Cambridge International Examinations

Cambridge International Advanced Subsidiary and Advanced Level

*9763634822*

CHEMISTRY 9701/36
Paper 3 Advanced Practical Skills 2 October/November 2014
2 hours
Candidates answer on the Question Paper.
Additional Materials: As listed in the Confidential Instructions

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 an HB pencil for any diagrams or graphs.
Do not use staples, paper clips, glue or correction fluid.
DO NOT WRITE IN ANY BARCODES.

Answer all questions.

Electronic calculators may be used.
You may lose marks if you do not show your working or if you do not use appropriate units.
Use of a Data Booklet is unnecessary.
Session
Qualitative Analysis Notes are printed on pages 10 and 11.

At the end of the examination, fasten all your work securely together. Laboratory
The number of marks is given in brackets [ ] at the end of each question or
part question.

For Examiner’s Use

Total

This document consists of 10 printed pages and 2 blank pages.

IB14 11_9701_36/6RP
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1 You are to determine the concentration of a solution of sodium thiosulfate, Na2S2O3.

To do this you will first produce a known amount of iodine by reacting iodate(V) ions, IO3–, with an
excess of iodide ions, I–. The equation for this reaction is below.

IO3– + 5I– + 6H+ → 3I2 + 3H2O

The amount of iodine produced in this reaction can be found by titrating with thiosulfate ions. The
equation for this reaction is below.

I2 + 2S2O32– → 2I– + S4O62–

FB 1 is aqueous sodium thiosulfate, Na2S2O3.

FB 2 is aqueous potassium iodate(V) containing 3.60 g dm–3 KIO3.
FB 3 is sulfuric acid, H2SO4.
FB 4 is aqueous potassium iodide, KI.
starch indicator

(a) Method

● Fill a burette with FB 1.

● Pipette 25.0 cm3 of FB 2 into the conical flask.
● Use the measuring cylinder to add 25 cm3 of FB 3 into the conical flask.
● Use the measuring cylinder to add 10 cm3 of FB 4 into the conical flask. Brown iodine
solution is produced.
● Add FB 1 from the burette until most of the iodine has been removed and the solution in
the conical flask is yellow.
● Add 10 drops of starch indicator to the contents of the conical flask. The solution will turn
blue-black.
● Continue adding FB 1, from the burette, until the blue-black colour just disappears.
● Carry out a rough titration and record your burette readings in the space below.

The rough titre is ......................... cm3.

● Carry out as many accurate titrations as you think necessary to obtain consistent results.
● Make certain any recorded results show the precision of your practical work.
● Record, in a suitable form below, all of your burette readings and the volume of FB 1
added in each accurate titration.

II

III

IV

VI

[6]

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(b) From your accurate titration results, obtain a suitable value to be used in your calculations.
Show clearly how you have obtained this value.

25.0 cm3 of FB 2 required .................. cm3 of FB 1. [1]

(c) Calculations

Show your working and appropriate significant figures in the final answer to each step of your
calculations.

(i) Calculate the number of moles of KIO3 present in 25.0 cm3 of FB 2.

[Ar: O, 16.0; K, 39.1; I, 126.9]

moles of KIO3 = .......................... mol

(ii) The equations for the production of iodine and its titration with thiosulfate are shown below.

IO3– + 5I– + 6H+ → 3I2 + 3H2O

I2 + 2S2O32– → 2I– + S4O62–

Use these equations to calculate the number of moles of thiosulfate present in the volume
of FB 1 you calculated in (b).

moles of S2O32– = .......................... mol

(iii) Calculate the concentration, in mol dm–3, of sodium thiosulfate in FB 1.

concentration = .......................... mol dm–3

[5]

[Total: 12]

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2 In Question 1 iodide ions were oxidised by iodate(V) ions. Iodide ions can also be oxidised by
peroxodisulfate ions, S2O82–, and you are to investigate the rate of this reaction.

2I– + S2O82– → I2 + 2SO42–

The rate of this reaction can be measured by adding thiosulfate ions, S2O32–, and starch solution to
the mixture. As the iodine is produced, it reacts immediately with the thiosulfate ions and is reduced
back to iodide according to the reaction below.

I2 + 2S2O32– → 2I– + S4O62–

After all the thiosulfate has reacted, the iodine turns the starch indicator blue-black. The rate of
reaction may be determined by timing how long it takes for the mixture to turn blue-black.
1
The rate of the reaction can be represented by rate = .
reaction time
(a) Method

FB 4 is aqueous potassium iodide, KI.

FB 5 is 0.020 mol dm–3 potassium peroxodisulfate, K2S2O8.
FB 6 is 0.010 mol dm–3 sodium thiosulfate, Na2S2O3.
starch indicator

Read through the method before you start any practical work and prepare a suitable table for
your results in the space at the top of page 5.

● Empty and wash thoroughly the burette that you used in Question 1.

Experiment 1
● Use the measuring cylinder to add 20 cm3 of FB 4 into a 100 cm3 beaker.
● Use the 10 cm3 pipette to add 10.0 cm3 of FB 6 to the beaker.
● Add 10 drops of starch indicator to the beaker.
● Fill a burette with FB 5.
● Run 20.00 cm3 of FB 5 into a second 100 cm3 beaker.
● Add the contents of the first beaker to the second beaker and start timing immediately.
● Stir the mixture once and place the beaker on a white tile.
● Stop timing as soon as the solution goes blue-black.
● Record this reaction time to the nearest second.
● Wash out both beakers and shake dry.

Experiment 2
● Use the measuring cylinder to add 20 cm3 of FB 4 into a 100 cm3 beaker.
● Use the 10 cm3 pipette to add 10.0 cm3 of FB 6 to the beaker.
● Add 10 drops of starch indicator to the beaker.
● Fill the second burette with distilled water.
● Run 10.00 cm3 of FB 5 into the second 100 cm3 beaker.
● Run 10.00 cm3 of distilled water into this second beaker containing FB 5.
● Add the contents of the first beaker to the second beaker and start timing immediately.
● Stir the mixture once and place the beaker on a white tile.
● Stop timing as soon as the solution goes blue-black.
● Record this reaction time to the nearest second.
● Wash out both beakers and shake dry.

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Record your results in the space below. You should show the volume of FB 5, the volume of
water and the reaction time for each experiment.

[3]

(b) Carry out three further experiments to investigate how the reaction time changes with different
volumes of peroxodisulfate. Remember that the combined volume of peroxodisulfate solution,
FB 5, and distilled water must always be 20.00 cm3. Do not use a volume of FB 5 that is less
than 4.00 cm3.
Record the volume of FB 5, the volume of water and the reaction time for each experiment.

II

III

IV

[4]

(c) Use your results from (a) and (b) to complete the table below. You should show the volume of
FB 5, the reaction time and the volume of FB 5 × reaction time.

[2]

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(d) A student who had carried out these experiments concluded that the rate of reaction was
directly proportional to the volume of FB 5.

Using your values from (c), explain whether your results agree with this conclusion.

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

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

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

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

(e) Another student thought that the experiment could be made more accurate by giving longer
reaction times. To do this he repeated Experiment 1 with the same volumes but using
0.100 mol dm–3 sodium thiosulfate instead of FB 6. He found that the reaction never turned
blue-black. Explain why.

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

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

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

(f) Describe how you could modify this experiment to investigate the effect of the concentration of
iodide ions, FB 4, on the rate of the reaction.

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

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

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

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

[Total: 13]

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3 Qualitative Analysis

At each stage of any test you are to record details of the following.

● colour changes seen

● the formation of any precipitate
● the solubility of such precipitates in an excess of the reagent added

Where gases are released they should be identified by a test, described in the appropriate place
in your observations.

You should indicate clearly at what stage in a test a change occurs.

Marks are not given for chemical equations.
No additional tests for ions present should be attempted.

If any solution is warmed, a boiling tube MUST be used.

Rinse and reuse test-tubes and boiling tubes where possible.

Where reagents are selected for use in a test, the name or correct formula of
the element or compound must be given.

Half fill the 250 cm3 beaker with water and heat it until the water is approximately 60 °C. Leave to
stand. This water will be used as a water bath. Turn off the Bunsen burner when the water is hot.

(a) FB 7 and FB 8 are aqueous solutions. One of the elements present in the different ions in FB 7
and FB 8 is the same.

Carry out the following tests on FB 7 and FB 8 and complete the table.

test observations
(i) To a 1 cm depth of FB 7 in a
test-tube add a 1 cm depth of
aqueous silver nitrate.

(ii) To a 1 cm depth of FB 7 in a
test-tube add aqueous sodium
hydroxide.

(iii) To a 1 cm depth of FB 7 in a
test-tube add a 1 cm depth of
aqueous sodium hydroxide and
then a 1 cm depth of hydrogen
peroxide. Leave to stand.

(iv) Before starting this test, the

Bunsen burner must be turned off.
To a 2 cm depth of dilute sulfuric
acid add a few drops of FB 8 then
add a 1 cm depth of ethanol. Leave
to stand in the water bath.

[5]

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(b) What element is present in both FB 7 and FB 8?

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

(c) Solid FB 9 and aqueous solution FB 10 both contain the same cation.

(i) Transfer approximately half of the FB 9 into a hard-glass test-tube and heat.

observations .......................................................................................................................

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

(ii) Transfer the remaining FB 9 into a boiling tube and carefully add dilute sulfuric acid.

observations .......................................................................................................................

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

(iii) To a 1 cm depth of FB 10 in a test-tube, add a piece of magnesium ribbon. Leave to stand.

observations .......................................................................................................................

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

(iv) To a 1 cm depth of FB 10 in a test-tube, add an equal depth of concentrated hydrochloric

acid (care: this is very corrosive).

observations .......................................................................................................................

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

(v) Suggest which cation is present in both FB 9 and FB 10.

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

(vi) What change in the oxidation state of magnesium is occurring during reaction (c)(iii)?

Oxidation state change from ................................... to ...................................

[8]

(d) In which part of the Periodic Table are the elements identified as being present in FB 7, FB 8,
FB 9 and FB 10?

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

[Total: 15]

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Qualitative Analysis Notes

Key: [ppt. = precipitate]

1 Reactions of aqueous cations

reaction with
ion
NaOH(aq) NH3(aq)

aluminium, white ppt. white ppt.

Al 3+(aq) soluble in excess insoluble in excess

ammonium, no ppt.
–
NH4+(aq) ammonia produced on heating

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 grey-green ppt.

Cr3+(aq) giving 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

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 off-white ppt. rapidly turning brown
manganese(II),
on contact with air on 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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2 Reactions of anions

ion reaction

carbonate, CO2 liberated by dilute acids

CO3 2–

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

Cl –(aq)

bromide, gives 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)
SO4 (aq) 2–

sulfite, SO2 liberated with dilute acids;

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

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, Cl 2 bleaches damp litmus paper
hydrogen, H2 “pops” with a lighted splint
oxygen, O2 relights a glowing splint
turns acidified aqueous potassium manganate(VII) from purple to
sulfur dioxide, SO2
colourless

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© UCLES 2014 9701/36/O/N/14