Practical Guide EDEXCEL

This guide includes details about the core practicals for A-level chemistry. It also contains information about
other experiments that often occur in A-level examinations. You may be asked to describe these experiments in
details or be asked about reasons for doing individual steps.
You may be asked about other unfamiliar experiments but these will be using the skills and techniques that are
described in the following experiments.

Safety and hazards

Irritant - dilute acid and alkalis- wear googles Hazardous substances in low
Corrosive- stronger acids and alkalis wear goggles concentrations or amounts will
Flammable – keep away from naked flames not pose the same risks as the
Toxic – wear gloves- avoid skin contact- wash hands after use pure substance.
Oxidising- Keep away from flammable / easily oxidised materials

Measuring gas volumes

Make sure you don’t leave gaps in
Using a gas syringe your diagram where gas could
Gas syringes can be used for a variety of escape
experiments where the volume of a gas is
measured, possibly to work out moles of
gas or to follow reaction rates.

Potential errors in using a gas syringe

•gas escapes before bung inserted If drawing a gas syringe make sure
•syringe sticks you draw it with some
• some gases like carbon dioxide or sulphur dioxide are measurement markings on the
soluble in water so the true amount of gas is not barrel to show measurements can
measured. be made.

The volume of a gas depends on pressure Alternatively gas volumes can be

and temperature so when recording volume measured ‘over water’ with an up-turned
it is important to note down the measuring cylinder in a trough of water
temperature and pressure of the room.

Moles of gas can be calculated from gas

volume (and temperature and pressure)
using ideal gas equation PV = nRT or using
the molar gas volume (1mol gas =24dm3 at
room temperature and pressure

N Goalby chemrevise.org 1
Core Practical 1: Measure the molar volume of a gas

Detailed method
1. Measure 30 cm3 of 1 mol dm⁻3 ethanoic acid and transfer
to a conical flask.

Volume of CO2 in cm3

2. Attach conical flask to gas syringe or use collection over
water method (see previous page)
3. Measure the mass of a weighing bottle with approximately
0.05 g of calcium carbonate
4. Add the calcium carbonate to the conical flask- quickly
resealing the bung so no gas escapes
5. Measure the final total volume of gas
6. Reweigh the empty weighing bottle test tube from step 3
7. Repeat the experiment several more times, increasing the
mass of calcium carbonate by about 0.05 g each time.
Mass of CaCO3 in g

Analysis
From the graph read the volume of CO2 given off with 0.25 g CaCO3
Work out the moles of CaCO3 in 0.25g = 0.25/100.1 = 2.5 x 10-3
Assume the moles of CO2 = moles of CaCO3
Work out molar volume of CO2 = volume of CO2/ moles of CO2

Method for using a gas syringe to calculate the Mr of propanone

1. Extract 0.20 cm3 of propanone into a hypodermic syringe and then measure the mass of this syringe
2. using hand protection, remove a gas syringe from the oven and note the volume of air already in the
barrel – about 5 cm3.
3. inject the propanone through the self-seal cap into the barrel. The plunger will move straight away.
4. Put the gas syringe back into the oven.
5. Measure the mass of the empty hypodermic syringe immediately.
6. After a few minutes measure the volume of the gas in the gas syringe, record the temperature of the oven
shelf and the pressure of the room.

Example 1 : 0.150g of a volatile liquid was injected into a sealed gas syringe. The gas syringe was placed in an oven at
70oC at a pressure of 100kPa and a volume of 80cm3 was measured. Calculate the Mr of the volatile liquid (R = 8.31)

moles = PV/RT 100 kPa = 100 000 Pa

= 100 000 x 0.00008 / (8.31 x 343) 80 cm3 = 0.00008 m3
= 0.00281 mol

Mr = mass/moles
= 0.15 / 0.00281
= 53.4 g mol-1

N Goalby chemrevise.org 2
 This method could be used for measuring mass loss in various
Heating in a crucible
thermal decomposition reactions and also for mass gain when
reacting magnesium in oxygen.

The water of crystallisation in calcium sulfate crystals can be The lid improves the accuracy of the
removed as water vapour by heating as shown in the following experiment as it prevents loss of solid
equation. from the crucible but should be loose
CaSO4.xH2O(s) → CaSO4(s) + xH2O(g) fitting to allow gas to escape.
Method.
•Weigh an empty clean dry crucible and lid .
•Add 2g of hydrated calcium sulphate to the crucible and weigh
again
•Heat strongly with a Bunsen for a couple of minutes
•Allow to cool
•Weigh the crucible and contents again
•Heat crucible again and reweigh until you reach a constant mass (
do this to ensure reaction is complete).

Large amounts of hydrated calcium sulfate, such as 50g,

should not be used in this experiment as the decomposition is
likely to be incomplete. Small amounts of the solid , such as
0.100 g, should not be used in this
The crucible needs to be dry otherwise a wet crucible would experiment as the percentage
give an inaccurate result. It would cause mass loss to be too uncertainties in weighing will be too
large as the water would be lost when heating. high.

Example 2. 3.51 g of hydrated zinc sulfate were heated and 1.97 g of anhydrous zinc sulfate were obtained.
Use these data to calculate the value of the integer x in ZnSO4.xH2O
Calculate the mass of H2O = 3.51 – 1.97 = 1.54g
Calculate moles of Calculate moles of = 1.54
= 1.97 H2O
ZnSO4 161.5 18

= 0.0122 =0.085

Calculate ratio of mole of 0.0122 = 0.085

ZnSO4 to H2O =
0.0122 0.0122
=7
=1
X=7

N Goalby chemrevise.org 3
Core practical 2. Make up a volumetric solution and carry out a simple acid–base titration

Making a solution

• Weigh the sample bottle containing the required mass of solid Alternatively the known mass of solid
on a 2 dp balance in the weighing bottle could be
• Transfer to beaker transferred to beaker, washed and
• Reweigh empty sample bottle washings added to the beaker.
• Record the difference in mass

• Add 100cm3 of distilled water to the beaker. Use a glass rod to

stir to help dissolve the solid.

•Sometimes the substance may not dissolve well in cold water so

the beaker and its contents could be heated gently until all the
solid had dissolved.
Remember to fill so the bottom of the
• Pour solution into a 250cm3 graduated flask via a funnel. meniscus sits on the line on the neck of the
• Rinse beaker and funnel and add washings from the beaker flask. With dark liquids like potassium
and glass rod to the volumetric flask. manganate it can be difficult to see the
• make up to the mark with distilled water using a dropping meniscus.
pipette for last few drops.
• Invert flask several times to ensure uniform solution. Shake the volumetric flask thoroughly to
ensure a uniform concentration

A graduated flask has one mark on the neck which the level to
fill to get the accurate volume. Do not heat or put hot
solutions in the volumetric flask because the heat would cause
the flask to expand and the volume would then be incorrect.

Measuring mass accurately:

In many experiments the best method for measuring mass is
1. Measure mass on 2 or 3d.p. balance of a weighing bottle
with the required quantity of solid in it
2. Empty mass into reaction vessel/flask
3. Reweigh the now empty weighing bottle
4. Subtract the mass of the empty weighing bottle from the
Graduated/volumetric flask first reading to give exact of mass actually added.

Dilutions

Diluting a solution
Using a volumetric pipette is more accurate
than a measuring cylinder because it has a
•Pipette 25cm3 of original solution into a 250cm3 volumetric smaller uncertainty
flask
•make up to the mark with distilled water using a dropping Use a teat pipette to make up to the mark in
pipette for last few drops. volumetric flask to ensure volume of solution
• Invert flask several times to ensure uniform solution. accurately measured and one doesn’t go over
the line

N Goalby chemrevise.org 4
Titrations Core Practical 3: Make up a volumetric solution and carry out a simple acid–base titration
General Method
•rinse equipment (burette with acid, pipette with alkali, conical flask with distilled water)
•pipette 25 cm3 of alkali into conical flask
•touch surface of alkali with pipette ( to ensure correct amount is added)
•adds acid solution from burette
•make sure the jet space in the burette is filled with acid
•add a few drops of indicator and refer to colour change at end point
•phenolphthalein [pink (alkali) to colourless (acid): end point pink colour just disappears] [use if NaOH is used]
•methyl orange [yellow (alkali) to red (acid): end point orange] [use if HCl is used]
•use a white tile underneath the flask to help observe the colour change
•add acid to alkali whilst swirling the mixture and add acid drop wise at end point
•note burette reading before and after addition of acid
•repeats titration until at least 2 concordant results are obtained- two readings within 0.1 of each other

Titrations are done often to find out the concentration of one

substance by reacting it with another substance of known
concentration.
They are often done with neutralisation reactions, but can be
done with redox reactions. burette

One substance (generally the one we don’t know the

concentration) is put in the conical flask. It is measured
using a volumetric pipette. conical
The other substance is placed in the burette flask

However, the standard phrase: titrate solution A

with solution B means that A should be in the
conical flask and B should be in the burette.

A conical flask is used in preference to a beaker because

it is easier to swirl the mixture in a conical flask without
spilling the contents.
pipette

Detailed Method for Titration

Make sure bottom of
Using the pipette meniscus is on line on
neck of pipette

•rinse pipette with substance to go in it (often alkali).

•pipette 25 cm3 of solution A into conical flask. The
volumetric pipette will have a mark on its neck to show
the level to fill to. The bottom of the meniscus should
sit on this line.
•touch surface of solution with pipette ( to ensure
correct amount is added). A small amount of solution
will be left in the pipette at this stage. The calibration
of the pipette will take into account this effect. It
should not be forced out.

N Goalby chemrevise.org 5
 Using the burette
The burette should be rinsed out with substance that will be
put in it. If it is not rinsed out the acid or alkali added may be
diluted by residual water in the burette or may react with
substances left from a previous titration. This would lead to
the concentration of the substance being lowered and a larger
titre being delivered.

Don’t leave the funnel in the burette because small drops of

liquid may fall from the funnel during the titration leading to a
false burette reading (would give a lower titre volume)

make sure the jet space in the burette is filled with the
solution and air bubbles are removed.

If the jet space in the burette is not filled properly prior to commencing the
titration it will lead to errors if it then fills during the titration, leading to a
larger than expected titre reading.

Read the bottom of the meniscus on the burette

This is reading 9.00cm3

Even though a burette has marking reading to 0.1cm 3, the burette readings
should always be given to 2dp either ending in 0.00 or 0.05. 0.05cm3 is the
volume of 1 drop of solution delivered from a burette and so this is the
smallest difference in readings that can be measured. If the bottom of the
meniscus sits on a line it should end with a 0.00 as in the above example
9.00cm3. If the meniscus sits between two lines it should end 0.05. e.g. if the
bottom of the meniscus sits between the lines marked 9.1 and 9.2, you should
record 9.15

Adding indicator
Indicators are generally weak acids so only add a few
Add a few drops of indicator and refer to colour change drops of them. If too much is added they will affect
at end point the titration result
phenolphthalein Methyl orange
If acid is added from the burette the colour change would
Methyl orange is a suitable indicator for neutralisation
be pink (alkali) to colourless (acid): end point pink colour
reactions where strong acids are used.
just disappears [use with titrations using strong alkalis e.g.
It is red in acid and yellow in alkali. It is orange at the end
NaOH ]
point.

Methyl orange
Methyl orange Methyl orange
Alkali colour
end point acid colour
phenolphthalein phenolphthalein acid
colour Use a white tile underneath the flask to help
Alkali colour
observe the colour change

N Goalby chemrevise.org 6
Add solution from burette whilst swirling the mixture and add drop-wise at end
point

Distilled water can be added to the conical flask during a titration to wash the
sides of the flask so that all the acid on the side is washed into the reaction
mixture to react with the alkali.
It does not affect the titration reading as water does not react with the reagents
or change the number of moles of acid added.

note burette reading before and after addition of solution

Only distilled water should be used to
repeats titration until at least 2 concordant results are wash out conical flasks between titrations
obtained- two readings within 0.1 of each other because it does not add any extra moles
of reagents
A single titration could be flawed. Repeating allows for
anomalous titres to be spotted and discounted
lf 2 or 3 values are within 0.10cm3 and
therefore concordant or close then we
Recording results can say results are accurate and
•Results should be clearly recorded in a table repeatable and the titration technique
•Result should be recorded in full (i.e. both initial and final readings) is good and consistent
•Record titre volumes to 2dp (0.05 cm3)

Working out average titre results

Titration number 1 2 3 Only make an average of the
concordant titre results

Initial burette reading (cm3 ) 0.50 2.50 1.55 Average titre = (24.50+ 24.40)/2 =
24.45
Final burette reading (cm3 ) 24.50 27.00 25.95

Titre (cm3 ) 24.00 24.50 24.40

Safety precautions
Common Titration Equations
Acids and alkalis are corrosive CH3CO2H + NaOH  CH3CO2-Na+ + H2O
(at low concentrations acids are irritants)
Wear eye protection and gloves H2SO4 + 2NaOH  Na2SO4 +2H2O
If spilled immediately wash affected parts after spillage HCl + NaOH  NaCl +H2O
NaHCO3 + HCl  NaCl + CO2 + H2O
If substance is unknown treat it as potentially toxic and wear
gloves. Na2CO3 + 2HCl 2NaCl + CO2 + H2O

Titrating mixtures
Testing batches If titrating a mixture to work out the concentration of
In quality control it will be necessary to do titrations/testing an active ingredient it is necessary to consider if the
on several samples as the amount/concentration of the mixture contains other substances that have acid
chemical being tested may vary between samples. base properties.
If they don’t have acid base properties we can titrate
with confidence.

N Goalby chemrevise.org 7
Uncertainty
Readings and Measurements
Readings Measurements In general, if uncertainty is not indicated
the values found from a single the values taken as the on apparatus, the following assumptions
judgement when using a piece difference between the are made:
of equipment judgements of two values For an analogue scale-
(e.g. using a burette in a The uncertainty of a reading (one
titration)
judgement) is at least ±0.5 of the smallest
scale reading.
Calculating Apparatus Uncertainties
The uncertainty of a measurement (two
Each type of apparatus has a sensitivity uncertainty
judgements) is at least ±1 of the smallest
•balance  0.001 g (if using a 3 d.p. balance) scale reading.
•volumetric flask  0.1 cm3 - If the apparatus has a digital scale, the
•25 cm3 pipette  0.1 cm3 uncertainty is  the resolution of the
•burette (start & end readings and end point )  0.15 cm3 apparatus in each measurement

Calculate the percentage error for each piece of equipment used by

Uncertainty of a measurement using
% uncertainty =  uncertainty x 100 a burette. If the burette used in the
Measurement made on apparatus titration had an uncertainty for each
reading of +/– 0.05 cm3 then during a
e.g. for burette titration two readings would be taken
% uncertainty = 0.15/average titre result x100 so the uncertainty on the titre volume
would be +/– 0.10 cm3 .
To calculate the maximum total percentage apparatus uncertainty in the
final result add all the individual equipment uncertainties together.

Reducing uncertainties in a titration To decrease the apparatus uncertainties

you can either decrease the sensitivity
Replacing measuring cylinders with pipettes or burettes which have uncertainty by using apparatus with a
lower apparatus uncertainty will lower the % uncertainty. greater resolution (finer scale divisions ) or
you can increase the size of the
To reduce the % uncertainty in a burette reading it is necessary to make measurement made.
the titre a larger volume. This could be done by: increasing the volume
and concentration of the substance in the conical flask or by decreasing
the concentration of the substance in the burette. If looking at a series of measurements in
an investigation, the experiments with
the smallest readings will have the
highest experimental uncertainties.
Reducing uncertainties in measuring mass
Using a balance that measures to more decimal places or using
a larger mass will reduce the % uncertainty in weighing a solid.

Weighing sample before and after addition and then calculating

difference will ensure a more accurate measurement of the
mass added.
If the %uncertainty due to the apparatus < percentage
Calculating the percentage difference between the actual difference between the actual value and the calculated
value and the calculated value value then there is a discrepancy in the result due to
other errors.
If we calculated an Mr of 203 and the real value is 214, then
the calculation is as follows: If the %uncertainty due to the apparatus > percentage
Calculate difference 214-203 = 11 difference between the actual value and the calculated
% = 11/214 x100 value then there is no discrepancy and all errors in the
=5.41% results can be explained by the sensitivity of the
equipment.

N Goalby chemrevise.org 8
Core practical 4: Investigation of the rates of hydrolysis of some halogenoalkanes

Testing for halogenoalkanes method

• Arrange three test tubes in a row and add three drops of halogenoalkane in the sequence 1-chlorobutane, 1-
bromobutane, 1-iodobutane.
• Add 4 cm3 of 0.02 M silver nitrate to each halogenoalkane.
• Without delay, put all three test tubes simultaneously in a hot water bath.
• Note the order in which precipitates appear

Comparing the rate of hydrolysis of halogenoalkanes reaction

Hydrolysis is defined as the splitting of a molecule ( in this case a Water is a poor nucleophile but it can react
haloalkane) by a reaction with water slowly with halogenoalkanes in a
substitution reaction
CH3CH2X + H2O  CH3CH2OH + X- + H+

Aqueous silver nitrate is added to a halogenoalkane and the halide CH3CH2I + H2O  CH3CH2OH + I- + H+
leaving group combines with a silver ion to form a silver halide
Ag+ (aq) + I-(aq)  AgI (s) - yellow precipitate
precipitate.
The precipitate only forms when the halide ion has left the The iodoalkane forms a precipitate with the
halogenoalkane and so the rate of formation of the precipitate can silver nitrate first as the C-I bond is weakest
be used to compare the reactivity of the different halogenoalkanes. and so it hydrolyses the quickest.

The quicker the precipitate is formed, the faster the substitution

reaction and the more reactive the halogenoalkane AgI (s) - yellow precipitate
AgBr(s) – cream precipitate forms faster
The rate of these substitution reactions depends on the strength of the AgCl(s) – white precipitate
C-X bond . The weaker the bond, the easier it is to break and the faster
the reaction.

N Goalby chemrevise.org 9
Core practical 5. Oxidation of an alcohol
Partial Oxidation of Primary Alcohols H
O

Reaction: primary alcohol  aldehyde

Reagent: potassium dichromate (VI) solution and dilute sulfuric acid. H C C

Conditions: (use a limited amount of dichromate) warm gently and distil out
the aldehyde as it forms: H
H

Ethanal

Observation: the orange

H H H H H O dichromate ion (Cr2O72-) reduces
+ [O] H C C C + H2O to the green Cr 3+ ion
H C C C O H
H H H H H H SAFETY
You must wear gloves when handling
O + H2O
OH + [O] solid potassium dichromate(Vl) since it is
highly toxic and a category 2 carcinogen;
CH3CH2CH2OH + [O]  CH3CH2CHO + H2O it is also an irritant. Avoid inhaling any
propanal dust.
propan-1-ol Concentrated sulphuric acid is corrosive.

Detailed Method: The partial oxidation of propan-1-ol

This experiment uses a limited quantity of oxidising agent (0.01 mol) and the product is distilled from the reaction
mixture immediately it is formed. In this way we hope to achieve a partial oxidation of propan-1-ol.

 Place about 10 cm3 of dilute sulfuric acid in a flask and add about 3g of potassium dichromate(VI) and 2 or 3 anti-
bumping granules. Shake the contents of the flask until solution is complete (do not warm).
 Add 1.5 cm3 of propan-1-ol in drops from a dropping pipette, shaking the flask so as to mix the contents, and
then assemble distillation apparatus as shown below
 Gently heat and slowly distil 2 cm3 of liquid into a test tube, taking care that none of the reaction mixture
splashes over.

Distillation It’s important to be able to

draw and label this apparatus
In general used as separation technique to separate an accurately. Don’t draw lines
thermometer between flask, adaptor and
organic product from its reacting mixture. Need to
condenser.
collect the distillate of the approximate boiling point
range of the desired liquid.

Note the bulb of the thermometer should be Liebig condenser

at the T junction connecting to the
condenser to measure the correct boiling
point

Note the water goes in the bottom of the Water

condenser to go against gravity. This allows more out
efficient cooling and prevents back flow of water.
Round Water in
bottomed
flask
Electric heaters are often used to heat organic Heat
chemicals. This is because organic chemicals are
normally highly flammable and could set on fire
with a naked flame.

N Goalby chemrevise.org 10
Reflux: Full Oxidation of Primary Alcohols
H H
Reaction: primary alcohol  carboxylic acid
O

Reagent: potassium/sodium dichromate(VI) solution and H C C C

sulfuric acid
Conditions: use an excess of dichromate, and heat under O H
reflux: (distil off product after the reaction has
H H

finished) Propanoic acid

OH + 2[O] OH
+ H2O
Observation: the
O orange dichromate
ion (Cr2O72-)
CH3CH2CH2OH + 2[O]  CH3CH2COOH + H2O
reduces to the
propan-1-ol Propanoic acid green Cr 3+ ion

Detailed method
 Measure 5 cm3 of water into a boiling tube. Add 6 g of sodium dichromate(VI), shake and set aside to dissolve.
 Put about 1.5 cm3 propan-1-ol into a 50 cm3 round bottomed flask and add about 5 cm3 of water and two or
three anti-bumping granules. Put a condenser on the flask for reflux, as shown in figure below.
 Add 2 cm3 of concentrated sulfuric acid down the condenser in drops from a dropping pipette. While the
mixture is still warm, start to add your sodium dichromate(VI) solution down the condenser in drops from a
dropping pipette. The energy released from the reaction should make the mixture boil. Add the solution a drop
at a time so that the mixture continues to boil without any external heating.
 When all the sodium dichromate(VI) solution has been added, use a low Bunsen burner flame to keep the
mixture boiling for 10 minutes, not allowing any vapour to escape.
 At the end of that time remove the Bunsen burner and arrange the apparatus for distillation. Gently distil 2-3
cm3 of liquid into a test tube.

Reflux
Reflux is used when heating organic reaction mixtures for long periods. The
condenser prevents organic vapours from escaping by condensing them back Water out
to liquids. The reactant vapours of volatile compound are condensed and
returned to the reaction mixture.
condenser
Never seal the end of the condenser as the build up of gas
pressure could cause the apparatus to explode. This is true of any
apparatus where volatile liquids are heated including the
distillation set up

Anti-bumping granules are added to the flask in both distillation Water in

and reflux to prevent vigorous, uneven boiling by making small
bubbles form instead of large bubbles

Round
It’s important to be able to draw and label this apparatus bottomed
flask
accurately.
• Don’t draw lines between flask and condenser.
• Don’t have top of condenser sealed
• Condenser must have outer tube for water that is sealed
Heat
at top and bottom
• Condenser must have two openings for water in and out
that are open

N Goalby chemrevise.org 11
Fractional Distillation: In the laboratory
Fractional distillation is used to
• Heat the flask, with a Bunsen burner or electric mantle
separate liquids with different
• This causes vapours of all the components in the mixture
boiling points
to be produced.
• Vapours pass up the fractionating column.
• The vapour of the substance with the lower boiling point
reaches the top of the fractionating column first.
• The thermometer should be at or below the boiling point
of the most volatile substance.
• The vapours with higher boiling points condense back
into the flask.
• Only the most volatile vapour passes into the condenser.
• The condenser cools the vapours and condenses to a
condenser
liquid and is collected.
fractionating column

flask

N Goalby chemrevise.org 12
Purifying an organic liquid

General method
• Put the distillate of impure product into a separating funnel
Sodium hydrogencarbonate will neutralise
• wash product by adding either
any remaining reactant acid.
• sodium hydrogencarbonate solution , shaking and
releasing the pressure from CO2 produced.
Sodium chloride will help separate the
• Saturated sodium chloride solution
organic layer from the aqueous layer
•Allow the layers to separate in the funnel, and then run and
discard the aqueous layer. The layer with lower density will be the
upper layer. This is usually the organic layer
•Run the organic layer into a clean, dry conical flask and add three
spatula loads of drying agent (e.g. anhydrous sodium sulfate, The drying agent should
calcium chloride) to dry the organic liquid. When dry the organic •be insoluble in the organic liquid
liquid should appear clear. • not react with the organic liquid

• Carefully decant the liquid into the distillation flask Decant means carefully pour off organic
liquid leaving the drying agent in the
•Distill to collect pure product conical flask

Separating funnel

Distillation It’s important to be able to

draw and label this apparatus
In general used as separation technique to separate accurately. Don’t draw lines
thermometer between flask, adaptor and
an organic product from its reacting mixture. In order
condenser.
to maximise yield collected, only collect the distillate
at the approximate boiling point of the desired
aldehyde and not higher.

Note the bulb of the thermometer should be Liebig condenser

at the T junction connecting to the
condenser to measure the correct boiling
point

Note the water goes in the bottom of the Water

condenser to go against gravity. This allows more out
efficient cooling and prevents back flow of water.
Round Water in
bottomed
flask
Electric heaters are often used to heat organic Heat
chemicals. This is because organic chemicals are
normally highly flammable and could set on fire The collection flask can be
with a naked flame. cooled in ice to help improve
yield of distillate

N Goalby chemrevise.org 13
Core practical 6: Chlorination of 2-methylpropan-2-ol using concentrated hydrochloric acid

Detailed method for preparing and purifying a halogenoalkane from an alcohol

1. Measure 8 cm3 of 2-methylpropan-2-ol in a measuring cylinder and measure its mass.
2. Pour the 2-methylpropan-2-ol into a separating funnel, and reweigh the measuring cylinder to find the
mass of the 2-methylpropan-2-ol used.
3. In a fume cupboard, add 20 cm3 of concentrated hydrochloric acid to the separating funnel, in portions
of 3cm3. After each portion, stopper the flask and invert it several times . Open the tap when doing this
to release the pressure.
4. Allow the separating funnel to stand in the fume cupboard for about 20 minutes. Gently shake it at
intervals.
5. After 20 minutes, allow the layers to separate in the funnel. Open the tap and remove the lower
aqueous layer. Dispose of this layer.
6. Add sodium hydrogencarbonate solution in 2 cm3 portions to the separating funnel. This neutralises any
remaining acid. Shake the funnel after each addition, and release the pressure. Continue until no more
bubbles of CO2 are seen.
7. Allow the layers to separate in the funnel. Again remove and pour away the lower aqueous layer. Run
off the organic layer into a clean conical flask and add two spatulas of anhydrous sodium sulfate.
Stopper the flask, shake the contents and allow this to stand until the liquid becomes clear. This step
dries the organic liquid.
8. Decant the liquid into a weighed clean distillation flask.
9. Distil the liquid by holding a 250ml beaker half-full of boiled water around the flask using standard
distillation set up. Collect the liquid that distils in the range 47-53oC.
10. Measure the mass of the 2-chloro-2-methylpropane collected.

Detailed method for preparing and purifying Cyclohexene from cyclohexanol

OH
Conc
H3PO4
+H2O

a) Pour about 20 cm3 of cyclohexanol into a weighed 50 cm3 pear-shaped flask. Reweigh the flask and record
the mass of cyclohexanol.
b) Using a plastic graduated dropping pipette, carefully and with frequent shaking, add to the flask
approximately 8 cm3 of concentrated phosphoric acid.
c ) Add a few anti-bumping granules to the flask and assemble the distillation apparatus, so that the contents
of the flask may be distilled. Heat the flask gently, distilling over any liquid which boils below 100 °C.
d) Pour the distillate into a separating funnel and add 50 cm 3 of saturated sodium chloride solution. Shake
the mixture and allow the two layers to separate.
e) run off the lower layer into a beaker and then transfer the upper layer, which contains the crude
cyclohexene, into a small conical flask.
f) Add a few lumps of anhydrous calcium chloride or anhydrous sodium sulfate(VI) or anhydrous magnesium
sulfate to the crude cyclohexene to remove water. Stopper the flask, shake the contents and allow this to
stand until the liquid becomes clear.
g) Decant the liquid into a clean, dry, weighed sample container.
h) Reweigh the container, calculate the mass of dry cyclohexene produced

N Goalby chemrevise.org 14
Detailed Method for Preparing and Purifying an Ester
Propyl ethanoate can be made in the laboratory from propan-
1-ol and ethanoic acid.
The equation for the reaction is
CH3COOH + CH3CH2CH2OH  CH3COOCH2CH2CH3 + H2O
Procedure
1. Propan-1-ol (50 cm3) and ethanoic acid (50 cm3) are mixed
thoroughly in a 250 cm3 round-bottomed flask.
2. Concentrated sulfuric acid (10 cm3) is added drop by drop Sulfuric acid is a catalyst
Adding conc H2SO4 is an exothermic reaction- to
to the mixture, keeping the contents of the flask well-shaken
prevent uncontrolled boiling over add drop by drop
and cooled in an ice-water bath. and cool

3. When the acid has all been added, a reflux condenser is In reflux the reactant vapours of volatile compound
fitted to the flask and the mixture gently boiled over an are condensed and returned to the reaction mixture.
electric heating mantle for about 30 minutes. The reaction is slow so it is heated for 30 minutes
The electric heating mantle allows for controlled
heating and stops flammable vapour lighting
4. The mixture is cooled, and the apparatus rearranged for
distillation. The crude ester (about 60 cm3) is distilled off. Sodium carbonate reacts with unreacted acid and
5. The distillate is placed in a separating funnel and shaken remaining catalyst still present after distillation.
with about half its volume of 30% sodium carbonate solution, The reaction produces CO2 so the pressure of gas
with the pressure being released at intervals. The lower needs to be released.
The upper layer is organic because it has a lower
aqueous layer is then discarded.
density than water

6. The crude ester is shaken in a separating funnel with about

half its volume of 50% calcium chloride solution, which
removes unreacted alcohol. The lower layer is discarded.
Calcium chloride is a drying agent. The liquid will
7. The ester is run into a clean, dry flask containing some appear clear when dry.
anhydrous calcium chloride and swirled.

8. The ester is filtered into a clean, dry flask, with a few anti- Anti-bumping granules are added to the prevent
bumping granules, and distilled. The fraction boiling between vigorous, uneven boiling by making small bubbles
100°C and 103°C is collected. form instead of large bubbles

Measuring boiling point

Purity of liquid can be determined by measuring a boiling point. This can be done
in a distillation set up or by simply boiling a tube of the sample in an heating oil To get a correct measure of
bath. If the liquid is pure it will have the boiling point referred to in data books. If boiling point the
impure the boiling point tends to be higher than the pure liquid thermometer should be
above the level of the surface
of the boiling liquid and be
Pressure should be noted as changing pressure can change the boiling point of
measuring the temperature
a liquid
of the saturated vapour.

Measuring boiling point is not the most accurate method of identifying a

substance as several substances may have the same boiling point.

N Goalby chemrevise.org 15
Core practical 7 + 15: Analysis of some inorganic unknowns
Testing for cations
Flame tests
Method Lithium : Scarlet red
Use a nichrome wire ( nichrome is an unreactive metal and Sodium : Yellow
will not give out any flame colour) Potassium : lilac
Clean the wire by dipping in concentrated hydrochloric acid Rubidium : red
Caesium: blue
and then heating in Bunsen flame Magnesium: no flame colour (energy emitted of a
If the sample is not powdered then grind it up. wavelength outside visible spectrum)
Dip wire in solid and put in Bunsen flame and observe flame Calcium: brick red
Strontium: red
Barium: apple green

Method: adding dilute sodium hydroxide This test can be used

a) Place about 10 drops of 0.1 mol dm–3 metal ion solution in a test tube. on group 2 metal
b) Add about 10 drops of 0.6 mol dm–3 sodium hydroxide solution, mixing well. ions and transition
c) Continue to add sodium hydroxide solution, dropwise with gentle shaking, until in excess metal ions.

Results for Group 2

The results in this test are an application of the trend that group II hydroxides become more soluble down the group.

Magnesium hydroxide is classed as insoluble in water and

will appear as a white precipitate. A suspension of magnesium hydroxide in water
will appear slightly alkaline (pH 9) so some
Simplest Ionic Equation for formation of Mg(OH)2 (s) hydroxide ions must therefore have been
Mg2+ (aq) + 2OH-(aq)  Mg(OH)2 (s). produced by a very slight dissolving.

Calcium hydroxide is classed as partially soluble in water and

will appear as a white precipitate (it may need more sodium A suspension of calcium hydroxide in water will
hydroxide to be added before it appears compared to a appear more alkaline (pH 11) than magnesium
magnesium solution.) hydroxide as it is more soluble so there will be
more hydroxide ions present in solution.
Simplest Ionic Equation for formation of Ca(OH)2 (s)
Ca2+ (aq) + 2OH-(aq)  Ca(OH)2 (s).
Strontium and barium salts will not form a hydroxide precipitate on addition of
sodium hydroxide due to their high solubility. The solutions will be highly alkaline

Results for transition metals

[Cu(H2O)6]2+ (aq) + 2OH- (aq)  Cu(H2O)4(OH)2 (s) + 2H2O (l)
Copper(II) solutions form a blue ppt,
Cobalt(II) solutions form a blue ppt, [Co(H2O)6]2+ (aq) + 2OH- (aq)  Co(H2O)4(OH)2 (s) + 2H2O (l)
iron (II) solutions form a green ppt [Fe(H2O)6]2+ (aq) + 2OH- (aq)  Fe(H2O)4(OH)2 (s) + 2H2O (l)
iron (III) solutions form a brown ppt [Fe(H2O)6]3+ (aq) + 3OH- (aq)  Fe(H2O)3(OH)3 (s) + 3H2O (l)
Chromium (III) solutions form a green
ppt which dissolves in excess to form a [Cr(H2O)6]3+(aq) + 3OH- (aq)  Cr(H2O)3(OH)3 (s) + 3H2O (l)
green solution
Cr(H2O)3(OH)3 (s) + 3OH- (aq ) [Cr(OH)6]3- (aq) + 3H2O(l)

Testing for Ammonium ions (NH4+)

a) Place about 10 drops of 0.1 mol dm–3 ammonium chloride in a test tube. Results: alkaline
b) Add about 10 drops of 0.4 mol dm–3 sodium hydroxide solution. Shake the mixture. ammonia gas is released
c) Warm the mixture in the test tube gently using a water bath. which turns the red
d) Test the fumes released from the mixture by holding a piece of damp red litmus litmus paper blue
paper in the mouth of the test tube.

N Goalby chemrevise.org 16
Core practical 7+15: Analysis of some inorganic unknowns
Testing for anions: – Group 7 (halide ions), OH– , CO32– , SO42–

Testing for presence of a sulfate ion

BaCl2 solution acidified with hydrochloric acid is used as a reagent to test for
sulphate ions.
If acidified barium chloride is added to a solution that contains sulfate ions a white
precipitate of barium sulfate forms.

Simplest ionic equation Other anions should give a negative

result which is no precipitate
Ba2+ (aq) + SO42-(aq)  BaSO4 (s).
forming.

The hydrochloric acid is needed to react with carbonate impurities that are often found in salts which
would form a white Barium carbonate precipitate and so give a false result. You could not used
sulphuric acid because it contains sulphate ions and so would give a false positive result.

2HCl + Na2CO3  2NaCl + H2O + CO2 Fizzing due to CO2 would be observed if a carbonate was present.

Testing for presence of halide ions with silver nitrate. The role of nitric acid is to react with any
carbonates present to prevent formation of the
This reaction is used as a test to identify which halide ion is precipitate Ag2CO3. This would mask the desired
present. The test solution is made acidic with nitric acid, and observations
then Silver nitrate solution is added dropwise.
2 HNO3 + Na2CO3  2 NaNO3 + H2O + CO2

Fluorides produce no precipitate

Chlorides produce a white precipitate
Ag+(aq) + Cl- (aq)  AgCl(s)
Bromides produce a cream precipitate
Ag+(aq) + Br- (aq)  AgBr(s)
Iodides produce a pale yellow precipitate
Ag+(aq) + I- (aq)  AgI(s)

The silver halide precipitates can be treated with ammonia solution to help differentiate between them
if the colours look similar:

Silver chloride dissolves in dilute ammonia to form a complex ion

AgCl(s) + 2NH3(aq) [Ag(NH3)2]+ (aq) + Cl- (aq)
Colourless solution
Silver bromide dissolves in concentrated ammonia to form a complex ion
AgBr(s) + 2NH3(aq) [Ag(NH3)2]+ (aq) + Br - (aq)
Colourless solution
Silver iodide does not react with ammonia – it is too insoluble.

Testing for presence of carbonate ions

Add any dilute acid and observe effervescence.
Bubble gas through limewater to test for CO2 – will turn limewater cloudy Fizzing due to CO2 would be
observed if a carbonate was
2HCl + Na2CO3  2NaCl + H2O + CO2 present

Testing for presence of a hydroxide ions

Alkaline hydroxide ions will turn red litmus paper blue

N Goalby chemrevise.org 17
Reactions of halide salts with concentrated sulfuric acid.
The halides show increasing power as reducing
Explanation of differing reducing power of halides
agents as one goes down the group. This can be
A reducing agent donates electrons.
clearly demonstrated in the various reactions of
The reducing power of the halides increases down group 7
the solid halides with concentrated sulfuric acid.
They have a greater tendency to donate electrons.
This is because as the ions get bigger it is easier for the outer
Know the equations and observations of these electrons to be given away as the pull from the nucleus on them
reactions very well. becomes smaller.

Fluoride and Chloride

F- and Cl- ions are not strong enough reducing agents to reduce the S in H 2SO4. No redox
reactions occur. Only acid-base reactions occur.

NaF(s) + H2SO4(l) NaHSO4(s) + HF(g)

These are acid –base reactions and not
Observations: White steamy fumes of HF are evolved.
redox reactions. H2SO4 plays the role of
NaCl(s) + H2SO4(l)  NaHSO4(s) + HCl(g) an acid (proton donor).
Observations: White steamy fumes of HCl are evolved.

Bromide
Br- ions are stronger reducing agents than Cl- and F- and after the initial acid-base
reaction reduce the sulfur in H2SO4 from +6 to + 4 in SO2
Observations: White steamy fumes of
Acid- base step: NaBr(s) + H SO (l)  NaHSO (s) + HBr(g) HBr are evolved.
2 4 4

Redox step: 2HBr + H2SO4  Br2(g) + SO2(g) + 2H2O(l) Red fumes of Bromine are also evolved
and a colourless, acidic gas SO2
Ox ½ equation 2Br -  Br2 + 2e-
Re ½ equation H2SO4 + 2 H+ + 2 e-  SO2 + 2 H2O Reduction product = sulfur dioxide

Note the H2SO4 plays the role of acid in the first step producing HBr and then
acts as an oxidising agent in the second redox step.

Iodide
I- ions are the strongest halide reducing agents. They can reduce the sulfur from +6 in
H2SO4 to + 4 in SO2, to 0 in S and -2 in H2S.

NaI(s) + H2SO4(l)  NaHSO4(s) + HI(g) Observations:

2HI + H2SO4  I2(s) + SO2(g) + 2H2O(l) White steamy fumes of HI are evolved.
6HI + H2SO4  3 I2 + S (s) + 4 H2O (l) Black solid and purple fumes of Iodine are also
8HI + H2SO4 4I2(s) + H2S(g) + 4H2O(l) evolved
A colourless, acidic gas SO2
A yellow solid of Sulphur
Ox ½ equation 2I -  I2 + 2e- H2S (Hydrogen Sulphide), a gas with a bad egg
Re ½ equation H2SO4 + 2 H+ + 2 e-  SO2 + 2 H2O smell,

Re ½ equation H2SO4 + 6 H+ + 6 e-  S + 4 H2O

Reduction products = sulfur dioxide, sulfur
Re ½ equation H2SO4 + 8 H+ + 8 e-  H2S + 4 H2O and hydrogen sulfide

Note the H2SO4 plays the role of acid in the first step producing HI and then
acts as an oxidising agent in the three redox steps

Often in exam questions these redox reactions are

worked out after first making the half-equations

N Goalby chemrevise.org 18
 More on Insoluble salts and Precipitation reactions

Insoluble salts can be made by mixing appropriate solutions of ions so that a precipitate is formed
Barium nitrate (aq) + sodium sulfate (aq)  Barium Sulfate (s) + sodium nitrate (aq)
These are called precipitation reactions. A precipitate is a solid

There are some common rules for solubility of salts. No syllabus requires these to be learnt but a good
chemist does know them.
Soluble salts Insoluble salts
All sodium, potassium and ammonium salts
All nitrates
Most chlorides, bromides, iodides Silver, lead chlorides, bromides iodides
Most sulfates Lead, strontium and barium sulfate
Sodium, potassium and ammonium Most other carbonates
carbonates
Sodium, potassium and ammonium Most other hydroxides
hydroxides

When making an insoluble salt, normally the salt would be removed by filtration, washed with distilled
water to remove soluble impurities and then dried on filter paper

Filtration
Filter
paper Buchner
residue
funnel
Filter Filter paper
funnel
Buchner flask (has
Air outlet to
thicker glass walls than
water pump
a normal flask to cope
filtrate with the vacuum )

This is gravitational filtration. Use This is vacuum filtration. The apparatus is

if small amounts of solid are connected to a water pump which will
formed. produce a vacuum. Use if larger amounts of
solid are formed.

For both types of filtration apparatus Edexcel expect filter paper to be drawn on the diagram

Writing Ionic equations for precipitation reactions

We usually write ionic equations to show precipitation Spectator ions are ions that are
reactions. Ionic equations only show the ions that are • Not changing state
reacting and leave out spectator ions. • Not changing oxidation number

Take full equation Ba(NO3)2 (aq) + Na2SO4 (aq)  BaSO4 (s) + 2 NaNO3 (aq)

Separate (aq) solutions into Ba2+(aq) + 2NO3-(aq) + 2Na+ (aq)+ SO42-(aq)  BaSO4(s) + 2 Na+(aq)+ 2NO3- (aq)
ions

Cancel out spectator ions leaving

Ba2+ (aq) + SO42-(aq)  BaSO4 (s).
the simplest ionic equation

N Goalby chemrevise.org 19
Core practical 7+15: Analysis of some organic unknowns
Tests for alcohol, aldehyde, alkene and carboxylic acid
Functional group test for an Alkene
To 0.5 cm3 of bromine water in a test tube add a few drops of the unknown and shake.
Observation: alkenes should decolourise bromine water

Reaction with 2,4-dinitro phenylhydrazine

2,4-DNP reacts with both aldehydes and ketones. The product Use 2,4-DNP to identify if the compound is a
is an orange precipitate, It can be used as a test for a carbonyl carbonyl. Then to differentiate an aldehyde
group in a compound. from a ketone use Tollen’s reagent.

The melting point of the crystal formed can be used to help

identify which carbonyl was used. Take the melting point of
orange crystals product from 2,4-DNP. Compare melting point
with known values in database

Functional group tests for an aldehyde

Tollen’s Reagent
Reagent: Tollen’s reagent formed by mixing aqueous ammonia and silver
nitrate. The active substance is the complex ion of [Ag(NH 3)2]+ .
Conditions: heat gently
Reaction: aldehydes only are oxidised by Tollen’s reagent into a carboxylic
acid and the silver(I) ions are reduced to silver atoms
Observation: with aldehydes, a silver mirror forms coating the inside of the
test tube. Ketones result in no change.

CH3CHO + 2Ag+ + H2O  CH3COOH + 2Ag + 2H+

Tollen's reagent method

Place 1 cm3 of silver nitrate solution in each of two clean boiling tubes.
Then add one drop of sodium hydroxide solution to form a precipitate of
silver oxide. Add ammonia solution dropwise until a clear, colourless
solution is formed. Add a few drops of the unknown and leave in the
water bath for a few minutes.

Fehling’s solution
Reagent: Fehling’s solution containing blue Cu 2+ ions. Fehling's solution method
Conditions: heat gently Place 1 cm3 of Fehling's A into each of
two boiling tubes, and then add Fehling's
Reaction: aldehydes only are oxidised by Fehling’s Solution
into a carboxylic acid and the copper (II) ions are B until the blue precipitate redissolves.
reduced to copper(I) oxide . Add a few drops of the unknown and
Observation: Aldehydes :Blue Cu 2+ ions in solution change leave in the water bath for a few
to a red precipitate of Cu2O. Ketones do not react minutes.

CH3CHO + 2Cu2+ + 2H2O  CH3COOH + Cu2O + 4H+

N Goalby chemrevise.org 20
Reaction of carbonyls with iodine in presence of alkali

Reagents: Iodine and sodium hydroxide Only carbonyls with a methyl group next to the O
Conditions: warm very gently C=O bond will do this reaction. Ethanal is the
only aldehyde that reacts. More commonly is H3C C H
The product CHI3 is a yellow crystalline methyl ketones.
precipitate with an antiseptic smell

This reaction is called the Iodoform test

Functional group test for a Carboxylic acid

To 0.5 cm3 of your unknown solution in a test tube add a The presence of a carboxylic acid can be tested by
small amount of sodium carbonate solid and observe. addition of sodium carbonate. It will fizz and produce
Result carboxylic acids will fizz with sodium carbonate due carbon dioxide
to CO2 produced 2CH3CO2H + Na2CO3  2CH3CO2-Na+ + H2O + CO2

Summary of Identification of Functional Groups by test-tube reactions

Functional group Reagent Result

Alkene Bromine water Orange colour

decolourises
Alcohols + carboxylic acids PCl5 Misty fumes of HCl
produced
Alcohols, phenols, Sodium metal Effervescence due to H2
carboxylic acids gas
Carbonyls 2,4,DNP Orange/red crystals
produced
Aldehyde Fehling’s solution Blue solution to red
precipitate
Aldehyde Tollen’s reagent Silver mirror formed

Carboxylic acid Sodium carbonate Effervescence of CO2

evolved
1o 2o alcohol and Sodium dichromate and Orange to green colour
aldehyde sulfuric acid change
chloroalkane Warm with silver nitrate Slow formation of white
precipitate of AgCl
Acyl chloride Silver nitrate Vigorous reaction- steamy
fumes of HCl- rapid white
precipitate of AgCl

N Goalby chemrevise.org 21
Core practical 8: To determine the enthalpy change of a reaction using Hess’s Law
Measuring the Enthalpy Change for a Reaction Experimentally
Calorimetric method This equation will only give the
energy for the actual quantities
For a reaction in solution we use the following equation used. Normally this value is
converted into the energy
energy change = mass of solution x heat capacity x temperature change
change per mole of one of the
Q (J) = m (g) x cp (J g-1K-1) x T ( K) reactants. (The enthalpy change
of reaction, H)

Calorimetric method
One type of experiment is one in which substances are mixed This could be a solid dissolving or reacting in a
in an insulated container and the temperature rise measured. solution or it could be two solutions reacting
together

General method
 washes the equipment (cup and pipettes etc) with the solutions to be used
 dry the cup after washing
 put polystyrene cup in a beaker for insulation and support
 Measure out desired volumes of solutions with volumetric pipettes and transfer to
insulated cup
 clamp thermometer into place making sure the thermometer bulb is immersed in
solution
 measure the initial temperatures of the solution or both solutions if 2 are used. Do this
every minute for 2-3 minutes
 At minute 3 transfer second reagent to cup. If a solid reagent is used then add the
solution to the cup first and then add the solid weighed out on a balance.
 If using a solid reagent then use ‘before and after’ weighing method
 stirs mixture (ensures that all of the solution is at the same temperature)
 Record temperature every minute after addition for several minutes

If the reaction is slow then the exact temperature rise can be

difficult to obtain as cooling occurs simultaneously with the
reaction

To counteract this we take readings at regular time intervals and

extrapolate the temperature curve/line back to the time the
reactants were added together.

We also take the temperature of the reactants for a few minutes

before they are added together to get a better average
temperature. If the two reactants are solutions then the
temperature of both solutions need to be measured before
addition and an average temperature is used.

Errors in this method Read question carefully. It

may be necessary to
• energy transfer from surroundings (usually loss) describe:
• approximation in specific heat capacity of solution. The method assumes all • Method
solutions have the heat capacity of water. • Drawing of graph with
• neglecting the specific heat capacity of the calorimeter- we ignore any energy extrapolation
absorbed by the apparatus. • Description of the
• reaction or dissolving may be incomplete or slow. calculation
• Density of solution is taken to be the same as water.

N Goalby chemrevise.org 22
Calculating the enthalpy change of reaction, Hr from experimental data
The heat capacity of water is 4.18
General method J g-1K-1. In any reaction where the
reactants are dissolved in water
1. Using q= m x cp x T calculate energy change for quantities used we assume that the heat capacity
is the same as pure water.
2. Work out the moles of the reactants used
3. Divide q by the number of moles of the reactant not in excess to give H Also assume that the solutions
have the density of water, which is
4. Add a sign and unit (divide by a thousand to convert Jmol -1 to kJmol-1
1g cm-3. Eg 25cm3 will weigh 25 g

Example 3. Calculate the enthalpy change of reaction for the reaction where 25.0cm3 of 0.20 mol dm-3 copper
sulfate was reacted with 0.01mol (excess of zinc). The temperature increased 7.0oC .

Step 1: Calculate the energy change for the amount of reactants in the test tube.
Q = m x cp x T Note the mass is the mass of the copper sulfate
Q = 25 x 4.18 x 7 solution only. Do not include mass of zinc powder.
Q = 731.5 J

Step 2 : calculate the number of moles of the reactant not in excess.

moles of CuSO4 = conc x vol If you are not told what is in excess, then you need to work
= 0.2 x 25/1000 out the moles of both reactants and work out using the
= 0.005 mol balanced equation which one is in excess.

Step 3 : calculate the enthalpy change per mole, H (the enthalpy change of reaction)
H = Q/ no of moles
= 731.5/0.005
= 146300 J mol-1
= 146 kJ mol-1 to 3 sf
Remember in these
Finally add in the sign to represent the energy change: if temp increases the questions: sign, unit
reaction is exothermic and is given a minus sign e.g. –146 kJ mol-1

Example 4. 25.0cm3 of 2.0M HCl was neutralised by 25.0cm3 of 2.0M NaOH. The temperature increased 13.5oC
Calculate the enthalpy change per mole of HCl?

Step 1: Calculate the energy change for the amount of reactants in the test tube.
Q = m x cp x T
Note the mass equals the mass of acid + the
Q = 50 x 4.18 x13.5 mass of alkali, as they are both solutions.
Q = 2821.5 J

Step 2 : calculate the number of moles of the HCl.

moles of HCl = conc x vol
= 2 x 25/1000
= 0. 05 mol

Step 3 : calculate H, the enthalpy change per mole, which might be called the enthalpy change of neutralisation
H = Q/ no of moles
= 2821.5/0.05 Remember in these
= 56430 J mol-1 Exothermic and so is given a minus sign questions: sign, unit,
= -56.4 kJ mol-1 to 3 sf

N Goalby chemrevise.org
23
Often Hess’s law cycles are used to measure the enthalpy change for a reaction that cannot be measured directly by
experiments. Instead alternative reactions are carried out that can be measured experimentally.

H reaction This Hess’s law is used to work out the

enthalpy change to form a hydrated salt from
CuSO4 (s) + 5H2O (l) CuSO4.5H2O (s)
an anhydrous salt.

-66.1 kJ mol-1 + aq + aq +11kJ mol-1

This cannot be done experimentally because it
is impossible to add the exact amount of water
CuSO4 (aq) without the solid dissolving and it is not easy to
measure the temperature change of a solid.

H reaction + 11kJmol-1 = -66.1 kJ mol-1 Instead both salts are dissolved in excess water
H reaction= -66.1 - 11 to form a solution of copper sulfate. The
temperature changes can be measured for
= -77.1 kJ mol-1
these reactions.

Detailed method for measuring enthalpy change of solution of anhydrous copper(II) sulfate
1. Weigh out between 3.90 g and 4.10 g of anhydrous copper(II) sulfate in a dry weighing bottle. The precise mass
should be recorded.
2. Using a volumetric pipette, place 25 cm3 of deionised water into a polystyrene cup and record its temperature at the
beginning (t=0), start the timer and then record the temperature again every minute, stirring the liquid continuously.
3. At the fourth minute, add the powdered anhydrous copper(II) sulfate rapidly to the water in the polystyrene cup and
continue to stir, but do not record the temperature.
4. Reweigh the empty weighing bottle
5. At the fifth minute and for every minute up to 15 minutes, stir and record the temperature of the solution in the
polystyrene cup.
6. Plot a graph of temperature (on the y-axis) against time. Draw two separate best fit lines; one, which joins the points
before the addition, and one, which joins the points after the addition, extrapolating both lines to the fourth minute.
7. Use your graph to determine the temperature change at the fourth minute, which theoretically should have
occurred immediately on addition of the solid.
8. Using q= m x cp x T calculate energy change
= 20 x 4.18 x T
9. Calculate Hsolution by dividing q by number of moles of anhydrous copper(II) sulfate in mass added

The above method is then repeated using hydrated copper sulfate. The two Hsolution can then be used to calculate
the H for the enthalpy change of forming a hydrated salt as in the example above

N Goalby chemrevise.org 24
Measuring Enthalpies of Combustion using Flame Calorimetry

Enthalpies of combustion can be calculated by using calorimetry.

Generally the fuel is burnt and the flame is used to heat up water in a
metal cup.
Need to measure
• mass of spirit burner before and after
• Temperature change of water
• Volume of water in cup

Errors in this method

• energy losses from calorimeter
• Incomplete combustion of fuel
• Incomplete transfer of energy
• Evaporation of fuel after weighing
• Heat capacity of calorimeter not included
• Measurements not carried out under standard conditions as H2O is
gas, not liquid, in this experiment

Example 5. Calculate the enthalpy change of combustion for the reaction where 0.65g of propan-1-ol was
completely combusted and used to heat up 150g of water from 20.1 to 45.5 oC

Step 1: Calculate the energy change used to heat up the water.

Q = m x cp x T
Note the mass in this equation is the mass of water in
Q = 150 x 4.18 x 25.4
the calorimeter and not the alcohol
Q = 15925.8 J

Step 2 : calculate the number of moles of alcohol combusted.

moles of propan-1-ol = mass/ Mr

= 0.65 / 60
= 0.01083 mol

Step 3 : calculate the enthalpy change per mole which is called cH (the enthalpy change of combustion)
H = Q/ no of moles
= 15925.8/0.01083
= 1470073 J mol-1
= 1470 kJ mol-1 to 3 sf
Remember in these
Finally add in the sign to represent the energy change: if temp increases the
questions: sign, unit
reaction is exothermic and is given a minus sign eg –1470 kJ mol-1

N Goalby chemrevise.org 25