UNIVERSITY OF CAMBRIDGE INTERNATIONAL EXAMINATIONS

General Certificate of Education Advanced Subsidiary Level and Advanced Level

*2645126014*

CHEMISTRY 9701/32
Paper 32 Advanced Practical Skills May/June 2009
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 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.
Session
Qualitative Analysis Notes are printed on pages 11 and 12.

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 Laboratory
question.

For Examiner’s Use

Total

This document consists of 12 printed pages.

SP (SHW 00157 2/08) T67843/4

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1 You are provided with the following. For

FB 1 is 0.023 mol dm–3 potassium manganate(VII), KMnO4. Examiner’s
FB 2 is aqueous ethanedioic acid, H2C2O4, made by dissolving the hydrated salt, Use

H2C2O4.2H2O.
You are also provided with the following.
1.0 mol dm–3 sulfuric acid, H2SO4
distilled water

You are required to determine the concentration, in g dm–3, of hydrated ethanedioic acid,
H2C2O4.2H2O, in FB 2.

Dilution of FB 2

(a) By using a burette, measure between 42.50 cm3 and 43.00 cm3 of FB 2 into the 250 cm3
graduated flask, labelled FB 3.
Record your burette readings and the volume of FB 2 added to the flask in the space
below.

Make up the contents of the flask to the 250 cm3 mark with distilled water. Place the
stopper in the flask and mix the contents thoroughly by slowly inverting the flask a
number of times.

Titration

Fill a second burette with FB 1.

Pipette 25.0 cm3 of FB 3 into a conical flask. Use the measuring cylinder provided to
add to the flask 25 cm3 of 1.0 mol dm–3 sulfuric acid and 40 cm3 of distilled water.
Put the thermometer in the flask and heat the solution until the temperature is just over
65 °C.
Carefully remove the thermometer and place the hot flask under the burette. If the neck
of the flask is too hot to hold safely, use a folded paper towel to hold the flask.
Run in 1 cm3 of FB 1. Swirl the flask until the colour of the potassium manganate(VII)
has disappeared then continue the titration as normal until a permanent pale pink colour
is obtained. This is the end-point.

If a brown colour appears during the titration, reheat the flask to 65 °C. The brown
colour should disappear and the titration can be completed as above.
If the brown colour does not disappear on reheating, discard the solution and start
the titration again.

Perform a rough (trial) titration and sufficient further titrations to obtain reliable i
results.
Record your titration results in the space below. Make certain that your recorded results ii
show the precision of your working. iii
iv
v
vi

[6]
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(b) From your titration results obtain a volume of FB 1 to be used in your calculations. Show For
clearly how you obtained this volume. Examiner’s
Use

[1]

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

(c) Calculate how many moles of KMnO4 were run from the burette into the conical flask.

………………… mol of KMnO4 were run from the burette into the conical flask.

Put the correct number of electrons into each of the following half-equations to balance
the electrical charges.

MnO4– + 8H+ + ……… e– Mn2+ + 4H2O

C2O2–
4 2CO2 + ……… e–

Calculate how many moles of ethanedioate ions, C2O2–

4 , reacted with the KMnO4 run
from the burette.

………………… mol of ethanedioate ions reacted with the KMnO4 run from the burette.

Calculate the concentration, in mol dm–3, of C2O2–

4 in FB 3.

The concentration of C2O2– –3

4 in FB 3 is ………………… mol dm .
i
Calculate the concentration, in mol dm–3, of C2O2–
4 in FB 2.
ii
iii
iv

The concentration of C2O2– –3 v

4 in FB 2 is ………………… mol dm .

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Calculate the concentration, in g dm–3, of H2C2O4.2H2O in FB 2. For

[Ar: H, 1.0; C, 12.0; O, 16.0] Examiner’s
Use

FB 2 contains ………………… g dm–3 H2C2O4.2H2O.

[5]

[Total: 12]

2 You are provided with the following.

FB 4, anhydrous sodium carbonate, Na2CO3
FB 5, solid sodium hydrogencarbonate, NaHCO3
3.0 mol dm–3 hydrochloric acid

You are to determine the enthalpy change of reaction,
H, for the following reactions.

Na2CO3(s) + 2HCl (aq) 2NaCl (aq) + CO2(g) + H2O(l)
H1

NaHCO3(s) + HCl (aq) NaCl (aq) + CO2(g) + H2O(l)
H2

(a) Reaction of FB 4, Na2CO3, with an excess of 3.0 mol dm–3 hydrochloric acid

Read through the following instructions carefully before starting the experimental work.

• Support the plastic cup in the 250 cm3 beaker provided.

• Use the measuring cylinder to transfer 50 cm3 of 3.0 mol dm–3 hydrochloric acid
into the plastic cup.
• Weigh the tube containing FB 4, anhydrous sodium carbonate.
• Measure and record the steady temperature of the acid in the beaker.
• Add the contents of the tube to the acid in three separate lots, taking care that
the mixture does not overflow.
• Stir and record the highest temperature obtained.
• Reweigh the tube containing residual FB 4.

Record in an appropriate form below all of your weighings and temperature

measurements together with the mass, m1, of FB 4 added and the temperature rise,

T1.

[1]

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(b) Calculate the temperature rise per gram of FB 4, Na2CO3, used in the experiment. For
Examiner’s
Use

T1 –1
m1 = ...................................... °C g [2]
(c) Calculate the enthalpy change,
H1, for the following reaction.

Na2CO3(s) + 2HCl (aq) 2NaCl (aq) + CO2(g) + H2O(l)

T

H1 = – (22.79 × m 1) kJ mol–1
1

H1 = – ........................................ kJ mol–1

(d) Reaction of FB 5, NaHCO3, with an excess of 3.0 mol dm–3 hydrochloric acid

50 cm3 of 3.0 mol dm–3 hydrochloric acid contains 0.15 mol HCl.

Calculate the mass of NaHCO3 that will react with 0.15 mol HCl.
[Ar: C, 12.0; H, 1.0; O, 16.0; Na, 23.0]

[1]

The reaction of NaHCO3(s) and HCl (aq) is endothermic.

The expected fall in temperature when 1.0 g NaHCO3(s) is added to 50 cm3, an
excess, of 3.0 mol dm–3 HCl is approximately 1.5 °C.

(e) The error in reading a –10 °C to +110 °C thermometer is ±0.5 °C.

What is the maximum error when using two temperature measurements to calculate a
temperature change?

The maximum error is ± .......................................... °C. [1]

(f) Determine the maximum percentage error in the calculated temperature change when
1.0 g of NaHCO3 is added to 50 cm3 of 3.0 mol dm–3 hydrochloric acid.

The maximum error is ± ........................................... %. [1]

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(g) Use your answer to (d) and the expected temperature change of −1.5 °C g–1 to select a For
mass of FB 5, NaHCO3, to use in an experiment with 50 cm3 of 3.0 mol dm–3 hydrochloric Examiner’s
acid. The mass selected should give an appropriate, measurable, temperature fall. Use

Note: The hydrochloric acid should be in excess and the percentage error in temperature
measurement should be kept to a minimum.

Mass of FB 5 to be used = .................................................. g.

Predicted temperature fall = ................................................ °C.

[1]

(h) Read through the instructions before starting any practical work.

• Empty, rinse, and shake dry the plastic cup used in (a).
• Support the plastic cup in the 250 cm3 beaker provided.
• Use the measuring cylinder to transfer 50 cm3 of 3.0 mol dm–3 hydrochloric acid
into the plastic cup.
• Weigh the empty tube labelled NaHCO3.
• Add the mass of FB 5 you have selected in (g) to the tube and reweigh.
• Measure and record the steady temperature of the acid in the beaker.
• Add the contents of the tube to the acid in three separate lots, taking care that
the mixture does not overflow.
• Stir and record the lowest temperature obtained.
• Reweigh the tube containing residual FB 5.

Record in an appropriate form below all of your weighings and temperature measurements
together with the mass, m2, of FB 5 added and the temperature fall,
T2.

[2]

(i) Calculate the temperature fall per gram of FB 5, NaHCO3, used in the experiment.

T2 –1
m2 = ........................................... °C g
[3]

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(j) Calculate the enthalpy change,
H2, for the following reaction. For
Examiner’s
NaHCO3(s) + HCl (aq) NaCl (aq) + CO2(g) + H2O(l) Use

T

H2 = + (18.06 × m 2 ) kJ mol–1
2

H2 = + ........................................ kJ mol–1

(k) It is not possible to measure experimentally the enthalpy change,
H3, for the following
reaction as it does not take place in the laboratory.

Na2CO3(s) + CO2(g) + H2O(l) 2NaHCO3(s)

It is possible, however, to calculate a “theoretical” value of
H3 for this reaction from the
results of the experiments you have carried out and a Hess cycle.

2HCl (aq) + Na2CO3(s) + H2O(l) + CO2(g)
H3 2NaHCO3(s) + 2HCl (aq)

H1 2
H2

2NaCl (aq) + 2CO2(g) + 2H2O(l)

Derive an equation to link
H1,
H2, and
H3.

Use your equation and the results from (c) and (j) to calculate a value for
H3.

H3 = ........................................ kJ mol–1

[2]

(l) Suggest a modification to the experimental method in order to reduce the transfer of
heat energy to or from the contents of the plastic cup during the experiment.

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

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

[Total: 15]

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3 FB 6 and FB 7 each contain one of the following sodium halides, NaCl, NaBr, NaI. For
Examiner’s
(a) Place half of the solid FB 6 provided in a test-tube. Half fill the test-tube with distilled Use

water and shake to dissolve the solid. Label the tube FB 6.

Do the same with FB 7, labelling the tube FB 7.
Keep the remaining solid for (c).

(b) You are to select appropriate reagents from those provided and to perform tests to
identify which halide ion is present in FB 6 and which in FB 7.
Retain some of the FB 7 solution for test (d).

In an appropriate form below record the tests performed and the results of those tests.

i
ii
iii
From the recorded observations the following halides are identified.
iv
FB 6 contains ......................................................

FB 7 contains ......................................................
[4]

(c) Carry out the following tests. [Care: unpleasant fumes may be produced]

test observations

FB 6 FB 7

Place the remaining solid in a clean,

dry test-tube and add 5 drops of
concentrated sulfuric acid (care: the
concentrated acid is very corrosive),

then as soon as you have made your

observation,

half fill the test-tube with distilled water

to dissolve the remaining solid and any
fumes produced.

Transfer 1 cm depth of the resulting

solution to a test-tube and add a few
drops of starch solution.

[2]
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(d) Carry out the following tests. For

Examiner’s
Use
test observations
Place 1 cm depth of the solution of FB 7
prepared in (a) in a test-tube.

Add 1 cm depth of aqueous bromine,

[Care: unpleasant fumes]
then,

add a few drops of starch solution.

[1]

(e) Use your observations and knowledge of halogen chemistry to explain the reactions in
(c) and identify the chemical behaviour of the concentrated sulfuric acid in the reaction.

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

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

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

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

Use your observations and knowledge of halogen chemistry to explain what happens
when the solutions are mixed in (d).

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

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

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

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

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(f) FB 8 and FB 9 each contain one cation from those listed on page 11. For
Examiner’s
Carry out the following tests to identify the cation present in each solution. Use

test observations

FB 8 FB 9

To 1 cm depth of solution in a test-tube,

add aqueous sodium hydroxide a little at
a time

then,

add an excess of the reagent to give no

more than 4 cm depth of solution in the
test-tube.

To 1 cm depth of solution in a test-tube,

add aqueous ammonia a little at a time

then,

add an excess of the reagent to give no

more than 4 cm depth of solution in the
test-tube.

The cation present in FB 8 is ......................................................

The cation present in FB 9 is ......................................................

[3]

[Total: 13]

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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, no ppt.
NH+
4 (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

iron(II), green ppt. turning brown on contact green ppt. turning brown on contact
Fe2+(aq) with air with air
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. rapidly turning brown off-white ppt. rapidly turning brown
Mn2+(aq) on contact with air on contact with air
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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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)

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

sulfite, 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, Cl 2 bleaches damp litmus paper

hydrogen, H2 “pops” with a lighted splint

oxygen, O2 relights a glowing splint

sulfur dioxide, SO2 turns aqueous acidified potassium dichromate(VI) (aq) from orange to green

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