in contact with FA 4. Tilt the cup if necessary to ensure that the bulb of the
thermometer is fully immersed. Use the thermometer to measure the temperature of
FA 4. The temperature, T1, is the initial temperature of FA 4. Record T1 to 0.1 oC.
3. Measure 40.0 cm3 of FA 5 using another 50 cm3 measuring cylinder.
4. Open the lid of the cup and transfer the 40.0 cm3 of FA 5 into the polystyrene cup
containing FA 4. Replace the lid quickly.
5. Using the thermometer, stir the mixture continuously until it reaches its highest
temperature. Record this temperature, T2, to 0.1 oC.
6. Discard the contents of the polystyrene cup. Wash and dry it carefully.
7. Repeat steps 1 to 6 using 15.0 cm3, 20.0 cm3, 25.0 cm3, 30.0 cm3 and 35.0 cm3 of
FA 4, each time using an appropriate volume of FA 5 so that the total volume of each
mixture is 50.0 cm3.
8. Record all measurements of volume, temperature and temperature change, T, in an
appropriate format in the space provided below.

Results

[3]
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(b) Plot a graph of temperature change, T, on the y-axis, against volume of FA 5 added, on
the x-axis, on the grid in Fig. 2.1.

Draw two best-fit straight lines for the points plotted, and extrapolate both lines to find
• the maximum temperature change, Tmax,
• the volume of FA 5 required to completely neutralise FA 4.

60.0

55.0

50.0

45.0

40.0

35.0

30.0

25.0

20.0
0 1 2 3 4 5 6
Fig. 2.1

Tmax = ………………… oC

volume of FA 5 required for complete neutralisation = ………………… cm3

Hence, volume of FA 4 required for complete neutralisation = ………………… cm3

[5]

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(c) Using your answers to (b), calculate the amount of H2SO4 in FA 4 and M(OH)x in FA 5
required for complete neutralisation.

amount of H2SO4 in FA 4 = …………………..........................

amount of M(OH)x in FA 5 = …………………..........................

[1]

(d) Hence, suggest the value of x.

value of x = ………………..[1]

(e) Given that FA 5 is prepared by dissolving 16.8 g of solid M(OH)x in 250 cm3 of deionised
water, calculate the relative atomic mass of M.
[Ar: H, 1.0; O, 16.0]

relative atomic mass of M = ………………….......................... [1]

(f) Calculate the enthalpy change of neutralisation, Hneut, for the reaction between H2SO4
and M(OH)x.
You should assume that the specific heat capacity of the resultant solution is
4.18 J g−1 K−1 and that its density is 1.00 g cm−3.

Hneut = …………………………………. [2]

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(g) State and explain the effect on the magnitude of Tmax if ethanedioic acid of the same
concentration was used instead of sulfuric acid in the experiment in (a).

effect on the magnitude of Tmax ………….……...…………….……………….……………….

explanation …………………………………..…………………...………………..…………….…

………....…………………………………………...………………..…………..…………….....…

………....…………………………………………………….………………….……………..….…

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

[Total: 15]

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3 Investigation of some inorganic reactions

FA 1 is a solution of halotrichite. It contains Fe2+, a metal ion X and an anion Y.

You are to identify X and Y present in FA 1.

Carry out the following tests. Carefully record your observations in Tables 3.1 and 3.2.

Unless otherwise stated, the volumes given below are approximate and should be estimated
rather than measured. Test and identify any gases evolved.

(a) Identification of metal ion X

Table 3.1

test observations

(i) 1. Using a measuring cylinder, transfer

10 cm3 of FA 1 to a clean boiling tube.
2. Using another measuring cylinder,
measure out 10 cm3 of aqueous sodium
carbonate.
3. Use a dropping pipette to transfer 1.0 cm3
of aqueous sodium carbonate from the
measuring cylinder to the boiling tube.
4. Mix the contents of the boiling tube
thoroughly.
5. Repeat points 3 and 4 until the measuring
cylinder is empty.

(ii) Add 1 cm depth of FA 1 to a test-tube.

Add aqueous sodium hydroxide slowly, with

shaking, until no further change is seen.

Swirl and filter the mixture, collecting the filtrate

in a test-tube. The filtrate is FA 6 which should
be retained for use in (iii).

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test observations

(iii) Add 1 cm depth of FA 6 to a test-tube.

Add dilute hydrochloric acid slowly, with

shaking, until no further change is seen.

[5]

(iv) Identify the metal ion X in FA 1. Use evidence from your observations to support
your deduction.

X is .…………………………….……………...………..……………….…………………

evidence …………………………………………………………………………………...

………………………………………………………………………………………………

………………………………………………………………………………………………
[2]

(b) Identification of anion Y

Table 3.2

test observations

(i) Add 1 cm depth of FA 1 to a test-tube.

Add 5 drops of aqueous barium chloride.

Then add dilute hydrochloric acid slowly, with

shaking, until no further change is seen.

[1]

(ii) Hence, identify the anion Y in FA 1.

Y is .…………………………….……………...………..……………….……………... [1]

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(c) Planning – Separation of two cations in solution Z

You are not provided with solution Z.

Solution Z is a solution containing the cations Cu2+ and Cr3+.

Plan a procedure to separate the two cations Cu2+ and Cr3+ in solution Z so that each
cation is present in separate precipitates.

You may assume that you are provided with:

• aqueous sodium hydroxide, NaOH,
• aqueous ammonia, NH3,
• dilute hydrochloric acid, HCl,
• deionised water,
• the equipment normally found in a school or college laboratory.

In your plan you should:

• only be using the chemicals provided, but not necessarily all of them
• give brief details of the quantities of chemicals used
• identify by formulae the precipitates obtained after each separation step.

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[Total: 12]

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4 Planning

Calcium hydroxide, Ca(OH)2, is a sparingly soluble salt. In a saturated solution containing some
undissolved solid Ca(OH)2, the following equilibrium is established.

Ca(OH)2(s) ⇌ Ca2+(aq) + 2OH–(aq)

The approximate solubilities of Ca(OH)2 in deionised water and in 0.020 mol dm–3 aqueous
sodium hydroxide at 25 ºC are given in Table 4.1.

Table 4.1

approximate solubility of Ca(OH)2 at 25 ºC / mol dm–3

deionised water 0.025

0.020 mol dm–3 aqueous

0.005
sodium hydroxide, NaOH

(a) Explain why the solubility of Ca(OH)2 is lower in 0.020 mol dm–3 aqueous NaOH than in
water.

………………...………………………………………………………………..….......................

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

(b) In this question, you are to plan a procedure that allows you to determine the solubility of
Ca(OH)2 in 0.020 mol dm–3 aqueous sodium hydroxide and the solubility product of
Ca(OH)2 at 25 C.

The solubility and solubility product, Ksp, of Ca(OH)2 can be determined by titrating a
saturated solution of Ca(OH)2 against dilute hydrochloric acid placed in a burette.

You should plan to prepare:

• 150 cm3 of FA 7, a saturated solution of Ca(OH)2 in 0.020 mol dm–3 aqueous
sodium hydroxide at 25 C, separated from any undissolved solid,
• 250 cm3 of FA 8, a solution of hydrochloric acid of a suitable concentration for
titration.

You may assume that you are provided with:

• solid calcium hydroxide, Ca(OH)2,
• 0.020 mol dm–3 aqueous sodium hydroxide, NaOH,
• 0.250 mol dm–3 dilute hydrochloric acid, HCl,
• methyl orange,
• 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 make,
• how you would determine the solubility of Ca(OH)2 in 0.020 mol dm–3 aqueous
sodium hydroxide and the solubility product of Ca(OH)2 at 25 C.

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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 –
NH4+(aq)

barium,
no ppt. (if reagents are pure) no ppt.
Ba2+(aq)

calcium,
white ppt. with high [Ca2+(aq)] no ppt.
Ca2+(aq)
grey-green ppt.
chromium(III), grey-green ppt.
soluble in excess
Cr3+(aq) insoluble in excess
giving dark green solution
blue-ppt.
copper(II), pale blue ppt.
soluble in excess
Cu2+(aq) insoluble in excess
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
CO32–

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
NO3–(aq)
NH3 liberated on heating with OH–(aq) and Al foil;
nitrite,
NO liberated by dilute acids
NO2–(aq)
(colourless NO → (pale) brown NO2 in air)
sulfate,
gives white ppt. with Ba2+(aq) (insoluble in excess dilute strong acids)
SO42–(aq)

sulfite, SO2 liberated with dilute acids;

SO32–(aq) gives white ppt. with Ba2+(aq) (soluble in dilute strong acids)

(c) Tests for gases

gas test and test result

ammonia, NH3 turns damp red litmus paper blue
gives a white ppt. with limewater
carbon dioxide, CO2
(ppt. dissolves with excess CO2)
chlorine, Cl2 bleaches damp litmus paper
hydrogen, H2 “pops” with a lighted splint
oxygen, O2 relights a glowing splint
turns aqueous acidified potassium manganate(VII) from purple to
sulfur dioxide, SO2
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

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