Edexcel IAL Chemistry Lab Book

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Lab Book
M01-iASAL_CHEM_LAB_44716_001-076.indd 1
AS/A LEVEL
CHEMISTRY
PEARSON EDEXCEL INTERNATIONAL
08/06/2018 11:44
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A note from the publishers:

While the Publishers have made every attempt to ensure that advice on the
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M01-iASAL_CHEM_LAB_44716_001-076.indd 2 08/06/2018 11:44

CONTENTS
INTRODUCTION2
CORE PRACTICALS OVERVIEW 3

PAPER 3 PRACTICAL SKILLS 4
PAPER 6 PRACTICAL SKILLS 5
1 MEASUREMENT OF THE MOLAR VOLUME OF A GAS 6
2 DETERMINATION OF THE ENTHALPY CHANGE OF A REACTION USING HESS’S LAW 9
3 FINDING THE CONCENTRATION OF A SOLUTION OF HYDROCHLORIC ACID 13
4 PREPARATION OF A STANDARD SOLUTION FROM A SOLID ACID AND ITS USE TO FIND
THE CONCENTRATION OF A SOLUTION OF SODIUM HYDROXIDE 16
5 INVESTIGATION OF THE RATES OF HYDROLYSIS OF SOME HALOGENOALKANES 19
6 CHLORINATION OF 2-METHYLPROPAN-2-OL WITH CONCENTRATED HYDROCHLORIC
ACID22
7 OXIDATION OF PROPAN-1-OL TO PRODUCE PROPANAL AND PROPANOIC ACID 25
8 ANALYSIS OF SOME INORGANIC AND ORGANIC UNKNOWNS 1 31
9A FOLLOWING THE RATE OF THE IODINE–PROPANONE REACTION BY A TITRIMETRIC
METHOD34
9B INVESTIGATING A ‘CLOCK REACTION’ (HARCOURT–ESSON, IODINE CLOCK) 37
10 FINDING THE ACTIVATION ENERGY OF A REACTION 42
11 FINDING THE Ka VALUE FOR A WEAK ACID 46
12 INVESTIGATING SOME ELECTROCHEMICAL CELLS 49
13A REDOX TITRATIONS WITH IRON(II) IONS AND POTASSIUM MANGANATE(VII) 52
13B REDOX TITRATIONS WITH SODIUM THIOSULFATE AND IODINE 55
14 PREPARATION OF A TRANSITION METAL COMPLEX 58
15 ANALYSIS OF SOME INORGANIC AND ORGANIC UNKNOWNS 2 61
16 PREPARATION OF ASPIRIN 67
ANSWERS70
MATHS SKILLS 73

INTRODUCTION
Practical work is central to the study of chemistry. The International Advanced Subsidiary/Advanced Level (IAS/IAL)
specification includes 16 core practical activities that link theoretical knowledge and understanding to practical
scenarios. By completing the core practical activities, you will learn to:
•• follow and interpret experimental instructions, covering a range of laboratory exercises throughout the course,
with minimal help from your teacher
•• manipulate apparatus, use chemicals, carry out all common laboratory procedures and use data logging (where
appropriate)
•• work sensibly and safely in the laboratory, paying due regard to health and safety requirements
•• gain accurate and consistent results in quantitative exercises, and make the most of the expected observations in
qualitative exercises.
By the end of this course, you should be able to use a variety of apparatus and techniques to:
•• design and carry out both the core practical activities and your own investigations
•• collect data that can be analysed
•• use data to draw valid conclusions.
Your knowledge and understanding of practical skills and activities will be assessed in all examination papers.
•• Papers 1 and 2 (IAS), and 4 and 5 (IAL) will include questions based on practical activities, including novel scenarios.
•• Papers 3 (IAS) and 6 (IAL) will test your ability to plan practical work, including risk management and selection of
apparatus.
Assessment for the Practical Skills Papers 3 and 6 will focus on four main areas:
•• independent thinking
•• use and application of scientific methods and practices
•• numeracy and the application of mathematical concepts
•• use of apparatus and equipment.
The ways in which you can demonstrate these practical skills are outlined in the tables on pages 4 and 5. You may
wish to tick off each element as you gain confidence.
You will find answers and maths skills required for the practicals in the back of the book.

CORE PRACTICALS OVERVIEW
UNIT 1 (IAS): FORMULAE, EQUATIONS AND AMOUNT OF SUBSTANCE

1 Measurement of the molar volume of a gas
UNIT 2 (IAS): ENERGETICS

2 Determination of the enthalpy change of a reaction using Hess’s Law
UNIT 2 (IAS): REDOX CHEMISTRY AND GROUPS 1, 2 AND 7

3 Finding the concentration of a solution of hydrochloric acid
4 Preparation of a standard solution from a solid acid and its use to find the concentration
of a solution of sodium hydroxide
UNIT 2 (IAS): ORGANIC CHEMISTRY: ALCOHOLS, HALOGENOALKANES AND SPECTRA

5 Investigation of the rates of hydrolysis of some halogenoalkanes
6 Chlorination of 2-methylpropan-2-ol with concentrated hydrochloric acid
7 Oxidation of propan-1-ol to produce propanal and propanoic acid
8 Analysis of some inorganic and organic unknowns 1
UNIT 4 (IAL): KINETICS

9a Following the rate of the iodine–propanone reaction by a titrimetric method
9b Investigating a ‘clock reaction’ (Harcourt–Esson, iodine clock)
10 Finding the activation energy of a reaction
UNIT 4 (IAL): ACID–BASE EQUILIBRIA

11 Finding the Ka value for a weak acid
UNIT 5 (IAL): REDOX EQUILIBRIA

12 Investigating some electrochemical cells
13a Redox titrations with iron(II) ions and potassium manganate(VII)
13b Redox titrations with sodium thiosulfate and iodine
UNIT 5 (IAL): TRANSITION METALS AND THEIR CHEMISTRY

14 Preparation of a transition metal complex
UNIT 5 (IAL): ORGANIC NITROGEN COMPOUNDS: AMINES, AMIDES, AMINO ACIDS AND PROTEINS
15 Analysis of some inorganic and organic unknowns 2
UNIT 5 (IAL): ORGANIC SYNTHESIS

16 Preparation of aspirin

PAPER 3 PRACTICAL SKILLS
Practical skills Core Practical

Independent thinking in a practical context 1 2 3 4 5 6 7 8
Solve problems set in a practical context
Apply scientific knowledge to practical contexts
Use and application of scientific methods and

1 2 3 4 5 6 7 8
practices
Identify and state how to control variables to
improve experimental validity
Present data in appropriate ways
Evaluate results and draw conclusions
Appreciate measurement uncertainties and errors
Comment on the method for an experiment
Numeracy and the application of mathematical

1 2 3 4 5 6 7 8
concepts in a practical context
Plot and interpret graphs
Process and analyse data using appropriate

mathematical skills
Use appropriate numbers of significant figures
based on the experimental data
Consider the accuracy and precision of data
Use of apparatus and equipment 1 2 3 4 5 6 7 8

Recognise a range of laboratory apparatus and
select appropriate apparatus for a particular
scenario
Understand how to use a range of apparatus and
techniques appropriate to the knowledge and
understanding included in the specification
Consider the range and resolution of apparatus
Identify health and safety issues and discuss how

these may be dealt with

PAPER 6 PRACTICAL SKILLS
Practical skills Core Practical

Independent thinking in a practical context 9a 9b 10 11 12 13a 13b 14 15 16
Solve problems set in a practical context
Apply scientific knowledge to practical contexts
Use and application of scientific methods and

9a 9b 10 11 12 13a 13b 14 15 16
practices
Identify and state how to control variables to
improve experimental validity
Present data in appropriate ways
Evaluate results and draw conclusions
Appreciate measurement uncertainties and errors
Comment on the method for an experiment
Numeracy and the application of mathematical

9a 9b 10 11 12 13a 13b 14 15 16
concepts in a practical context
Plot and interpret graphs
Process and analyse data using appropriate

mathematical skills
Use appropriate numbers of significant figures
based on the experimental data
Consider the accuracy and precision of data
Use of apparatus and equipment 9a 9b 10 11 12 13a 13b 14 15 16

Recognise a range of laboratory apparatus and
select appropriate apparatus for a particular
scenario
Understand how to use a range of apparatus and
techniques appropriate to the knowledge and
understanding included in the specification
Consider the range and resolution of apparatus
Identify health and safety issues and discuss how

these may be dealt with

CORE PRACTICAL 1: SPECIFICATION
REFERENCE
MEASUREMENT OF THE MOLAR VOLUME OF A GAS 1.11
Procedure
Objectives
1 Set up the apparatus to capture and measure gas evolved from a reaction
in the boiling tube. ●● To find the volume of one mole

of carbon dioxide gas
2 Place 30 cm3 of 1 mol dm−3 ethanoic acid in the boiling tube.
3 Place approximately 0.05 g of calcium carbonate in a test tube. Weigh the Equipment
test tube and its contents accurately. ●● boiling tube
●● stand and clamp
4 Remove the bung from the boiling tube and tip the calcium carbonate into
●● bung fitted with delivery tube
the boiling tube. Quickly replace the bung in the boiling tube.
to fit boiling tube
5 Once the reaction is over, measure the volume of gas produced. ●● water bath for gas collection
6 Reweigh the test tube that contained the calcium carbonate. ●● 100 cm3 measuring cylinder
7 Repeat the experiment six more times, increasing the mass of calcium ●● 50 cm3 measuring cylinder
carbonate by about 0.05 g each time. Do not exceed 0.40 g of calcium ●● test tube
carbonate. ●● mass balance (2 d.p.)
●● 1 mol dm−3 ethanoic acid
Learning tips ●● powdered calcium carbonate
●● Ensure that points plotted on a graph take up more than half the available
space on each scale. Axes must occupy at least half of the space on the
! Safety
graph paper. ●● Wear eye protection.
●● Keep scales simple: one large square as 5 or 10 or 20 is ideal. A scale where ●● Remove the bung if the
one large square represents 3 or 7 units (or similar) is very difficult to plot delivery tube gets blocked,
on, and this often leads to errors. clear the blockage and repeat
the procedure from the start.
●● Always consider whether the graph line should go through the origin.
●● Avoid skin contact with the
●● Straight lines should be drawn with the aid of a ruler long enough to cover ethanoic acid, especially if the
the full length of the line. skin is broken or sensitive.
Results (Use this space to record your results.)

REFERENCE
Analysis of results
1 Plot a graph of mass of calcium carbonate (on the x-axis) against volume of carbon dioxide
collected (on the y-axis). Draw a straight line of best fit – this line must pass through the
origin.
2 Use your graph to find the volume of carbon dioxide that would be made from 0.25 g of
calcium carbonate.
3 In this reaction, one mole of calcium carbonate makes one mole of carbon dioxide. Calculate
the number of moles of calcium carbonate in 0.25 g and hence calculate the volume of one
mole of carbon dioxide gas in dm3.

REFERENCE
Questions
1 Write a chemical equation for the reaction between ethanoic acid, CH3COOH, and calcium carbonate.
2 Why is it more accurate to find the mass of the calcium carbonate used by weighing the test tube containing the
calcium carbonate and then reweighing the test tube after the calcium carbonate has been tipped out, rather than
by weighing the empty test tube at the start?
3 Identify the major source of error caused by the procedure used here.
4 What change to the procedure/apparatus could you make to eradicate this error?
5 Carry out two calculations to show that the ethanoic acid was in excess in all experimental runs.

REFERENCE
DETERMINATION OF THE ENTHALPY CHANGE OF A REACTION USING HESS’S LAW 6.7
Procedure Objectives
1 Place approximately 3 g of solid potassium carbonate in a test tube.
●● To calculate the molar

Accurately weigh the test tube and its contents.
enthalpy change for two
2 Use a burette to dispense 30 cm3 of 2 mol dm–3 hydrochloric acid into a reactions and use Hess’s Law
polystyrene cup, which is supported in a beaker. to determine the enthalpy
3 Measure the temperature of the acid. change for the reactions
4 Gradually add potassium carbonate to the acid, stirring all the time and Equipment
monitoring the temperature of the acid.
●● two test tubes
5 Reweigh the empty test tube.
●● 2 mol dm–3 dilute hydrochloric
6 Repeat steps 1–5 using approximately 3.5 g of potassium hydrogencarbonate acid
instead of the potassium carbonate. This time, record the lowest temperature
●● solid potassium carbonate
reached.
●● solid potassium
Results (Use this space to record your results.) hydrogencarbonate
●● thermometer able to read up
Mass of test tube with potassium carbonate/g to 50 °C or more
●● polystyrene cup
Mass of test tube after emptying out potassium carbonate/g
●● 250 cm3 or 400 cm3 beaker
Mass of potassium carbonate used/g ●● burette, clamp and stand
Start temperature/°C ●● stirring rod
●● mass balance (2 d.p.)
Highest temperature/°C ●● spatula
Temperature change/°C ! Safety
●● Wear eye protection.
Mass of test tube with potassium hydrogencarbonate/g ●● Avoid skin contact with the
reactants and products.
Mass of test tube after emptying out potassium hydrogencarbonate/g
Mass of potassium hydrogencarbonate used/g
Start temperature/°C
Lowest temperature/°C
Temperature change/°C

REFERENCE
Learning tips
●● You can assume that the heat capacity of the final solution is the same as the heat capacity of
water. The volume of water produced in the reaction is so small it can be ignored.
●● For exothermic reactions, the enthalpy change, △H, is negative.
●● Be careful to use equals signs correctly. It is very easy to end up stating that a negative
number equals a positive number.
Analysis of results
1 The equations for the reactions occurring are:
reaction 1: K2CO3(s) + 2HCl(aq) → 2KCl(aq) + CO2(g) + H2O(l)
reaction 2: KHCO3(s) + HCl(aq) → KCl(aq) + CO2(g) + H2O(l)
Calculate the energy change for each reaction in J. (The specific heat capacity of water is
4.2 J g–1 °C–1.)
2 Calculate the enthalpy change, △H, for each reaction in kJ mol–1.

Assume that the hydrochloric acid is in excess.
3 Use your results to calculate the enthalpy change for the thermal decomposition of
potassium hydrogencarbonate:
reaction 3: 2KHCO3(s) → K2CO3(s) + CO2(g) + H2O(l)
10

REFERENCE
Questions
1 Why is it not possible to measure the enthalpy change for the decomposition of potassium
hydrogencarbonate directly?
2 Show that the hydrochloric acid is in excess in both reactions.
11

REFERENCE
3 Draw an energy level diagram for each reaction: 1, 2 and 3.

4 Explain why the reactions are conducted in a polystyrene cup rather than a glass beaker.
12

REFERENCE
FINDING THE CONCENTRATION OF A SOLUTION OF HYDROCHLORIC ACID 8.21
1 Wash out the 250 cm3 volumetric flask with distilled water.
●● To find the concentration of a

2 Use the pipette to transfer 25.0 cm3 of the hydrochloric acid solution into solution of hydrochloric acid
the volumetric flask. Use distilled water to make the solution up to the
mark. Equipment
3 Prepare your apparatus for the titration. The burette should contain the ●● burette, clamp and stand
sodium hydroxide solution (previously standardised) and the conical flask ●● sodium hydroxide solution
should contain the dilute hydrochloric acid solution. (approximately 0.08 dm3,
4 Pour a 25.0 cm3 aliquot of the diluted hydrochloric acid into the conical previously standardised)
flask. Use phenolphthalein as the indicator. ●● bench hydrochloric acid
5 Titrate the contents of the flask against the sodium hydroxide solution. (approximately 1 mol dm–3)
Record all burette readings to the nearest 0.05 cm3. ●● phenolphthalein
6 The end point of this titration is indicated by the contents of the flask ●● 250 cm3 conical flask
becoming pale pink. Continued swirling will cause the pink colour to fade ●● 25 cm3 volumetric pipette plus
and disappear. If the pink colour persists for 5 seconds or more, the end safety filler
point has been reached.
●● 100 cm3 beakers for transfer of
7 Conduct further titrations until you have two concordant titres. solutions
8 Ask your teacher or a technician to check one of your burette readings. ●● funnel for filling burette
9 Record your results in the table below. ●● 250 cm3 beaker
●● 250 cm3 volumetric flask
Learning tips
! Safety
●● Do not include your rough titration when calculating your mean.
●● Wear eye protection. Goggles
●● Give all burette readings to the nearest 0.05 cm3.
are preferred as sodium
●● When you scale up to find the number of moles in the full volume of hydroxide is particularly
solution in the volumetric flask, use this equation: hazardous to the eyes.
number of moles in full volume ●● Avoid skin contact with the
acid, alkali and indicator.
full volume × number of moles in aliquot volume
= ______________________________________________
    
        ●● Always use a pipette filler;
aliquot volume in which you know the number of moles
never use your mouth to suck
the liquid up.
●● Take care when clamping and
filling the burette that it does
not crack or topple over.
Rough Trial 1 Trial 2 Trial 3 Trial 4
Final burette reading/cm3
Initial burette reading/cm3
Titre/cm3
Concordant (Y/N)
13

REFERENCE
Analysis of results
1 Calculate the mean titre using your two concordant results.
2 Calculate the number of moles of sodium hydroxide that were contained in your mean titre.
3 Calculate the number of moles of hydrochloric acid that were contained in the full 250 cm3 of
diluted hydrochloric acid.
4 Calculate the concentration of the original solution of hydrochloric acid.
14

REFERENCE
Questions
1 Write a chemical equation for the reaction of hydrochloric acid with sodium hydroxide.
2 The pink colour seen at the end point fades because the excess sodium hydroxide reacts with carbon dioxide in
the air. This reaction produces sodium carbonate.
a Write an equation for the reaction of sodium hydroxide with carbon dioxide.
b When sodium hydroxide solution is stored, it reacts with carbon dioxide in the air.
i How will this change the concentration of the sodium hydroxide solution?
ii How will this affect the volume of sodium hydroxide solution required to reach the end point in the
titration? Explain your answer.
3 Explain why it is better to have a titre of around 25 cm3 than a titre of around 10 cm3.
15

REFERENCE
PREPARATION OF A STANDARD SOLUTION FROM A SOLID ACID AND ITS USE TO FIND
8.23
THE CONCENTRATION OF A SOLUTION OF SODIUM HYDROXIDE
Procedure
Objectives
1 Weigh an empty test tube. Scoop approximately 2.5 g of sulfamic acid into
the test tube. ●● To make a solution of a known

concentration of acid and use
2 Accurately reweigh the test tube and its contents.
it to find the concentration of
3 Dissolve the sulfamic acid in approximately 100 cm3 of water in a beaker. a solution of sodium hydroxide
4 Transfer the solution, including the washings, to a 250 cm3 volumetric
Equipment
flask and use distilled water to make up the solution to the mark.
●● burette, clamp and stand
5 Prepare your apparatus for the titration. The burette will contain the acid
and the conical flask will contain the sodium hydroxide solution. ●● solid sulfamic acid
6 Pour a 25.0 cm3 aliquot of sodium hydroxide solution of unknown ●● sodium hydroxide solution of
concentration into the 250 cm3 conical flask. unknown concentration
7 Use methyl orange as the indicator. ●● methyl orange indicator
8 Titrate the contents of the flask against the sulfamic acid solution you ●● 250 cm3 conical flask
prepared. Burette readings should be to the nearest 0.05 cm3. ●● 25 cm3 volumetric pipette plus
9 Conduct further titrations until you have two concordant titres. safety filler
10 Record your results in the table below. ●● 100 cm3 beaker for transfer of
solutions
Learning tips ●● funnel for filling burette
●● Indicators are very dilute weak acids. The more indicator you add, the less ●● 250 cm3 beaker
accurate your titration result will be. ●● 250 cm3 volumetric flask
●● When conducting a titration, use distilled water to wash down the inside of ●● mass balance (2 d.p.)
the conical flask from time to time.
! Safety
●● When you scale up to find the number of moles in the full volume of
●● Wear eye protection. Goggles
solution in the volumetric flask, use this equation:
are preferred as sodium
number of moles in full volume hydroxide is particularly
hazardous to the eyes.
full volume × number of moles in aliquot volume
= ______________________________________________
    
        ●● Avoid skin contact with
aliquot volume in which you know the number of moles
sulfamic acid and sodium
hydroxide.
●● Take care when clamping and
filling the burette that it does
not crack or topple over.
Mass of sulfamic acid = g

Rough Trial 1 Trial 2 Trial 3 Trial 4
Final burette reading/cm3
Initial burette reading/cm3
Titre/cm3
Concordant (Y/N)
16

REFERENCE
8.23
Analysis of results
1 Calculate the concentration of your sulfamic acid solution. The Mr of sulfamic acid is 97.1.
2 Calculate the mean titre using your concordant results.
3 Calculate the number of moles of sulfamic acid in your mean titre.
4 Sulfamic acid is a monoprotic acid. This means that one mole of sulfamic acid will react exactly with
one mole of sodium hydroxide. Calculate the concentration of the sodium hydroxide solution used.
17

REFERENCE
8.23
Questions
1 A 250 cm3 volumetric flask has an accuracy of ±0.6 cm3. Calculate the percentage uncertainty
in the volume of the sulfamic acid solution in the volumetric flask.
2 Each burette reading is accurate to ±0.05 cm3. Calculate the percentage uncertainty in one of
your titres.
3 Why should the pipette be rinsed with the sodium hydroxide solution after it has been
washed with water?
4 Why is there no need to dry the conical flask after washing it out between trials?
5 Identify another indicator you could use in this titration, and state the colour change you
would see at the end point.
18

REFERENCE
INVESTIGATION OF THE RATES OF HYDROLYSIS OF SOME HALOGENOALKANES 10.11
Part 1
●● To investigate the relative

1 Set up a water bath by filling the 250 cm3 beaker up to the three-quarters rates of hydrolysis of
mark with water at around 50 °C. primary, secondary and
2 Take three test tubes and add 5 cm3 of ethanol to each one. tertiary halogenoalkanes
3 Add four drops of 1-iodobutane to the first tube, four drops of and of chloro-, bromo- and
1-bromobutane to the second tube and four drops of 1-chlorobutane to iodoalkanes
the third tube. Label the tubes. Equipment
4 Loosely place a bung in each test tube and place the test tubes in the ●● 250 cm3 beaker
water bath.
●● 12 test tubes with bungs
5 Take three clean test tubes and pour 5 cm3 of silver nitrate solution into
●● 1-chlorobutane
each one. Then place the test tubes in the water bath.
●● 1-bromobutane
6 When the halogenoalkane–ethanol solutions have reached the
temperature of the water bath, add one test tube of silver nitrate solution ●● 1-iodobutane
to one of the halogenoalkane–ethanol solutions and replace the bung. ●● 2-bromobutane
At the same time, start the stop clock. ●● 2-bromo-2-methylpropane
7 Measure the time taken for a precipitate to appear. As soon as the solution ●● 0.05 mol dm–3 silver nitrate
becomes cloudy, stop the stop clock. solution
8 Repeat steps 6 and 7 for the other two halogenoalkanes. ●● 15 cm3 ethanol
Part 2 ●● dropping pipettes
9 Repeat Part 1 using 1-bromobutane, 2-bromobutane and ●● two 10 cm3 measuring cylinders
2-bromo-2-methylpropane instead of the other halogenoalkanes. ●● stop clock
●● labels for test tubes
●● kettle
! Safety
●● Wear eye protection.
●● Avoid skin contact with the
reactants.
●● There must be no naked
flames in the vicinity as
ethanol and halogenoalkanes
are highly flammable.
●● The laboratory needs to be
well ventilated to prevent the
inhalation of fumes.
19

REFERENCE
Learning tips
●● The hydrolysis of halogenoalkanes is a nucleophilic substitution reaction.
●● In this investigation, the nucleophile is water.

●● NaOH can be used instead of water to hydrolyse the halogenoalkanes but then any excess NaOH
must be neutralised by HNO3 before the AgNO3 is added. Otherwise a precipitate of Ag2O will form.
Analysis of results
1 Describe the pattern shown in your results for Part 1.
2 Describe the pattern shown in your results for Part 2.
Questions
1 Write an equation for the reaction of 1-bromobutane with water.
2 In these reactions, a precipitate forms. Identify the precipitate formed when the halogenoalkane
is 1-iodobutane.
20

REFERENCE
3 Explain why ethanol is used in these reactions.

4 Explain why water is able to act as a nucleophile.
5 Explain why water is used as the nucleophile rather than hydroxide ions.
6 Draw skeletal formulae for each of the halogenoalkanes used in this investigation (there are five of them).
Classify each halogenoalkane as primary, secondary or tertiary.
21

REFERENCE
CHLORINATION OF 2-METHYLPROPAN-2-OL WITH CONCENTRATED HYDROCHLORIC ACID 10.14
1 Pour 10 cm3 of 2-methylpropan-2-ol and 35 cm3 of concentrated
●● To produce and purify a sample

hydrochloric acid into a large conical flask. Very gently swirl the contents of
of 2-chloro-2-methylpropane
the flask.
2 Place the bung in the mouth of the flask. Gently swirl again, then remove Equipment
the bung to release the pressure. ●● 250 cm3 conical flask with bung
3 Continue swirling the mixture with the bung fitted, and then releasing ●● 100 cm3 (or larger) separating
the pressure, for around 20 minutes. You should see two layers in the funnel with bung
flask. The upper layer is the crude product. ●● 250 cm3 beaker for liquid run
4 Add approximately 6 g of powdered anhydrous calcium chloride to the off from separating funnel
flask and swirl until it has dissolved. This will ensure that any unreacted
●● filter funnel to fit separating
alcohol is in the lower aqueous layer.
funnel
5 Transfer the reaction mixture to a separating funnel. Allow the mixture to
●● apparatus for distillation
settle into the two layers. Run off and discard the lower layer. Retain the
with 50 cm3 pear-shaped (or
upper organic layer in the separating funnel.
round-bottomed) flask and
6 Add approximately 20 cm3 of sodium hydrogencarbonate solution to the thermometer able to read up
separating funnel. Swirl the funnel. The production of carbon dioxide will to 100 °C
cause the pressure to increase; remove the bung at frequent intervals to
●● 25 cm3 and 100 cm3 measuring
release this pressure. Run off and discard the lower aqueous layer.
cylinders
7 Repeat the washing with sodium hydrogencarbonate solution, shake
the separating funnel, and release the carbon dioxide gas produced, at ●● 2-methylpropan-2-ol
frequent intervals. ●● 0.1 mol dm–3 sodium
8 Run off and discard the lower layer. Ensure none of the aqueous layer hydrogencarbonate solution
remains in the tap. ●● 6 g powdered anhydrous
9 Run off the organic layer into a small conical flask. Add a full spatula calcium chloride
of anhydrous sodium sulfate. Place the bung in the flask and swirl the ●● anhydrous sodium sulfate
contents to mix. Leave the mixture until the liquid looks completely clear, ●● small conical flasks with bungs
swirling occasionally.
●● sample tube
10 Decant the organic liquid into a 50 cm3 pear-shaped (or round-bottomed)
●● 0.05 mol dm–3 silver nitrate
flask.
solution
11 Set up the flask for distillation.
●● dilute (0.5 mol dm–3) sodium
12 Collect the fraction boiling between 50 °C and 52 °C.
hydroxide solution
13 Place your pure product in a labelled sample tube.
●● dilute (0.1 mol dm–3) nitric acid
14 Carry out the test described in the ‘Analysis’ section of this practical.
●● 70 cm3 concentrated
Learning tips hydrochloric acid
●● The OH group in an alcohol can be replaced by a halogen. As well as the ●● test tubes
method used here to chlorinate an alcohol, PCl5 can be used to make a ●● spatulas
chloroalkane. HBr (which is made in situ) can be used to make a bromoalkane. ●● 5 cm3 ethanol
Red phosphorus with iodine can be used to make an iodoalkane. ●● Bunsen burner
●● You can check the purity of a substance by measuring its boiling temperature. ●● beaker for water bath
! Safety
●● This procedure requires the use of a working fume cupboard.
●● Wear eye protection. Goggles are preferred.
●● Avoid skin contact with the reactants and products. Wear gloves.
●● Avoid inhaling vapours.
●● The product of the distillation process is flammable.
●● The fumes from the concentrated hydrochloric acid are toxic and corrosive and must not be inhaled, especially
by anyone with a respiratory problem.
22

REFERENCE

Analysis of results
Perform the following test on the distillate.
1 Place a few drops of the distillate in a test tube.
1 Add 5 cm3 of ethanol and 1 cm3 of aqueous sodium hydroxide to the test tube.
3 Warm the mixture in a water bath.
4 Add excess nitric acid to the mixture followed by a few drops of silver nitrate solution.
Describe what you see.
23

REFERENCE
Questions
1 Write an equation for the reaction of 2-methylpropan-2-ol with concentrated hydrochloric acid.
2 What is removed from the crude product when it is shaken with sodium hydrogencarbonate solution?
Write an equation for any reaction that occurs.
3 2-methylpropan-2-ol has a boiling temperature of 82 °C and is soluble in water.

2-chloro-2-methylpropane has a boiling temperature of 51 °C and is insoluble in water.
Explain these differences.
24

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What reaction occurs when 2-methylpropan-2-ol is treated with concentrated hydrochloric acid?

What reaction occurs when 2-methylpropan-2-ol is treated with concentrated hydrochloric acid?

What is removed from the crude product when it is shaken with sodium hydrogencarbonate solution and what reaction occurs?

What is removed from the crude product when it is shaken with sodium hydrogencarbonate solution and what reaction occurs?

Uncorrected proof, all content subject to change at publisher discretion. Not for resale, circulation or distribution in whole or in part.

Copies of official specifications for all Pearson Edexcel qualifications may be

Text © Pearson Education Limited 2018

First published 2018

British Library Cataloguing in Publication Data

Printed in Slovakia by Neografia

A note from the publishers:

M01-iASAL_CHEM_LAB_44716_001-076.indd 2 08/06/2018 11:44

CORE PRACTICALS OVERVIEW 3

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

1 Measurement of the molar volume of a gas

UNIT 2 (IAS): ENERGETICS

UNIT 2 (IAS): REDOX CHEMISTRY AND GROUPS 1, 2 AND 7

UNIT 2 (IAS): ORGANIC CHEMISTRY: ALCOHOLS, HALOGENOALKANES AND SPECTRA

6 Chlorination of 2-methylpropan-2-ol with concentrated hydrochloric acid

7 Oxidation of propan-1-ol to produce propanal and propanoic acid

8 Analysis of some inorganic and organic unknowns 1

UNIT 4 (IAL): KINETICS

9b Investigating a ‘clock reaction’ (Harcourt–Esson, iodine clock)

10 Finding the activation energy of a reaction

UNIT 4 (IAL): ACID–BASE EQUILIBRIA

UNIT 5 (IAL): REDOX EQUILIBRIA

13a Redox titrations with iron(II) ions and potassium manganate(VII)

13b Redox titrations with sodium thiosulfate and iodine

UNIT 5 (IAL): TRANSITION METALS AND THEIR CHEMISTRY

UNIT 5 (IAL): ORGANIC SYNTHESIS

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Practical skills Core Practical

Solve problems set in a practical context

Apply scientific knowledge to practical contexts

Use and application of scientific methods and

Evaluate results and draw conclusions

Appreciate measurement uncertainties and errors

Comment on the method for an experiment

Numeracy and the application of mathematical

Process and analyse data using appropriate

Use of apparatus and equipment 1 2 3 4 5 6 7 8

Identify health and safety issues and discuss how

M01-iASAL_CHEM_LAB_44716_001-076.indd 4 08/06/2018 11:44

Practical skills Core Practical

Solve problems set in a practical context

Apply scientific knowledge to practical contexts

Use and application of scientific methods and

Evaluate results and draw conclusions

Appreciate measurement uncertainties and errors

Comment on the method for an experiment

Numeracy and the application of mathematical

Process and analyse data using appropriate

Use of apparatus and equipment 9a 9b 10 11 12 13a 13b 14 15 16

Identify health and safety issues and discuss how

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in the boiling tube. ●● To find the volume of one mole

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CORE PRACTICALS OVERVIEW 3