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PEARSON EDEXCEL INTERNA
INTE RNATIONAL
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AS/A LEVEL
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CHEMISTRY
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Lab Book
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 Published by Pearson Education Limited, 80 Strand, London, WC2R 0RL.

www.pearsonglobalschools.com

Copies of official specifications for all Pearson Edexcel qualifications may be

found on the website: https://qualifications.pearson.com

8 Text © Pearson Education Limited 2018

1
0 Designed by Tech-Set Ltd, Gateshead, UK
2 Edited by Katharine Godfrey Smith, Helen Payne and Stephanie White
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o Typeset by Tech-Set Ltd, Gateshead, UK
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r Original illustrations © Pearson Education Limited 2018
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© The rights of Carl Howe and Nigel Saunders to be identified as authors of this
.t work have been asserted by them in accordance with the Copyright, Designs
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a and Patents Act 1988.
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r The Publishers would like to thank Mark Woods for his contributions to the text.
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e l First published 2018
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rit ISBN 978 1 292 24471 6
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accordance with the provisions of the Copyright, Designs and Patents Act
1988 or under the terms of a licence issued by the Copyright Licensing Agency,
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, Barnard’s
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e l for the copyright o wner’
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s publisher.
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r Printed in Slovakia by Neografia
o f
t
o Acknowledgements
Acknowled gements
N All artwork © Pearson Education
Education Limited 2018
.
n
o it A note from
from the publishers:
publishers:
e
r While the Publishers have made every attempt to ensure that advice on the
c
s i
qualification and its assessment is accurate, the official specification and
d associated assessment guidance materials are the only authoritative source of
r information and should always be referred to for definitive guidance. Pearson
e
h examiners have not contributed to any sections in this resource relevant to
s il examination papers for which they have responsibility.
responsibility. Examiners will not use
b this resource as a source of material for any assessment set by Pearson.
u
p
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a Neither Pearson, Edexcel nor the authors take responsibility for the safety
e of any activity. Before doing any practical activity you are legally required to
g carry out your own risk assessment. In particular,
particular, any local rules issued by
n
a your employer must be obeyed, regardless of what is recommended in this
h
c resource. Where students are required
required to write their own risk assessments they
o t must always be checked by the teacher and revised, as necessary, to cover any
t issues the students may have overlooked. The teacher should always have the
c
e j final control as to how the practical is conducted.
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 CONTENTS

INTRODUCTION 2
8
1 CORE PRACTICALS OVERVIEW 3
0
2
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o PAPER 3 PRACTICAL SKILLS 4
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PAPER 6 PRACTICAL SKILLS 5
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p 1 MEASUREMENT OF THE MOLAR VOLUME OF A GAS 6
n i
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o 2 DETERMINATION
DETERMINATION OF THE ENTHALPY CHANGE OF A REACTION USING HESS’S LAW 9
e l
o
h 3 FINDING THE CONCENTRA
CONCENTRATION
TION OF A SOLUTION OF HYDROCHLORIC ACID 13
w
n i
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o it
4 PREPARATION
PREPARATION OF A ST
STANDARD
ANDARD SOLUTION FROM A SOLID ACID AND ITS USE TO FIND
u
b THE CONCENTRA
CONCENTRATION
TION OF A SOLUTION OF SODIUM HYDROXIDE 16
rit
s i
r
d 5 INVESTIGATION
INVESTIGATION OF THE RA
RATES
TES OF HYDROL
HYDROLYSIS
YSIS OF SOME HALOGENOALKANES 19
o
n
o
ti
6 CHLORINATION OF 2-METHYLPROP
CHLORINATION 2-METHYLPROPAN-2-OL
AN-2-OL WITH CONCENTRA
CONCENTRATED
TED HYDROCHLORIC
a l
u ACID 22
c
ri
c
,
e
7 OXIDATION
OXIDATION OF PROP
PROPAN-1-OL
AN-1-OL TO PRODUCE PROP
PROPANAL
ANAL AND PROPA
PROPANOIC
NOIC ACID 25
l
a
s
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r 8 ANALYSIS
ANALYSIS OF SOME INORGANIC AND ORGANIC UNKNOWNS 1 31
r
o f
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o 9A FOLLOWING THE RA
RATE
TE OF THE IODINE–PROPAN
IODINE–PROPANONE
ONE REACTION BY A TITRIMETRIC
N
.
n METHOD 34
o it
e
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c 9B INVESTIGATING
INVESTIGATING A ‘CLOCK REACTION’ (HARCOURT–ESSON, IODINE CLOCK) 37
s i
d
r
e 10 FINDING THE ACTIVA
ACTIVATION
TION ENERGY OF A REACTION 42
h
s il
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b 11 FINDING THE Ka VALUE FOR A WEAK ACID 46
p
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e 12 INVESTIGATING
INVESTIGATING SOME ELECTROCHEMICAL CELLS 49
g
n
a
c
h 13A REDOX TITRA
TITRATIONS
TIONS WITH IRON(II) IONS AND POT
POTASSIUM
ASSIUM MANGANA
MANGANATE(VII)
TE(VII) 52
o t
c
t 13B REDOX TITRA
TITRATIONS
TIONS WITH SODIUM THIOSULFA
THIOSULFATE
TE AND IODINE 55
e j
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u 14 PREPARATION OF A TRANSI
TRANSITION
TION METAL COMPLE
COMPLEXX 58
s
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n 15 ANALYSIS
ANALYSIS OF SOME INORGANIC AND ORGANIC UNKNOWNS 2 61
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16 PREPARATION OF ASPIRI
ASPIRINN 67
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MATHS SKILLS 73
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1
 INTRODUCTION

Practical work is central to the study o chemistry. The International Advanced Subsidiary/Advanced Level (IAS/IAL)
8 specification includes 16 core practical activities that link theoretical knowledge and understanding to practical
1
0 scenarios. By completing the core practical activities, you will learn to:
2
n • ollow and interpret experimental instructions, covering a range o laboratory exercises throughout the course,
o
s
r
a with minimal help rom your teacher
e
P • manipulate apparatus, use chemicals, carry out all common laboratory procedures and use data logging (where
©
.t appropriate)
r
a
p • work sensibly and saely in the laboratory, paying due regard to health and saety requirements
n i
r • gain accurate and consistent results in quantitative exercises, and make the most o the expected observations in
o
e l qualitative exercises.
o
h
w
n i
By the end o this course, you should be able to use a variety o apparatus and techniques to:
n • design and carry out both the core practical
practical activities and your own investigations
o it
u
b • collect data that can be analysed
rit
s i • use data to draw valid conclusions.
d
r
o
n Your knowledge
knowledge and understanding o practical skills and activities will be assessed in all examination papers.
o
ti • Papers 1 and 2 (IAS), and 4 and 5 (IAL) will include questions based on practical activities, including novel scenarios.
a l
u
c
ri • Papers 3 (IAS) and 6 (IAL) will test your ability to plan practical work, including risk management and selection o
c
,
e
apparatus.
l
a
s
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r Assessment or the Practical Skills Papers 3 and 6 will ocus on our main areas:
r
o f • independent thinking
t
o
N • use and application o scientific methods and practices
.
n • numeracy and the application o mathematical concepts
o it
e
r
c
• use o apparatus and equipment.
s i
d
r The ways in which you can demonstrate these practical skills are outlined in the tables on pages 4 and 5. You may
e
h wish to tick off each element as you gain confidence.
s il
b
u
p You will find answers and maths skills required or the practicals in the back o the book.
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2
 CORE PRACTICALS OVERVIEW

8 UNIT 1 (IAS): FORMULAE, EQUATIONS AND AMOUNT OF SUBSTANCE

1
0
2 1 Measurement o the molar volume o a gas
n
o
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r
a UNIT 2 (IAS): ENERGETICS
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P 2 Determination o the enthalpy change o a reaction using Hess’s Law
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r
a UNIT 2 (IAS): REDOX CHEMISTRY AND GROUPS 1, 2 AND 7
p
n i 3 Finding the concentration o a solution o hydrochloric acid
r
o
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o 4 Preparation o a standard solution rom a solid acid and its use to find the concentration
h
w o a solution o sodium hydroxide
n i
n UNIT 2 (IAS): ORGANIC CHEMISTRY: ALCOHOLS, HALOGENOALKANES AND SPECTRA
o it
u 5 Investigation o the rates o hydrolysis o some halogenoalkanes
b
rit
s i
d 6 Chlorination o 2-methylpropan-2-ol with concentrated hydrochloric acid
r
o
n 7 Oxidation o propan-1-ol to produce propanal and propanoic acid
o
ti
a l
u
c 8 Analysis o some inorganic and organic unknowns 1
ri
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, UNIT 4 (IAL): KINETICS
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s 9a Followin
Following
g the rate o the iodine–propanone reaction by a titrimetric method
e
r
r
o f
t
9b Investigating a ‘clock reaction’ (Harcourt–Esson, iodine clock)
o
N
. 10 Finding the activation energy o a reaction
n
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r UNIT 4 (IAL): ACID–BASE EQUILIBRIA
c
s i
d 11 Finding the Ka value or a weak acid
r
e
h UNIT 5 (IAL): REDOX EQUILIBRIA
s il
b
u 12 Investigating some electrochemic
electrochemical
al cells
p
t
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e 13a Redox titrations with iron(II) ions and potassium manganate(VII)
manganate(VII)
g
n
a
h 13b Redox titrations with sodium thiosulate and iodine
c
o t
t UNIT 5 (IAL): TRANSITION METALS AND THEIR CHEMISTRY
c
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b 14 Preparation o a transition metal complex
u
s
t
n UNIT 5 (IAL): ORGANIC NITROGEN COMPOUNDS: AMINES, AMIDES, AMINO ACIDS AND PROTEINS
e t
n 15 Analysis o some inorganic and organic unknowns 2
o
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a UNIT 5 (IAL): ORGANIC SYNTHESIS
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o 16 Preparation o aspirin
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3
 PAPER 3 PRACTICAL SKILLS

Practical skills Core Practical

8 Independent thinking in a practical context 1 2 3 4 5 6 7 8
1
0
2 Solve problems set in a practical context
n
o
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a
e Apply scientific knowledge to practical contexts
P
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r Use and application of scientific methods and
a
p 1 2 3 4 5 6 7 8
n i practices
r
o Identiy and state how to control variables to
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o improve experimental validity
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w Present data in appropriate ways
n i
n
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u Evaluate results and draw conclusions
b
rit
s i
r
d Appreciate measurement
measurement uncertainties and errors
o
n
o
ti Comment on the method or an experiment
a l
u
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ri
c Numeracy and the application of mathematical
, 1 2 3 4 5 6 7 8
e l
a concepts in a practical context
s
e
r Plot and interpret graphs
r
o f
t
o Process and analyse data using appropriate
N
.
n mathematical skills
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r Use appropriate numbers o significant figures
c
s i based on the experimental data
d
r Consider the accuracy and precision o data
e
h
s il
b
u Use of apparatus and equipment 1 2 3 4 5 6 7 8
p
t
a Recognise a range o laboratory apparatus and
e
g
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select appropriate apparatus or a particular
a scenario
h
c
o t Understand how to use a range o apparatus and
t
c techniques appropriate
appropriate to the knowledge and
e j
b understanding included in the specification
u
s
t Consider the range and resolution o apparatus
n
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o
c Identiy health and saety issues and discuss how
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a
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4
 PAPER 6 PRACTICAL SKILLS

Practical skills Core Practical

8 Independent thinking in a practical context 9a 9b 10 11 12 13a 13b 14 15 16
1
0
2 Solve problems set in a practical context
n
o
s
r
a
e Apply scientific knowledge to practical contexts
P
©
.t
r Use and application of scientific methods and
a
p 9a 9b 10 11 12 13a 13b 14 15 16
n i practices
r
o Identiy and state how to control variables to
e l
o improve experimental validity
h
w Present data in appropriate ways
n i
n
o it
u Evaluate results and draw conclusions
b
rit
s i
r
d Appreciate measurement
measurement uncertainties and errors
o
n
o
ti Comment on the method or an experiment
a l
u
c
ri
c Numeracy and the application of mathematical
, 9a 9b 10 11 12 13a 13b 14 15 16
e l
a concepts in a practical context
s
e
r Plot and interpret graphs
r
o f
t
o Process and analyse data using appropriate
N
.
n mathematical skills
o it
e
r Use appropriate numbers o significant figures
c
s i based on the experimental data
d
r Consider the accuracy and precision o data
e
h
s il
b
u Use of apparatus and equipment 9a 9b 10 11 12 13a 13b 14 15 16
p
t
a Recognise a range o laboratory apparatus and
e
g
n
select appropriate apparatus or a particular
a scenario
h
c
o t Understand how to use a range o apparatus and
t
c techniques appropriate
appropriate to the knowledge and
e j
b understanding included in the specification
u
s
t Consider the range and resolution o apparatus
n
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n
o
c Identiy health and saety issues and discuss how
ll
a
,f these may be dealt with
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5
 CORE PRACTICAL 1: SPECIFICATION
REFERENCE

MEASUREMENT OF THE MOLAR VOLUME OF A GAS 1.11

Procedure
Objectives
8 1 Set up the apparatus to capture and measure gas evolved rom a reaction
1 ● To find the
the volume
volume o
o one mole
mole
0 in the boiling tube.
2
n o carbon dioxide gas
o 2 Place 30 cm3 o 1 mol dm−3 ethanoic acid in the boiling tube.
s
r
a 3 Place approximately 0.05 g o calcium carbonate in a test tube. Weigh the Equipment
e
P
test tube and its contents accurately. ● bo
boil
ilin
ing
g tu
tube
be
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.t ● st
stan
and d and
and clam
clampp
r 4 Remove the bung rom the boiling tube and tip the calcium carbonate into
a
p ● bung fitte
fittedd with
with delivery
delivery tube
n i
the boiling tube. Quickly replace the bung in the boiling tube.
r to fit boiling tube
o 5 Once the reaction is over, measure the volume o gas produced. ● wat
waterer bath
bath or
or gas col
collecti
lection
on
e l
o
h
6 Reweigh the test tube that contained the calcium carbonate. 3
● 100 cm measuring cylinder
w ● 50 cm3 measuring cylinder
n 7 Repeat the experiment six more times, increasing the mass o calcium
i
n carbonate by about 0.05 g each time. Do not exceed 0.40 g o calcium ● tes
estt tu
tube
o it
u carbonate. ● ma
massss balan
balancece (2 d.p
d.p.)
.)
b
rit mol dm−3 ethanoic acid
● 1 mo
s i Learning tips
d ● pow
powdered
dered calc
calcium
ium carb
carbonat
onatee
r
o ● Ensure that points
points plotted on
on a graph take
take up more than hal the available
available
n ! Safety
o
ti
space on each scale. Axes must occupy at least hal o the space on the
a l ● Wear
Wear eye prot
protectio
ection.
n.
u graph paper.
c
ri ● Re
Remo
moveve the
the bung
bung i the
c ● Keep scales
scales simple: one large square
square as 5 or
or 10 or 20 is ideal.
ideal. A scale where
, delivery tube gets blocked,
e l one large square represents 3 or 7 units (or similar) is very difficult to plot
a clear the blockage and repeat
s on, and this ofen leads to errors.
e
r
r
the procedure rom the start.
o f
● Always consider whether
whether the graph line should
should go through
through the origin.
t
● Avo
Avoid
id skin
skin conta
contact
ct with
with the
the
o ● Straight lines should
should be drawn
drawn with the aid o a ruler long enough to
to cover
N ethanoic acid, especially i the
. the ull length o the line.
n
o
skin is broken or sensitive.
it
e
r
c Results (Use this space to record your results.)
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6
 CORE PRACTICAL 1: SPECIFICATION
REFERENCE

MEASUREMENT OF THE MOLAR VOLUME OF A GAS 1.11

Analysis of results
8 1 Plot a graph o mass o calcium carbonate (on the x-axis) against volume o carbon dioxide
1
0 collected (on the y-axis). Draw
Draw a straight line o best fit – this line must pass through the
2
n origin.
o
s
r
a
e
P
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r
a
p
n i
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o
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w
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,
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a
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e
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o f
t
o
N
.
n
o it
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c
s i
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b
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t
a
e
g
n 2 Use your graph to find the volume o carbon dioxide that would be made rom 0.25 g o
a
h
c calcium carbonate.
o t
t
c
e j
b
u
s
t
n
e t
n 3 In this reaction, one mole o calcium carbonate makes one mole o carbon dioxide. Calculate
o
c
ll the number o moles o calcium carbonate in 0.25 g and hence calculate the volume o one
a
,f mole o carbon dioxide gas in dm 3.
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7
 CORE PRACTICAL 1: SPECIFICATION
REFERENCE

MEASUREMENT OF THE MOLAR VOLUME OF A GAS 1.11

Questions
8 1 Write a chemical equation or the reaction between ethanoic acid, CH3COOH, and calcium carbonate.
1
0
2
n
o
s
r
a
e
P
©
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r
a 2 Why is it more accurate to find the mass o the calcium carbonate
carbonate used by weighing the test tube containing the
p
n i calcium carbonate
carbonate and then reweighing the test tube afer the calcium carbonate has been tipped out, rather than
r
o by weighing the empty test tube at the start?
e l
o
h
w
n i
n
o it
u
b
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s i
d
r
o
n
o
ti
a l
u
c
ri
c 3 Identiy the major source o error caused by the procedur
proceduree used here.
,
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a
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o f
t
o
N
.
n
o it
e
r 4 What change to the procedure/apparatus could you make to eradicate this error?
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n
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b 5 Carry out two calculations to show that the ethanoic acid was in excess in all experimental runs.
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8
 CORE PRACTICAL 2: SPECIFICATION
REFERENCE

DETERMINATION
DETERMINATION OF THE ENTHALPY CHANGE OF A REACTION USING HESS’S LAW 6.7

Procedure Objectives
8 1 Place approximately 3 g o solid potassium carbonate in a test tube.
1 ● To calcul
calculate
ate the molar
molar
0 Accurately
Accurately weigh the test tube and its contents.
2
n enthalpy change or two
o
s
cm3 o 2 mol dm–3 hydrochloric acid into a
2 Use a burette to dispense 30 cm
reactions and use Hess’s Law
r
a polystyrene cup, which is supported in a beaker. to determine the enthalpy
e
P
© 3 Measure the temperature o the acid. change or the reactions
.t
r 4 Gradually add potassium carbonate
carbonate to the acid, stirring all the time and
a Equipment
p
n i
monitoring the temperature o the acid.
r ● tw
two
o test
test tub
tubes
es
o 5 Reweigh the empty test tube.
e l ● 2 mol dm–3 dilute hydrochloric
o 6 Repeat steps 1–5 using approximately 3.5 g o potassium hydrogencarbonate
h acid
w instead o the potassium carbonate. This time, record the lowest temperature
n i ● soli
solid
d potas
potassium
sium carb
carbonat
onatee
n reached.
o it ● solid
solid pot
potas
assiu
sium
m
u
rit
b Results (Use this space to record your results.) hydrogencarbonate
s i
d ● thermomet
thermometer er able
able to
to read
read up
up
r
o Mass o test tube with potassium carbonate/g to 50 °C or more
n
o ● pol
polys
ysty
tyren
renee cup
cup
ti
a l Mass o test tube afer emptying out potassium carbonate/g
u
c
● 250 cm3 or 400 cm
cm3 beaker
ri
,
c Mass o potassium carbonate used/g ● bur
burett
ette,
e, clamp
clamp and stan
stand
d
e l
a
s Start temperatur
temperature/°C
e/°C ● st
stir
irri
ring
ng ro
rod
d
e
r
r ● ma
mass
ss balan
balance
ce (2 d.p
d.p.)
.)
o f Highest temperatur
temperature/°C
e/°C
o
t ● sp
spaatu
tulla
N
.
n
Temperature change/°C ! Safety
o it
e
r ● We
Wear
ar eye prot
protectio
ection.
n.
c
s i Mass o test tube with potassium hydrogencarbonate/g ● Avoid
Avoid skin
skin conta
contact
ct with
with the
the
d
r
e reactants and products.
h Mass o test tube afer emptying out potassium hydrogencarbonate/g
s il
b
u Mass o potassium hydrogencarbonate used/g
p
t
a
e Start temperatur
temperature/°C
e/°C
g
n
a
h Lowest temperature/°C
c
o t
t
c
e
Temperature change/°C
j
b
u
s
t
n
e t
n
o
c
ll
a
,f
o
o
r
p
d
e t
c
e
rr
o
c
n
U

9
 CORE PRACTICAL 2: SPECIFICATION
REFERENCE

DETERMINATION
DETERMINATION OF THE ENTHALPY CHANGE OF A REACTION USING HESS’S LAW 6.7

Learning tips
8 ● You can
can assume that the heat
heat capacity o the final solution is the same
same as the heat capacity
capacity o
1
0 water. The volume o water produced in the reaction is so small it can be ignored.
2
n
o
s
● For exotherm
exothermic
ic reactions
reactions,, the enthalpy
enthalpy change,
change, △H, is negative.
r
a ● Be careul to
to use equals signs correctly
correctly.. It is very easy to
to end up stating that a negative
negative
e
P
© number equals a positive number.
.t
r
a
p Analysis of results
n i
r
o
1 The equations or the reactions occurring are:
e l reaction 1: K2CO3(s) + 2HCl(aq) → 2KCl(aq) + CO 2(g) + H2O(l)
o
h
w reaction 2: KHCO3(s) + HCl(aq) → KCl(aq) + CO 2(g) + H2O(l)
n i
n Calculate the energy change or each reaction in J. (The specific heat capacity o water is
Calculate
o it
u 4.2 J g–1 °C–1.)
b
rit
s i
d
r
o
n
o
ti
a l
u
c
ri
c
,
e l
a
s
e
r
r
o f
t
o
N
.
n
o it Calculatee the enthalpy change, △H, or each reaction in kJ mol–1.
2 Calculat
e
r Assume that the hydrochloric acid is in excess.
c
s i
d
r
e
h
s il
b
u
p
t
a
e
g
n
a
h
c
o t
t
c
e j
b
u
s
t
n
e t 3 Use your results to calculate the enthalpy change or the thermal decomposition o
n
o potassium hydrogencarbonate:
c
ll
a reaction 3: 2KHCO3(s) → K2CO3(s) + CO2(g) + H2O(l)
,f
o
o
r
p
d
e t
c
e
rr
o
c
n
U

10
 CORE PRACTICAL 2: SPECIFICATION
REFERENCE

DETERMINATION
DETERMINATION OF THE ENTHALPY CHANGE OF A REACTION USING HESS’S LAW 6.7

Questions
8 1 Why is it not possible to measure the enthalpy change or the decomposition o potassium
1
0 hydrogencarbonate directly?
2
n
o
s
r
a
e
P
©
.t
r
a
p
n i
r
o
e l
o
h
w
n i
n 2 Show that the hydrochlo
hydrochloric
ric acid is in excess in both reactions.
o it
u
b
rit
s i
d
r
o
n
o
ti
a l
u
c
ri
c
,
e l
a
s
e
r
r
o f
t
o
N
.
n
o it
e
r
c
s i
d
r
e
h
s il
b
u
p
t
a
e
g
n
a
h
c
o t
t
c
e j
b
u
s
t
n
e t
n
o
c
ll
a
,f
o
o
r
p
d
e t
c
e
rr
o
c
n
U

11
 CORE PRACTICAL 2: SPECIFICATION
REFERENCE

DETERMINATION
DETERMINATION OF THE ENTHALPY CHANGE OF A REACTION USING HESS’S LAW 6.7

3 Draw an energy level diagram or each reaction: 1, 2 and 3.

8
1
0
2
n
o
s
r
a
e
P
©
.t
r
a
p
n i
r
o
e l
o
h
w
n i
n
o it
u
b
rit
s i
d
r
o
n
o
ti
a l
u
c
ri
c
,
e l
a
s
e
r
r
o f
t
o
N
.
n
o it
e
r
c
s i
d
r
e
h
s il
b
u
p
t
a
e
g
n
a
h
c
o t
t
c
e j
b
u
s
t
n
e t
n
o
c
ll
a
,f 4 Explain why the reactions are conducted in a polystyrene cup rather than a glass beaker.
o
o
r
p
d
e t
c
e
rr
o
c
n
U

12
 CORE PRACTICAL 3: SPECIFICATION
REFERENCE

FINDING THE CONCENTRATION

CONCENTRATION OF A SOLUTION OF HYDROCHLORIC ACID 8.21

Procedure Objectives
8 1 Wash out the 250 cm 3 volumetric flask with distilled water.
1 ● To find the
the concen
concentrat
tration
ion o a
0
2 2 Use the pipette to transer 25.0 cm3 o the hydrochlo
hydrochloric
ric acid solution into
n solution o hydrochloric acid
o
s
the volumetric flask. Use distilled water to make the solution up to the
r Equipment
a mark.
e
P ● bure
burette,
tte, clam
clamp
p and
and stand
stand
© 3 Prepare your apparatus or the titration. The burette should contain the
.t
r sodium hydroxide solution (previously standardised) and the conical flask ● sodium
sodium hydr
hydroxid
oxidee solutio
solution
n
a
p should contain the dilute hydrochloric acid solution. (approximately 0.08 dm , 3
n i
r 4 Pour a 25.0 cm3 aliquot o the diluted hydrochloric
hydrochloric acid into the conical previously standardised)
o
e l flask. Use phenolphthalein as the indicator. ● bench
bench hydr
hydrochl
ochloric
oric acid
o
h (approximately 1 mol dm–3)
w 5 Titrate the contents o the flask against the sodium hydroxide solution.
n i Record all burette readings to the nearest 0.05 cm 3. ● phe
phenol
nolpht
phthal
halein
ein
n
o it
u
6 The end point o this titration is indicated by the contents o the flask ● 250 cm3 conical flask
b
rit becoming pale pink. Continued swirling will cause the pink colour to ade ● 25 cm3 volumetric pipette plus
s i
d and disappear. I the pink colour persists or 5 seconds or more, the end saety filler
r
o point has been reached.
n ● 100 cm3 beakers or transer o
o 7 Conduct urther titrations until you have two concordant
concordant titres.
ti solutions
a l
u
c
8 Ask your teacher or a technician to check one o your burette readings. ● un
unnel
nel or
or filling
filling buret
burette
te
ri
c 9 Record your results in the table below.
, ● 250 cm3 beaker
e l
a ● 250 cm3 volumetric flask
s
e
r
r
Learning tips
o f ! Safety
t ● Do not include
include your
your rough titration when calculating your mean.
mean.
o ● Wear
Wear eye
eye protect
protection.
ion. Gogg
Goggles
les
N ● Give all
all burette
burette readings
readings to the nearest 0.05 cm3.
nearest 0.05
.
n are preerred as sodium
o it ● When you scale up to find the number
number o moles in the ull volume
volume o
e hydroxide is particularly
r solution in the volumetric flask, use this equation:
c hazardous to the eyes.
s i
d
r
e number o moles in ull volume ● Avoid
Avoid skin
skin conta
contact
ct with
with the
the
h
s il acid, alkali and indicator.
ull volume × number o moles in aliquot volume
u
b
= ______________________________________________ ● Always
Always use a pipet
pipette
te filler;
filler;
p
t
aliquot volume in which you know the number o moles
a never use your mouth to suck
e the liquid up.
g
n
a ● Take care
care when
when clampin
clamping g and
h
c
o t filling the burette that it does
t
c not crack or topple over.
e j Results (Use this space to record your results.)
b
u
s
t
n Rough Trial 1 Trial 2 Trial 3 Trial 4
e t
n
o
c Final burette reading/cm3
ll
a
,f
o Initial burette reading/cm3
o
r
p
d Titre/cm 3
e t
c
e
rr
o
c
Concordant
Concordant (Y/N)
n
U

13
 CORE PRACTICAL 3: SPECIFICATION
REFERENCE

FINDING THE CONCENTRATION

CONCENTRATION OF A SOLUTION OF HYDROCHLORIC ACID 8.21

Analysis of results
8 1 Calculate the mean titre using your two concordant results.
1
0
2
n
o
s
r
a
e
P
©
.t
r
a
p
n i
r
o
e l
o
h
w
n i
n 2 Calculat
Calculatee the number o moles o sodium hydroxide that were contained in your mean titre.
o it
u
b
rit
s i
d
r
o
n
o
ti
a l
u
c
ri
c
,
e l
a
s
e
r
r
o f
t
o
N
.
n
o it 3 Calculat
Calculatee the number o moles o hydrochl
hydrochloric cm 3 o
oric acid that were contained in the ull 250 cm
e
r
c diluted hydrochloric acid.
s i
d
r
e
h
s il
b
u
p
t
a
e
g
n
a
h
c
o t
t
c
e j
b
u
s
t
n
e t
n
o
c 4 Calculat
Calculatee the concentra
concentration
tion o the original solution o hydrochloric acid.
ll
a
,f
o
o
r
p
d
e t
c
e
rr
o
c
n
U

14
 CORE PRACTICAL 3: SPECIFICATION
REFERENCE

FINDING THE CONCENTRATION

CONCENTRATION OF A SOLUTION OF HYDROCHLORIC ACID 8.21

Questions
8 1 Write a chemical equation or the reaction o hydrochloric acid with sodium hydroxide.
1
0
2
n
o
s
r
a
e
P
©
.t
r
a 2 The pink colour seen at the end point ades because the excess sodium hydroxide
hydroxide reacts with carbon dioxide in
p
n i the air. This reaction produces sodium carbonate.
r
o a Write an equation or the reaction o sodium hydroxide with carbon dioxide.
e l
o
h
w
n i
n
o it
u
b
rit
s i b When sodium hydroxide solution is stored, it reacts with carbon dioxide in the air.
d
r
o i How will this change the concentra
concentration
tion o the sodium hydroxide solution?
n
o
ti
a l
u
c
ri
c
,
e l
a
s ii How will this affect the volume o sodium hydroxide solution required to reach the end point in the
e
r
r titration? Explain your answer.
o f
t
o
N
.
n
o it
e
r
c
s i
d
r
e
h
s il
b
u
p
t
a
e
g
n
a
h
c
o t
t
c
e j
b
u
s
t
n
e t
n
o
c
ll
a
,f 3 Explain why it is better to have a titre o around 25 cm 3 than a titre o around 10 cm3.
o
o
r
p
d
e t
c
e
rr
o
c
n
U

15
 CORE PRACTICAL 4: SPECIFICATION
REFERENCE
PREPARATION
PREPARATION OF A ST
STANDARD
ANDARD SOLUTION FROM A SOLID ACID AND ITS
I TS USE TO FIND
8.23
THE CONCENTRATION OF A SOLUTION OF SODIUM HYDROXIDE

Procedure
Objectives
8 1 Weigh an empty test tube. Scoop approximately 2.5 g o sulamic acid into
1 ● To make
make a solutio
solution
n o a known
known
0 the test tube.
2
n concentration o acid and use
o 2 Accurately reweigh the test tube and its contents.
s
r it to find the concentra
concentration
tion o
a cm3 o water in a beaker.
3 Dissolve the sulamic acid in approximately 100 cm
e a solution o sodium hydroxide
P
© 4 Transer the solution, including the washings, to a 250 cm 3 volumetric
.t Equipment
r flask and use distilled water to make up the solution to the mark.
a
p ● bure
burette,
tte, clam
clamp
p and
and stand
stand
n i 5 Prepare your apparatus or the titration. The burette will contain the acid
r ● sol
solid
id sul
sulami
amicc acid
acid
o and the conical flask will contain the sodium hydroxide solution.
e l
o 6 Pour a 25.0 cm3 aliquot o sodium hydroxide solution o unknown ● sodium
sodium hydro
hydroxide
xide solu
solution
tion o
h
w tion into the 250 cm3 conical flask.
concentration
concentra unknown concentration
n i
n 7 Use methyl orange as the indicator. ● methy
methyll oran
orange
ge indic
indicator
ator
o it
u 8 Titrate the contents o the flask against the sulamic acid solution you ● 250 cm3 conical flask
b
rit ● 25 cm3 volumetric pipette plus
s prepared. Burette readings should be to the nearest 0.05 cm3.
i
d saety filler
r 9 Conduct urther titrations until you have two concordant titres.
o
n 10 Record your results in the table below. ● 100 cm3 beaker or transer o
o
ti solutions
a l
u
c
ri Learning tips ● un
unnel
nel or
or filling
filling buret
burette
te
c
, ● 250 cm3 beaker
e l ● Indicators are very dilute
dilute weak acids.
acids. The
The more indicator
indicator you add,
add, the less
a
s
e accurate your titration result will be. ● 250 cm3 volumetric flask
r
r ● ma
mass
ss balan
balance
ce (2 d.p
d.p.)
.)
o f
● When conducting
conducting a titration,
titration, use distilled
distilled water to
to wash down
down the inside o
o
t
o the conical flask rom time to time.
N ! Safety
. ● When you scale up to find the number
number o moles in the ull volume
volume o
n
o it ● Wear
Wear eye
eye protect
protection.
ion. Gogg
Goggles
les
e
solution in the volumetric flask, use this equation:
r are preerred as sodium
c
s i hydroxide is particularly
d number o moles in ull volume
r hazardous to the eyes.
e
h ull volume × number o moles in aliquot volume
s il = ______________________________________________ ● Avoid
Avoid skin
skin con
contact
tact with
u
b aliquot volume in which you know the number o moles
p sulamic acid and sodium
t
a hydroxide.
e
g ● Take care
care when
when clampin
clamping g and
n
a
c
h filling the burette that it does
o t not crack or topple over.
t Results (Use this space to record your results.)
c
e j
b
u
s
t
Mass of sulfamic acid = g
n
e t Rough Trial 1 Trial 2 Trial 3 Trial 4
n
o
c
ll Final burette reading/cm3
a
,f
o
o
r
Initial burette reading/cm3
p
d
e t Titre/cm 3
c
e
rr
o
c Concordant
Concordant (Y/N)
n
U

16
 CORE PRACTICAL 4: SPECIFICATION
REFERENCE
PREPARATION
PREPARATION OF A ST
STANDARD
ANDARD SOLUTION FROM A SOLID ACID AND ITS
I TS USE TO FIND
8.23
THE CONCENTRATION OF A SOLUTION OF SODIUM HYDROXIDE

Analysis of results
8 1 Calculate the concentration o your sulamic acid solution. The Mr o sulamic acid is 97.1.
1
0
2
n
o
s
r
a
e
P
©
.t
r
a
p
n i
r
o
e l
o
h
w
n i
n
o it
u
rit
b 2 Calculate the mean titre using your concordant results.
s i
d
r
o
n
o
ti
a l
u
c
ri
c
,
e l
a
s
e
r
r
o f
t
o
N
.
n
o it
e
r
c 3 Calculat
Calculatee the number o moles o sulamic acid in your mean titre.
s i
d
r
e
h
s il
b
u
p
t
a
e
g
n
a
h
c
o t
t
c
e j
b
u
s
t
n
e t
n
o
c
4 Sulamic acid is a monoprotic acid. This means that one mole o sulamic acid will react exactly with
ll
a one mole o sodium hydroxide. Calculate the concentration o the sodium hydroxide solution used.
,f
o
o
r
p
d
e t
c
e
rr
o
c
n
U

17
 CORE PRACTICAL 4: SPECIFICATION
REFERENCE
PREPARATION
PREPARATION OF A ST
STANDARD
ANDARD SOLUTION FROM A SOLID ACID AND ITS
I TS USE TO FIND
8.23
THE CONCENTRATION OF A SOLUTION OF SODIUM HYDROXIDE

Questions
8 1 A 250 cm3 volumetric flask has an accuracy o ±0.6 cm 3. Calculate the percentage uncertainty
1
0 in the volume o the sulamic acid solution in the volumetric flask.
2
n
o
s
r
a
e
P
©
.t
r
a
p
n i
r
o
e l
o
h
w
n i
n
o it
u
b
rit 2 Each burette reading is accurate to ±0.05 cm 3. Calculate the percentage uncertainty in one o
s i
d your titres.
r
o
n
o
ti
a l
u
c
ri
c
,
e l
a
s
e
r
r
o f
t
o
N
.
n
o it
e
r
c
s i 3 Why should the pipette be rinsed with the sodium hydroxide
hydroxide solution afer it has been
d
r
e
washed with water?
h
s il
b
u
p
t
a
e
g
n
a
h
c
o t
t
c
e j
b 4 Why is there no need to dry the conical flask afer washing it out between trials?
u
s
t
n
e t
n
o
c
ll
a
,f
o
o
r
p
d
e t
c
e
rr
o 5 Identiy another indicator you could use in this titration, and state the colour change you
c
n would see at the end point.
U

18
 CORE PRACTICAL 5: SPECIFICATION
REFERENCE

INVESTIGATION OF THE RATES OF HYDROLYSIS OF SOME HALOGENOALKANES 10.11

Procedure Objectives
8 Part 1
1 ● To investig
investigate
ate the
the relativ
relativee
0
2 1 Set up a water bath by filling the 250 cm3 beaker up to the three-quarters
n rates o hydrolysis o
o
s
mark with water at around 50 °C. primary, secondary and
r
a 2 Take three test tubes and add 5 cm 3 o ethanol to each one.
e tertiary halogenoal
halogenoalkanes
kanes
P
© 3 Add our drops o 1-iodobutane to the first tube, our drops o and o chloro-, bromo- and
.t
r 1-bromobutane to the second tube and our drops o 1-chlorobutane to iodoalkanes
a
p
n i
the third tube. Label the tubes. Equipment
r
o 4 Loosely place a bung in each test tube and place the test tubes in the
e l
● 250 cm3 beaker
o water bath.
h ● 12 test
test tubes
tubes with
with bung
bungss
w 5 Take three clean test tubes and pour 5 cm 3 o silver nitrate solution into
n i ● 1-
1-ch
chlo
loro
robu
buta
tane
ne
n each one. Then place the test tubes in the water bath.
o it ● 1-
1-br
brom
omob
obut
utan
anee
u 6 When the halogenoal
halogenoalkane–ethanol
kane–ethanol solutions have reached the
b
rit temperature o the water bath, add one test tube o silver nitrate solution ● 1-
1-io
iodo
dobu
buta
tane
ne
s i
d to one o the halogenoalkane–ethanol solutions and replace the bung. ● 2-
2-br
brom
omob
obut
utan
anee
r
o At the same time, start the stop clock.
n ● 2-bro
2-bromo-2-
mo-2-methy
methylpro
lpropane
pane
o
ti 7 Measure the time taken or a precipitate to appear. As soon as the solution ● 0.05
0.05 mo dm–3 silver nitrate
moll dm
a l
u
c
becomes cloudy, stop the stop clock. solution
ri
c 8 Repeat steps 6 and 7 or the other two halogenoalkanes.
halogenoalkanes.
, ● 15 cm3 ethanol
e l
a Part 2 ● dro
droppi
pping
ng pip
pipett
ettes
es
s
e
r
r
o
9 Repeat Part 1 using 1-bromobutane, 2-bromobutane
2-bromobutane and 10 cm3 measuring cylinders
● two 10
f
o
t 2-bromo-2-methylpropane
2-bromo-2-methylpropane instead o the other halogenoa
halogenoalkanes.
lkanes. ● st
stop
op cl
cloc
ockk
N
. ● lab
labels
els or
or test
test tub
tubes
es
n Results (Use this space to record your results.)
o it
e ● kettle
r
c
s i
d ! Safety
r
e
h ● Wear eye
eye prot
protect
ection
ion..
s il
u
b ● Avoid
Avoid skin
skin conta
contact
ct with
with the
the
p reactants.
t
a
e ● There
There mus
mustt be no
no naked
naked
g
n
a flames in the vicinity as
h
c ethanol and halogenoalk
halogenoalkanes
anes
o t
c
t are highly flammable.
e j
b ● The labo
laborato
ratory
ry needs
needs to
to be
u
s well ventilated to prevent the
t
n
e t inhalation o umes.
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19
 CORE PRACTICAL 5: SPECIFICATION
REFERENCE

INVESTIGATION OF THE RATES OF HYDROLYSIS OF SOME HALOGENOALKANES 10.11

Learning tips
8 ● The hydrolysis
hydrolysis o halogenoalk
halogenoalkanes
anes is a nucleophilic
nucleophilic substitution
substitution reaction.
reaction.
1
0
2 ● In this investigation, the nucleophile
nucleophile is water
water..
n
o ● NaOH can be used instead
instead o water
water to hydrolyse
hydrolyse the halogenoalkanes
halogenoalkanes but then any
any excess NaOH
NaOH
s
r
a must be neutralised by HNO3 beore the AgNO3 is added. Otherwise a precipitate o Ag 2O will orm.
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.t Analysis of results
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a
p 1 Describe the pattern shown in your results or Part 1.
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.
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2 Describe the pattern shown in your results or Part 2.
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a
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o Questions
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d
1 Write an equation or the reaction o 1-bromobutane with water.
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2 In these reactions, a precipitate orms. Identiy the precipitate ormed when the halogenoalkane
is 1-iodobutane.

20
 CORE PRACTICAL 5: SPECIFICATION
REFERENCE

INVESTIGATION OF THE RATES OF HYDROLYSIS OF SOME HALOGENOALKANES 10.11

3 Explain why ethanol is used in these reactions.

8
1
0
2
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4 Explain why water is able to act as a nucleophile.
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u
b
rit
s i
d 5 Explain why water is used as the nucleophile rather than hydroxid
hydroxidee ions.
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ti
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,
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a
s
e
r
r 6 Draw skeletal ormulae or each o the halogenoa
halogenoalkanes
lkanes used in this investigation (there are five o them).
o f
t Classiy each halogenoalkane as primary, secondary or tertiary.
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21
 CORE PRACTICAL 6: SPECIFICATION
REFERENCE

CHLORINATION
CHLORINATION OF 2-METHYLPROP
2-METHYLPROPAN-2-OL
AN-2-OL WITH CONCENTRA
CONCENTRATED
TED HYDROCHLORIC ACID 10.14

Procedure Objectives
8 1 Pour 10 cm3 o 2-methylpropan-2-ol and 35 cm3 o concentrated
concentrated
1 ● To produce
produce and
and puriy
puriy a sample
sample
0 hydrochloric acid into a large conical flask. Very gently swirl the contents o
2
n o 2-chloro-2-methylpropa
2-chloro-2-methylpropanene
o the flask.
s
r
a 2 Place the bung in the mouth o the flask. Gently swirl again, then remove Equipment
e
P the bung to release the pressure. ● 250 cm3 conical flask with bung
©
.t 3 Continue swirling the mixture with the bung fitted, and then releasing
r ● 100 cm3 (or larger) separating
a
p the pressure, or around 20 minutes. You should see two layers in the unnel with bung
n i
r flask. The upper layer is the crude product. ● 250 cm3 beaker or liquid run
o
e l 4 Add approximately 6 g o powdered anhydrous calcium chloride to the off rom separating unnel
o
h flask and swirl until it has dissolved. This will ensure that any unreacted
w ● filter
filter unnel
unnel to
to fit separ
separating
ating
n i alcohol is in the lower aqueous layer.
n
unnel
o it 5 Transer the reaction mixture to a separating unnel. Allow the mixture to
u
● apparatu
apparatuss or
or distil
distillatio
lation
n
b settle into the two layers. Run off and discard the lower layer. Retain the
rit
3
with 50 cm pear-shaped (or
s i
upper organic layer in the separating unnel.
d round-bottomed)
round-bottom ed) flask and
r 6 Add approximately 20 cm3 o sodium hydrogencarbonate solution to the thermometer able to read up
o
n separating unnel. Swirl the unnel. The production o carbon dioxide will to 100 °C
o
ti cause the pressure to increase; remove the bung at requent intervals to
a l
u ● 25 cm3 and 100 cm
cm3 measuring
c
ri
release this pressure. Run off and discard the lower aqueous layer.
c cylinders
, 7 Repeat the washing with sodium hydrogencarbonate solution, shake
e l ● 2-m
2-meth
ethyl
ylpro
propan
pan-2-
-2-ol
ol
a the separating unnel, and release the carbon dioxide gas produced, at
s
e
r requent intervals. ● 0.1
0.1 mo dm–3 sodium
mol dm
r
o f 8 Run off and discard the lower layer. Ensure none o the aqueous layer hydrogencarbonate solution
t
o remains in the tap. ● 6 g powde
powdered
red anhy
anhydro
drous
us
N
.
n 9 Run off the organic layer into a small conical flask. Add a ull spatula calcium chloride
o it
e
r
o anhydrous sodium sulate. Place the bung in the flask and swirl the ● anhy
anhydrou
drouss sodium
sodium sul
sulate
ate
c
s i contents to mix. Leave the mixture until the liquid looks completely clear, ● smal
smalll conical
conical flas
flasks
ks with
with bungs
bungs
d
r swirling occasionally.
e
h
● sa
samp
mple
le tu
tube
be
s il 10 Decant the organic liquid into a 50 cm3 pear-shaped (or round-bottomed)
b ● 0.05
0.05 mo dm–3 silver nitrate
moll dm
u flask.
p solution
t 11 Set up the flask or distillation.
a
e dilutee (0.5 mol dm–3) sodium
● dilut
g 12 Collect the raction boiling between 50 °C and 52 °C.
n
a
hydroxide solution
h 13 Place your pure product in a labelled sample tube.
c ● dilutee (0.1 mol dm–3) nitric acid
dilut
o t 14 Carry out the test described in the ‘Analysis’ section o this practical.
c
t ● 70 cm3 concentrated
e j
b Learning tips hydrochloric acid
u
s ● te
test
st tu
tube
bess
t ● The OH group in an alcohol
alcohol can
can be replaced
replaced by a halogen.
halogen. As well as the
n
e t ● sp
spaatu
tullas
n method used here to chlorinate an alcohol, PCl 5 can be used to make a
o
c
ll
chloroalkane. HBr (which is made in situ) can be used to make a bromoalkane. ● 5 cm3 ethanol
a
,f
Red phosphorus with iodine can be used to make an iodoalkane. ● Bu
Buns
nsen
en bu
burn
rner
er
o
o
r
● You can
can check the purity
purity o a substance
substance by measuring
measuring its boiling
boiling temperature.
temperature. ● bea
beake
kerr or wa
wate
terr bath
bath
p
d
e t ! Safety
c
e
rr
o
● This procedure
procedure requires
requires the use oo a working ume cupboard.
cupboard.
c
n ● Wear eye protection.
protection. Goggles are
are preerred.
preerred.
U
● Avoid skin contact with the reactants and products.
products. Wear
Wear gloves.
● Avoid
Avoid inhalin
inhaling
g vapour
vapours.
s.
● The product
product o the distillation
distillation process
process is flammable.
● The umes rom the concentrated
concentrated hydrochloric
hydrochloric acid are toxic and corrosive
corrosive and must not be inhaled, especially
especially
by anyone with a respiratory problem.
22
 CORE PRACTICAL 6: SPECIFICATION
REFERENCE

CHLORINATION
CHLORINATION OF 2-METHYLPROP
2-METHYLPROPAN-2-OL
AN-2-OL WITH CONCENTRA
CONCENTRATED
TED HYDROCHLORIC ACID 10.14

Results (Use this space to record your results.)

8
1
0
2
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Analysis of results
c
o t Perorm the ollowing test on the distillate.
t
c 1 Place a ew drops o the distillate in a test tube.
e j
b
u
s
1 Add 5 cm3 o ethanol and 1 cm3 o aqueous sodium hydroxide to the test tube.
t
n 3 Warm the mixture in a water bath.
e t
n
o 4 Add excess nitric acid to the mixture ollowed by a ew drops o silver nitrate solution.
c
ll
a Describe what you see.
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23
 CORE PRACTICAL 6: SPECIFICATION
REFERENCE

CHLORINATION
CHLORINATION OF 2-METHYLPROP
2-METHYLPROPAN-2-OL
AN-2-OL WITH CONCENTRA
CONCENTRATED
TED HYDROCHLORIC ACID 10.14

Questions
8 1 Write an equation or the reaction o 2-methylpropan-2-ol with concentrated hydrochloric acid.
1
0
2
n
o
s
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a 2 What is removed rom the crude product when it is shaken with sodium hydrogencarbonate
hydrogencarbonate solution?
p
n i Write an equation or any reaction that occurs.
r
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o
h
w
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n
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u
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rit
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d
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o
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o
ti
3 2-methylpropan-2-ol has a boiling temperature o 82 °C and is soluble in water.
a l
u 2-chloro-2-methylpropane has a boiling temperature o 51 °C and is insoluble in water.
c
ri
c
Explain these differences.
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24