UNIVERSITY OF CAMBRIDGE INTERNATIONAL EXAMINATIONS

General Certificate of Education Advanced Subsidiary Level and Advanced Level

*3318230628*

CHEMISTRY 9701/31
Paper 31 Practical Test October/November 2007
2 hours
Candidates answer on the Question Paper.
Additional Materials: As listed in the Instructions to Supervisors

READ THESE INSTRUCTIONS FIRST

Write your Centre number, candidate number and name on all the work you hand in.
Give details of the practical session and laboratory where appropriate, in the boxes provided.
Write in dark blue or black pen.
You may use a soft pencil for any diagrams, graphs or rough working.
Do not use staples, paper clips, highlighters, glue or correction fluid.
DO NOT WRITE IN ANY BARCODES.

Answer all questions.

You are advised to show all working in calculations.
Use of a Data Booklet is unnecessary.

Qualitative Analysis Notes are printed on pages 11 and 12. Session

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
part question. Laboratory

For Examiner’s Use

Total

This document consists of 12 printed pages and 1 Insert.

SP (SM/KS) T47239/2
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 2 For
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1 Read through question 1 before starting any practical work.

You are provided with the following reagents.

FA 1 containing 37.0 g dm–3 of hydrated sodium thiosulphate, Na2S2O3.5H2O
FA 2 2.0 mol dm–3 hydrochloric acid, HCl
distilled water

Aqueous thiosulphate ions, S2O32–, decompose in the presence of hydrogen ions, H+.

S2O32–(aq) + 2H+(aq) → S(s) + SO2(g) + H2O(l)

The rate of reaction can be followed by observing the formation of a fixed amount of sulphur
as a fine suspension of solid particles in the solution.

The rate of decomposition at a fixed temperature is affected by

• the concentration of thiosulphate ions, [S2O32–];
• the concentration of hydrogen ions, [H+].

In a series of experiments where the concentration of a reagent is changed

• 1/time can be used as a measure of rate,
• the volume of the reagent used can be taken as a measure of its concentration,
providing the total volume of the mixture is kept constant in each experiment.

The order of reaction with respect to thiosulphate ions can be obtained by plotting a graph of
log rate against log [S2O32–].

log rate order of reaction = gradient of straight line

log [S2O32–]

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(a) Method

Experiment 1

• Fill the burette labelled FA 1 with FA 1.

• Run 50.00 cm3 of FA 1 from the burette into a 250 cm3 beaker.
• Measure 5 cm3 of FA 2 in a measuring cylinder.
• Tip the acid FA 2 from the measuring cylinder into the beaker and immediately
start a stop-clock or note the start time on a clock with a second hand.
• Swirl the beaker to mix the reagents and place the beaker over the printing on the
insert provided.
• Observe the printing by looking down through the solution in the beaker.
• Stop the clock or note the time when the printing is just no longer visible.
• Record the time taken to the nearest second.

The time taken is ................. s.

Experiment 2

• Empty and rinse the beaker used in experiment 1. Carefully dry the beaker with a
paper towel.
• Refill the burette labelled FA 1 with FA 1.
• Fill the second burette, labelled water, with distilled water.
• Run 10.00 cm3 of FA 1 and 40.00 cm3 of distilled water from the burettes into the
250 cm3 beaker.
• Measure 5 cm3 of FA 2 in a measuring cylinder.
• Tip the acid FA 2 into the beaker, start the clock or note the time, mix the reagents
and place over the printing as in experiment 1.
• Stop the clock or note the time when the printing is just no longer visible.
• Record the time taken to the nearest second.

The time taken is ................. s.

[2]

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(b) In experiment 1 you will have obtained the time taken for a ‘fast’ reaction and in
experiment 2 the time taken for a ‘slow’ reaction.

You are to repeat the experiment with further mixtures in which only the concentration
of thiosulphate ions is varied.
In selecting the mixtures to be used you should consider
• how many mixtures need to be used,
• what concentrations of thiosulphate ion should be used,
• what range these concentrations should cover,
• that only the concentration of thiosulphate ion must change.

Remember – you already have reaction times for two mixtures with different
concentrations of thiosulphate ion.

In the space below prepare to record, in an appropriate form, the results of the
experiments you will perform and the results of experiments 1 and 2.

Your recorded results should include calculated values to enable you to plot

log (1/time) against log (volume of FA 1).

Carry out the additional experiments and record your results.

ii

iii

iv

vi

vii

viii

ix

xi
[11]

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(c) Use the grid below to plot a graph of log (1/time) against log (volume of FA 1).
Draw an appropriate straight line through the points plotted.

[4]
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(d) Draw construction lines on your graph and obtain data from them to enable you to
calculate the gradient of the graph.
Calculate the gradient of the line drawn, which is the order of reaction with respect to
thiosulphate ions.

The reaction is ................................ order with respect to thiosulphate ions, S2O32–. [3]

(e) The moment at which the printing is just obscured can be difficult to judge and will vary
from person to person.
Explain why this uncertainty for experiment 1 in section (a) will be less than the uncertainty
for experiment 2 in section (a).

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

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

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

Estimate a value (± seconds) for the uncertainty in each of experiments 1 and 2 and
express this uncertainty as a percentage of the time for the reaction.

experiment 1 experiment 2

reaction time / s

uncertainty / s ± ±

percentage uncertainty

[3]

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(f) The experimental method can be modified to enable the rate of reaction with respect to
hydrogen ions, H+, to be investigated.
You will perform two further experiments using the method for experiment 2 in
section (a). You will keep the concentration of thiosulphate ions constant and vary the
concentration of hydrogen ions.
First copy the reaction time from your results to experiment 2 in section (a) into the table
below. Then complete the table below to show the volumes of FA 1, FA 2, and distilled
water you will use in these two further experiments.
Carry out each experiment as before and record the time taken in each case.

volume of FA 1 volume of FA 2 volume water reaction time

/ cm3 / cm3 / cm3 /s

experiment 2
10.00 5 40.00
in section (a)

experiment i

experiment ii

[1]

(g) Use the experimental results from the three experiments to draw a conclusion as to how
the rate of reaction is affected by changing the concentration of hydrogen ions.

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

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

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

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

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

[Total: 25]

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2 The four solutions FA 3, FA 4, FA 5 and FA 6 each contain one of the following anions.
nitrate, NO3–
nitrite, NO2–
sulphate, SO42–
sulphite, SO32–

(a) Use information from the Qualitative Analysis Notes on page 12 to answer the following
questions.

What single reagent could you use to identify the solution containing the nitrite ion?

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

What reagents could you use to identify the sulphate and sulphite ions?

................................................................. and .................................................................

[1]

(b) Use the reagents selected in (a) to test each of the four solutions.
Record in the space below, the reagents used and the observations made.

From your observations identify the solutions containing nitrite, sulphate and sulphite
ions.

Solution ................ contains the nitrite ion.

supporting evidence ........................................................................................................

Solution ................ contains the sulphate ion.

supporting evidence ........................................................................................................

Solution ................ contains the sulphite ion.

supporting evidence ........................................................................................................

[7]

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(c) You are to perform the tests given in the table below with each of the solutions FA 3, FA 4,
FA 5 and FA 6 to identify three of the cations present. One of these cations is the
Ba2+ ion.
Record details of colour changes seen, the formation of any precipitate and the solubility
of any such precipitate in an excess of the reagent added.
Where gases are released they should be identified by a test, described in the
appropriate place in the table.
You should indicate clearly at what stage in a test a change occurs.
Marks are not given for chemical equations.
No additional tests should be attempted.

observations
test
FA 3 FA 4 FA 5 FA 6

(i) To 1 cm depth of solution

in a boiling-tube, add
aqueous sodium
hydroxide a little at a
time until there is no
further change.

If no precipitate forms,
carefully warm the
solution.
CARE - heated
solutions containing
sodium hydroxide can
be ejected from the
boiling-tube.

(ii) To 1 cm depth of
solution in a test-tube,
add aqueous ammonia
a little at a time until
there is no further
change.

(iii) To 1 cm depth of
solution in a test-tube
add 1 cm depth of dilute
sulphuric acid.

(iv) To 1 cm depth of
solution in a test-tube
add 1 cm depth of
aqueous sodium
sulphite.

If a precipitate forms,
add 2 cm depth of dilute
hydrochloric acid.

[3]
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(d) From your observations in (c) you should be able to identify the cation present in three
of the solutions.

Solution ................ contains the ................ ion.

supporting evidence ........................................................................................................

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

Solution ................ contains the ................ ion.

supporting evidence ........................................................................................................

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

Solution ................ contains the ................ ion.

supporting evidence ........................................................................................................

..........................................................................................................................................
[3]

(e) Do not carry out this test.

What other reagent could you use to confirm the presence of Ba2+ in one of the
solutions?

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

[Total: 15]

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 11

Qualitative Analysis Notes

Key: [ppt. = precipitate]

1 Reactions of aqueous cations

ion reaction with

NaOH(aq) NH3(aq)

aluminium, white ppt. white ppt.

Al 3+(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)

chromium(III), grey-green ppt. soluble in excess giving grey-green ppt.

Cr3+(aq) dark green solution insoluble in excess

copper(II), pale blue ppt. blue ppt. soluble in excess

Cu2+(aq) insoluble in excess giving dark blue solution

iron(II), green ppt. green ppt.

Fe2+(aq) insoluble in excess insoluble in excess

iron(III), red-brown ppt. red-brown ppt.

Fe3+(aq) insoluble in excess insoluble in excess

lead(II), white ppt. white ppt.

Pb2+(aq) soluble in excess insoluble in excess

magnesium, white ppt. white ppt.

Mg2+(aq) insoluble in excess insoluble in excess

manganese(II), off-white ppt. off-white ppt.

Mn2+(aq) insoluble in excess insoluble in excess

zinc, white ppt. white ppt.

Zn2+(aq) soluble in excess soluble in excess

[Lead(II) ions can be distinguished from aluminium ions by the insolubility of lead(II) chloride.]

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 12

2 Reactions of anions

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

chromate(VI), yellow solution turns orange with H+(aq);

CrO2–
4
(aq) gives yellow ppt. with Ba2+(aq);
gives bright yellow ppt. with Pb2+(aq)

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

Cl –(aq) gives white ppt. with Pb2+(aq)

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

Br –(aq) gives white ppt. with Pb2+(aq)

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

I– (aq) gives yellow ppt. with Pb2+(aq)

nitrate, NH3 liberated on heating with OH–(aq) and Al foil

NO–3 (aq)

nitrite, NH3 liberated on heating with OH–(aq) and Al foil;

NO–2 (aq) NO liberated by dilute acids
(colourless NO → (pale) brown NO2 in air)

sulphate, gives white ppt. with Ba2+(aq) or with Pb2+(aq) (insoluble in excess dilute
SO2–
4
(aq) strong acid)

sulphite, SO2 liberated with dilute acids;

SO2–
3
(aq) gives white ppt. with Ba2+(aq) (soluble in excess dilute strong acid)

3 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

sulphur dioxide, SO2 turns potassium dichromate(VI) (aq) from orange to green

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