Chemistry Practicals

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The document describes procedures for preparing volumetric solutions and using titration to determine concentrations. It also describes the use of thin layer chromatography to separate and identify compounds.

The experiment aims to prepare a sodium hydroxide solution of known concentration and then use it to determine the concentration of a sodium hydrogensulfate solution via acid-base titration.

The steps involved in preparing a volumetric solution described are: weighing the solid, dissolving it in water, transferring it to a volumetric flask, and diluting it to the graduation mark.

A-level Chemistry exemplar for required practical No.

1 part a

Make up a volumetric solution and carry out a simple acid-base titration:


To prepare a solution of sodium hydrogensulfate that has a known concentration

Student sheet

Requirements

You are provided with the following:

weighing bottle or boat


250 cm3 volumetric (graduated) flask
sodium hydrogensulfate solid
filter funnel
spatula
deionised or distilled water in a wash bottle
250 cm3 beaker
glass rod
digital mass balance (reading to 2 or 3 decimal places).

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Suggested method

The task is to prepare 250 cm3 of a solution of sodium hydrogensulfate with a known concentration
in the range 0.090 to 0.110 mol dm3

The procedure is as follows:

a) Calculate the mass of sodium hydrogensulfate solid needed to produce 250 cm3 of a
0.100 mol dm3 solution. Show your working. If you are using the anhydrous solid, the mass to
weigh out will be between 2.7 and 3.3 g, and if you are using the monohydrate, the mass to
weigh out should be between 3.1 and 3.8 g
b) Weigh a clean dry weighing bottle (or weighing boat).
c) Place the weighing bottle on the pan of a digital balance and, using a spatula, place into
the bottle approximately the mass of sodium hydrogensulfate that you have calculated to be
necessary.
d) Weigh the weighing bottle and its contents accurately and record the precise mass.
e) Pour the contents of the weighing bottle into a beaker and re-weigh the weighing bottle
(which may still contain traces of sodium hydrogensulfate).
f) Calculate the mass of sodium hydrogensulfate that you have transferred. Remember to record
all weighings to the resolution of the balance that you have used.
g) Add approximately 100 cm3 of deionised (or distilled) water to the beaker containing the
solid and use a glass rod to stir the contents of the beaker until all of the sodium
hydrogensulfate dissolves.
h) Using a funnel, pour the contents of the beaker into a 250 cm3 volumetric (graduated)
flask and then using the wash bottle rinse the beaker and funnel into the same volumetric
flask. Rinse the glass rod into these washings.
i) Make the volumetric flask up to the graduated mark by carefully adding deionised water
from the wash bottle. You will need to be careful so that you do not over-shoot the mark.
j) Stopper the volumetric flask and shake it thoroughly to mix the contents of the flask.
k) Calculate the exact concentration in mol dm3 of your solution quoting the value to the
appropriate precision. Show all of your working.

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A-level Chemistry exemplar for required practical No. 1 part b

Make up a volumetric solution and carry out a simple acid-base titration:


To determine the concentration of a solution of sodium hydroxide by titration using a
sodium hydrogensulfate solution that has a known concentration

Student sheet

Requirements

You are provided with the following:

burette
stand and clamp
25 cm3 pipette
pipette filler
two 250 cm3 conical flasks
two 250 cm3 beakers
funnel
wash bottle
phenolphthalein indicator
sodium hydrogensulfate solution
sodium hydroxide solution.

The sodium hydrogensulfate solution may be the solution which you prepared in part a of this
experiment or it could be a solution provided to you by your teacher.

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Suggested method

a) Pour approximately 100 cm3 of the sodium hydrogensulfate solution into a clean, dry beaker
that is labelled sodium hydrogensulfate. Use a small volume of this solution to rinse the
burette before filling it with the sodium hydrogensulfate solution.
b) Pour approximately 100 cm3 of the sodium hydroxide solution into a second clean, dry beaker
labelled sodium hydroxide.
c) Rinse a 25 cm3 pipette with the sodium hydroxide solution provided and then, using a pipette
filler, pipette exactly 25.0 cm3 of sodium hydroxide solution into a 250 cm3 conical flask
(which has been rinsed with deionised water).
d) Add two to three drops of phenolphthalein indicator to the solution in the conical flask and
note the colour of the indicator in alkali.
e) Before you start to titrate, construct a table ready to record your results.
f) Record the initial burette reading. Make sure that all your burette readings are to the
appropriate precision.
g) Titrate the contents of the conical flask by adding sodium hydrogensulfate solution to it from
the burette. Add the sodium hydrogensulfate solution slowly, swirling the flask gently to mix
the solution. Add the sodium hydrogensulfate solution dropwise near the end-point until the
indicator undergoes a definite colour change; this is the end-point of the titration. Record the
colour change in your results. Record the final burette reading in your table of results.

h) Calculate and record in your table of results the volume of sodium hydrogensulfate solution
used.
i) Repeat the titration until you obtain two results which are concordant. You should normally
carry out at least three titrations. Record all of the results that you obtain.
j) Calculate and record the mean volume of sodium hydrogensulfate solution used in the
titration. Show your working.
k) Use your results to calculate the concentration of the sodium hydroxide. Show your working.

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A-level Chemistry exemplar for required practical No. 2

Measurement of an enthalpy change:


To determine an enthalpy change which cannot be measured directly. The reaction
involves the conversion of anhydrous copper(II) sulfate into hydrated copper(II) sulfate.

Student sheet

Requirements

You are provided with the following:

hydrated copper(II) sulfate crystals


anhydrous copper(II) sulfate powder
polystyrene cups with lids
250 cm3 or 4003 cm beaker (as appropriate for holding the cup)
stand and clamp
0 C to 50 C glass or digital thermometer
two 25 cm3 measuring cylinders
two weighing bottles
stopwatch
graph paper
stirrer
deionised or distilled water
access to a digital mass balance (measuring to 2 decimal places).

Consider the Hesss Law cycle below


H3
anhydrous copper(II) sulfate + aq hydrated copper(II) sulfate

H1 H2

copper(II) sulfate solution

We can measure accurately by experiment both the values H1 and H2


By applying Hess's Law, we can calculate the value for H3, since the two routes from
anhydrous copper(II) sulfate to copper(II) sulfate solution have the same overall enthalpy
change.

ie H1 = H2 + H3
therefore H3 = H1 H2

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Suggested method

Experiment 1 - Collecting data for the determination of H1

a) Weigh out between 3.90 g and 4.10 g of anhydrous copper(II) sulfate in a dry stoppered
weighing bottle, keeping the stock of solid in a closed container during weighing.
Take care to avoid skin contact. The precise mass should be recorded.
b) Construct a suitable table of results to allow you to record temperatures at minute
intervals up to 15 minutes.
c) Using a measuring cylinder, 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.

d) 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. At
the fifth minute and for every minute up to 15 minutes, stir and record the temperature of
the solution in the polystyrene cup.
e) 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.
f) Use your graph to determine the temperature change at the fourth minute, which
theoretically should have occurred immediately on addition of the solid.

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Experiment 2 - Collecting data for the determination of H2

a) Weigh out between 6.20 g and 6.30 g of hydrated copper(II) sulfate in a dry stoppered
weighing bottle. The precise mass should be recorded.
b) Construct a suitable table of results to allow you to record temperatures at minute intervals
up to 15 minutes as you did for Experiment 1.
c) Using a measuring cylinder, place 24 cm3 of deionised water into a polystyrene cup. Since the
hydrated crystals contain water, the total amount of water will be approximately the same as
in Experiment 1.
d) Repeat the procedure adopted in Experiment 1. Add the copper(II) sulfate crystals to the
water in the polystyrene cup and obtain temperature data for 15 minutes.
e) Plot a graph similar to that in Experiment 1 and determine the temperature change in this
experiment.

Analysing the data and calculating H3

You should be familiar with the expression

Heat change = mass specific heat capacity temperature change

Heat change = m c T

In this experiment, we will ignore heat loss to the surroundings.

The specific heat capacity of the polystyrene cup is negligible when compared to the mass of
water and the aqueous solutions can be considered to have the same specific heat capacity
as water.
(For many aqueous chemical reactions, it can be assumed that the only substance heated is
water).

In each of Experiment 1 and Experiment 2 you need the mass of water, m (in g), which has
changed in temperature. As the density of water can be assumed to be 1 g cm3 the mass can
be directly taken from the volume of water ie 25 g in each case. Do not add on the mass of the
solid used.

You will also need the temperature change, T (in K), from your graph in order to be able to
calculate the heat change.

For water, the specific heat capacity, c = 4.18 J K1 g1 and, so, the value that you obtain for
the heat change in each experiment will be in joules. You can convert this value into
kilojoules by dividing it by 1000.

You can then calculate the enthalpy changes, H1 and H2 , in kJ mol1, using the masses of
the solids used in each experiment.

You need to use the values that you have obtained for H1 and H2 and apply Hess's
Law to calculate H3 in kJ mol1 for the hydration of copper(II) sulfate.

CuSO4(s) + aq CuSO4.5H2O(s)

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A-level Chemistry exemplar for required practical No. 3

Investigation of how the rate of a reaction changes with temperature:


To investigate how the rate of the reaction of sodium thiosulfate with hydrochloric acid
changes as the temperature of the reaction is changed

Student sheet

Sodium thiosulfate reacts with hydrochloric acid according to the equation

Na2S2O3(aq) + 2HCl(aq) 2NaCl(aq) + SO2(g) + S(s)

The reaction produces a precipitate of sulfur. The rate of this reaction can be monitored by
measuring the time taken for a fixed amount of sulfur to be produced. An easy method to do
this is by timing how long it takes for a cross, marked under the bottom of the reaction vessel,
to disappear as it is obscured by the sulfur precipitate.

Dilute hydrochloric acid will be added to sodium thiosulfate solution at different


temperatures in a series of experiments.

This table shows the approximate temperatures for five experiments.

Experiment 1 2 3 4 5

Approximate temperature / C room* ~25 ~35 ~45 ~55**

[* The temperature of the room is likely to be 15 to 18 C]


[** The temperature must not exceed 55 C]

It is not necessary for these exact temperatures to be used although the temperature used
must not exceed 55 C. However, the actual temperature at which each experiment is carried
out must be known as accurately as possible. One way that this can be achieved is to
measure both the initial temperature and the final temperature and then use a mean
temperature when plotting your graph.

Requirements

You are provided with the following:

thermometer
400 cm3 beaker (for use as a water bath)
plastic container with lid
2 glass tubes to hold 1214 cm3 of liquid
0.05 mol dm3 sodium thiosulfate solution
1.0 mol dm3 hydrochloric acid (or 0.5 mol dm3 sulfuric acid)
10 cm3 measuring cylinder
plastic graduated pipette
stopwatch
graph paper.

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Suggested method

a) Add about 10 cm3 of 1 mol dm3 hydrochloric acid (or 0.5 mol dm3 sulfuric(VI) acid) to the
acid tube. Place this tube into the correct hole in the plastic container (ie the one without the
cross under it).
b) Use a measuring cylinder to add 10.0 cm3 of 0.05 mol dm3 sodium thiosulfate solution to the
second tube. Place this tube into the correct hole in the plastic container (ie the one with the
cross under it) and carefully place a thermometer in this tube.
c) Note the start temperature and then add 1 cm3 of the acid to the thiosulfate solution and start
timing.
d) Look down through the tube from above and record the time for the cross to disappear from
view.
e) Record the temperature of the reaction mixture. Pour the cloudy contents of the vial into the
sodium carbonate solution (the stop bath).
f) Now add water from a very hot water tap (or kettle) to the plastic container. The water should
be no hotter than 55 C. Add cold water if necessary.
g) Measure another 10.0 cm3 of 0.05 mol dm3 sodium thiosulfate solution into a clean tube.
Insert this tube into the correct hole in the plastic container (ie the one with the cross under it).
h) Leave the tube to warm up for about 3 minutes.
i) Repeat steps (c) to (e) above.
j) Repeat to obtain results for at least 5 different temperatures in total.

Analysing the data

In these experiments at different temperatures, the concentrations of all the reactants are the
same. You are investigating the time taken to produce the same amount of sulfur at different
temperatures. If you were to plot a graph of the amount of sulfur produced against time, it would
initially be a straight line because the reaction has only just started. Therefore,

the initial rate of reaction = (amount of sulfur)/time


1
so the initial rate of reaction is proportional to 1/time ( ).

AS analysis

calculate the mean temperature of each reaction mixture


1
for each of the five temperatures, calculate to 3 significant figures, where t is the time taken

for the cross to be obscured
1
plot a graph of on the y-axis against average temperature

1
the plotting of the points may be more straightforward if you multiply all of the values for by
t
a common factor (eg 104).

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A-level analysis

The rate constant for a reaction varies with temperature according to the following equation, where
T is the temperature in kelvins:

k = AeEa/RT

taking natural logarithms

Ea 1
ln k = ( ) + ln A
R T

1
In this experiment, the rate constant is directly proportional to . Therefore

1 Ea 1
ln = ( ) + constant
t R T

1 1
plot a graph of ln on the y-axis against
t T
Ea
the graph should be a straight line with gradient so measure the gradient
R
calculate a value for the activation energy and express your answer in kJ mol1
R = 8.31 J K1 mol1

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A-level Chemistry exemplar for required practical No. 4

To carry out tests for the presence of cations and anions and to make accurate
observations

Student sheet

These tests may be split over several lessons.

Requirements

You are provided with the following:

General
test tubes and stoppers
test-tube racks
plastic graduated dropping pipettes
deionised or distilled water
forceps.

Test 1
0.1 mol dm3 barium chloride solution
0.6 mol dm3 sodium hydroxide solution
0.1 mol dm3 calcium bromide solution (or calcium nitrate/potassium bromide)
0.1 mol dm3 magnesium chloride solution
0.1 mol dm3 strontium chloride solution.

Test 2
0.1 mol dm3 barium chloride solution
1.0 mol dm3 sulfuric acid
0.1 mol dm3 calcium bromide solution (or calcium nitrate/potassium bromide)
0.1 mol dm3 magnesium chloride solution
0.1 mol dm3 strontium chloride solution.

Test 3
0.1 mol dm3 ammonium chloride
0.4 mol dm3 sodium hydroxide solution
red litmus paper
kettle
water bath.

Test 4
0.4 mol dm3 sodium hydroxide solution
red litmus paper (or universal indicator paper)
1.0 mol dm3 ammonia solution
petri dish with lid.

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Test 5
0.5 mol dm3 sodium carbonate solution
0.5 mol dm3 hydrochloric acid
0.02 mol dm3 calcium hydroxide solution (limewater).

Test 6
0.1 mol dm3 barium chloride solution
0.1 mol dm3 magnesium sulfate solution.

Test 7
0.1 mol dm3 potassium chloride solution
0.1 mol dm3 potassium bromide solution
0.1 mol dm3 potassium iodide solution
0.1 mol dm3 nitric acid
0.05 mol dm3 silver nitrate solution
concentrated ammonia solution
2.0 mol dm3 ammonia solution

Test 8
potassium chloride solid
potassium bromide solid
potassium iodide solid
0.1 mol dm3 lead nitrate solution (or lead ethanoate solution)
blue litmus paper
filter paper
small spatula.
concentrated sulfuric acid in dropping bottles
0.5 mol dm3 acidified potassium dichromate(VI) solution

Suggested method

In every case, you should present all of your observations in a neat table. The presentation of
a clearly organised record of your observations is an important skill which you will be expected
to demonstrate.

Tests 1 and 2: Testing for Group 2 metal cations

Test 1 dilute sodium hydroxide

a) Place about 10 drops of 0.1 mol dm3 barium chloride in a clean test tube. Add about 10
drops of 0.6 mol dm3 sodium hydroxide solution, mixing well.

b) Now continue to add this sodium hydroxide solution, dropwise with gentle shaking, until in
excess.

The test tube should not be more than half full. Once completed, dispose of the contents by
placing the test tube in a bowl of water.

c) Repeat this test with the calcium bromide, magnesium chloride and
strontium chloride.

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Test 2 dilute sulfuric acid

a) Place about 10 drops of 0.1 mol dm3 barium chloride in a clean test tube. Add about 10
drops of 1.0 mol dm3 sulfuric acid, mixing well.

b) Now continue to add this dilute sulfuric acid, dropwise with gentle shaking, until in excess.

The test tube should not be more than half full. Once completed, dispose of the contents by
placing the test tube in a bowl of water.

c) Repeat this test with the calcium bromide, magnesium chloride and strontium chloride.

Test 3: Testing for ammonium ions

a) Place about 10 drops of 0.1 mol dm3 ammonium chloride in a clean test tube. Add about
10 drops of 0.4 mol dm3 sodium hydroxide solution. Shake the mixture.

b) Warm the mixture in the test tube gently using a water bath.

c) Test the fumes released from the mixture by using forceps to hold a piece of damp red
litmus paper in the mouth of the test tube.

d) Dispose of the contents by using the previous method.

Tests 4, 5, and 7: Tests for anions in aqueous solution

Test 4: Test for hydroxide ions in aqueous solution

a) Test about 1 cm3 of 0.4 mol dm3 sodium hydroxide solution in a test tube with red litmus
paper or universal indicator paper.

b) Record your observations. Dispose of the test tube contents.

This approach can also be used to test for the alkaline gas, ammonia, which forms
hydroxide ions when it comes into contact with water.

c) Take 5 drops of 1 mol dm3 ammonia solution and place on a filter paper and place inside a
petri dish with lid. Dampen a piece of red litmus paper with deionised water and place on
the other side of the petri dish. Replace the lid and observe over a few minutes.

d) Record your observations.

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Test 5: Test for carbonate ions in aqueous solution

a) Have about 2 cm3 of calcium hydroxide (limewater) ready in a test tube.

b) To about 3 cm3 of 0.5 mol dm3 sodium carbonate solution in a test tube, add an equal
volume of 1.0 mol dm-3 dilute hydrochloric acid.

c) Immediately put in delivery tube with open end into the limewater test tube. Make sure that
the end of the tube is below the level of the liquid.

d) Record your observations. Dispose of the test tube contents.

Test 6: Test for sulfate ions in aqueous solution

a) To about 1 cm3 of 0.1 mol dm 3 magnesium sulfate solution in a test tube, add an
equal volume of dilute hydrochloric acid followed by an equal volume of 0.1 mol dm3
barium chloride solution.

b) Record your observations. Dispose of the test tube contents.

Test 7: Test for halide ions in aqueous solution

Test for chloride, bromide and iodide ions in aqueous solution

a) Place about 10 drops of 0.1 mol dm3 potassium chloride in a clean test tube. Add
about 5 drops of dilute nitric acid. Shake well.

b) To the solution add another 10 drops of 0.05 mol dm3 silver nitrate solution.

c) Then add an excess of 2 mol dm3 ammonia solution and shake to mix thoroughly.
Dispose of the tube contents

d) Repeat steps a) and b), but this time add an excess of concentrated ammonia solution,
working in a fume cupboard. Dispose of the tube contents

e) Repeat steps a) to d) but using potassium bromide and then potassium iodide instead
of potassium chloride.

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Test 8: Test for halide ions in solid salts using concentrated sulfuric acid

Test for chloride, bromide and iodide ions in solid potassium halides

Note: Gloves must be worn for this procedure

These experiments must be done in a fume hood

a) Place a small spatula of solid potassium chloride in a clean dry test tube.

b) Slowly add a few (2 to 5) drops of concentrated sulfuric acid.

c) Record what happens.

d) Test the gas evolved with moist blue litmus paper, taking care that the paper does not touch
the sides of the test tube.

e) Repeat this experiment with solid potassium bromide, but this time test the gas produced
using a narrow strip of filter paper that has been dipped in acidified potassium dichromate
solution.

f) Repeat this experiment with potassium iodide, but this time test the gas produced using a
narrow strip of filter paper that has been dipped in lead nitrate solution.

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Sample results

Test 1

Calcium Magnesium Strontium


Barium chloride
bromide chloride chloride
colourless colourless colourless colourless
Initial
solution solution solution solution
10 drops of
colourless slight white slight white slight white
0.6 mol dm3
solution precipitate precipitate precipitate
NaOH
colourless slight white slight white
Excess NaOH white precipitate
solution precipitate precipitate

Test 2

Calcium Magnesium Strontium


Barium chloride
bromide chloride chloride
10 drops of
slight white slight white
1.0 mol dm3 white precipitate white precipitate
precipitate precipitate
H2SO4
slight white colourless
Excess H2SO4 white precipitate white precipitate
precipitate solution

Test 3

Ammonium chloride + sodium hydroxide Damp red litmus paper = blue

Test 4

Sodium hydroxide Damp red litmus paper = blue


Ammonia solution Damp red litmus paper = blue

Test 5

Limewater - colourless solution to cloudy

Test 6

Test of sulfate ions white precipitate forms

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Test 7

+ HNO3 + 2 M NH3 + concentrated NH3


Potassium
white precipitate colourless solution colourless solution
chloride
Potassium
cream precipitate cream precipitate colourless solution
bromide
Potassium
yellow precipitate yellow precipitate yellow precipitate
iodide

Test 8

Concentrated sulfuric acid Result of paper test


Potassium
effervescence red
chloride
effervescence
Potassium
brown gas produced
bromide
solution turns deep brown/red
solution goes red/brown
Potassium
immediately turns black/grey
iodide
brown gas produced

Photographs of an exemplar set-up of this practical can be found in our mini-guide for each
practical, which are available on our practical resources page

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A-level Chemistry exemplar for required practical No. 5 alternative a

Distillation of a product from a reaction:


To prepare cyclohexene by the dehydration of cyclohexanol and to distil the
cyclohexene from the reaction mixture

Student sheet

Requirements

You are provided with the following:

semi-micro distillation apparatus OR Quickfit apparatus fitted with a thermometer and


collection vessel
concentrated phosphoric acid
cyclohexanol
protective gloves
stand and clamp
micro-burner
10 cm3 measuring cylinder
25 cm3 measuring cylinder
anti-bumping granules
separating funnel
250 cm3 beaker
100 cm3 conical flask fitted with a stopper
saturated sodium chloride solution
anhydrous calcium chloride (or molecular sieves)
plastic graduated dropping pipette
acidified potassium manganate(VII) solution
sample container
access to a digital mass balance (reading to 0.1 g).

Suggested method

The dehydration of cyclohexanol to form cyclohexene

This experiment must be carried out in a fume cupboard.

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 semi-micro 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 cm3 of saturated sodium chloride
solution. Shake the mixture and allow the two layers to separate.

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e) Carefully run off the lower layer into a beaker (for later disposal) 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 (or use molecular sieves (4A), if available) 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 and determine the
percentage yield of your product. You should assume that the whole of the dry distillate is
cyclohexene.
i) Test the distillate as described below, to confirm that it contains an alkene.

A test on the product to confirm the formation of an alkene

a) To approximately 1 cm3 of the distillate in a test tube, add an equal volume of acidified
potassium manganate(VII) solution. Shake the contents of the test tube well.
b) Record your observations.

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A-level Chemistry exemplar for required practical No. 5 alternative b

Distillation of a product from a reaction:


To prepare ethanal by the oxidation of ethanol and to distil the ethanal from the reaction
mixture

Student sheet

Requirements

You are provided with the following:

simple distillation apparatus OR Quickfit apparatus


acidified sodium dichromate(VI)
protective gloves
stand and clamp
10 cm3 measuring cylinder
25 cm3 measuring cylinder
anti-bumping granules
test tube
thermometer
two 250 cm3 beakers
ethanol
teat pipette
0.05 mol dm3 silver nitrate solution
2 mol dm3 dilute ammonia solution
2 mol dm3 sodium hydroxide solution
1 mol dm3 dilute sulfuric acid.

Suggested method

The oxidation of ethanol to ethanal

a) Using a 25 cm3 measuring cylinder, carefully measure out 12 cm3 of the solution of acidified
sodium dichromate(VI). Pour this oxidising agent into a boiling tube. You should wear
protective gloves when handling the corrosive oxidising agent.
b) Cool the boiling tube in cold water in a beaker.
c) Using a 10 cm3 measuring cylinder, carefully measure out 2 cm3 of ethanol.
d) Using a teat pipette, slowly add the 2 cm3 of ethanol dropwise, to the oxidising agent in the
cooled boiling tube (immersed in cold water in a beaker), shaking the tube gently to mix the
contents.
e) After the addition of ethanol, add a few anti-bumping granules to the boiling tube and attach to
it a bung fitted with a right-angled glass delivery tube.
f) Clamp the boiling tube at about 45 in a beaker of water. Heat this beaker of water gently
and slowly distil off approximately 5 cm3 of liquid distillate into a test tube which is immersed
in cold water in a beaker. Keep the test tube cool to avoid loss of the volatile ethanal.
g) Carry out the test described below on the distillate to confirm that ethanal has been formed
in this reaction.

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Test on the distillate to confirm the formation of ethanal

Tollens silver mirror test:

a) Prepare a sample of Tollens reagent by adding 5 drops of sodium hydroxide solution to


2 cm3 of silver nitrate solution in a test tube.
b) To this test tube add just enough dilute ammonia solution to dissolve the brown
precipitate completely.
c) Using a beaker of hot water (5060 C), gently warm approximately 5 cm3 of this test
reagent in a test tube.
d) Add 10 drops of the distillate containing ethanal to the warmed Tollens reagent in the test
tube. Wait a few minutes and note what happens. You should have produced a silver
mirror on the walls of the tube.

Make sure that you dispose of the Tollens reagent thoroughly by rinsing it away with
plenty of water and then rinsing any glassware that has contained the reagent with a little
dilute sulfuric acid when you are finished.

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A-level Chemistry exemplar for required practical No. 6

Tests for alcohol, aldehyde, alkene and carboxylic acid:


To carry out tests for the presence of organic functional groups and to make accurate
observations

Student sheet

Requirements

You are provided with the following:

ethanol
ethanal or propanal
cyclohexene
1-bromobutane
dilute ethanoic acid
small pieces of metallic sodium under petroleum ether
(a beaker of ethanol should be available for safe disposal of any excess sodium)
Fehlings solution A
Fehlings solution B
bromine water
sodium carbonate solution
sodium hydrogencarbonate solid
sodium hydroxide solution
silver nitrate solution (0.05 mol dm3)
dilute nitric acid
250 cm3 beaker
anti-bumping granules
test tubes, boiling tubes and a test-tube holder
thermometer
plastic graduated dropping pipettes.

Suggested method

This experiment is divided into five parts.

In every case, you should present all of your observations in a neat table. The presentation of
a clearly organised record of your observations is an important skill which you will be expected
to demonstrate as part of this assessment.

Part 1 A test for an alcohol

a) To about 1 cm3 of ethanol in a dry test tube, add a small piece of metallic sodium.
b) Record your observations.
c) Make sure that you dispose safely of any excess sodium using the beaker of ethanol
provided.

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Part 2 A test for an aldehyde using Fehlings solution.

a) In a clean test tube mix together equal volumes of Fehling's solution A and Fehling's
solution B. The resultant Fehling's test reagent should be a clear dark blue solution.
b) Add 5 drops of this test reagent to about 1 cm3 of sodium carbonate solution in a test
tube containing a few anti-bumping granules and then add about 1 cm3 of ethanal
(or propanal) to this same test tube.
c) Warm the test tube gently for approximately 2 minutes in a beaker half- filled with hot
water and then gradually bring the beaker of water to boiling and maintain this
temperature for a few minutes.
d) Using the test tube holder, carefully lift the test tube out of the boiling water and allow its
contents to stand for several minutes. Record your observations.

Part 3 A test for an alkene (a test for unsaturation)

a) To about 2 drops of cyclohexene in a test tube, add about 1 cm3 of bromine water and shake
the contents of the tube vigorously from side to side.
b) Record your observations.

Part 4 A test for a carboxylic acid

a) Place one small spatula measure of solid sodium hydrogencarbonate in a boiling tube
tube and add to it about 2 cm3 of dilute ethanoic acid.
b) Record your observations.

Part 5 A test for a halogenoalkane

a) Using a teat pipette, add 5 drops of 1-bromobutane to about 1 cm3 of sodium hydroxide
solution in a test tube. Warm the contents of the test tube for a few minutes, by placing it
into a beaker filled with hot water at approximately 60 C.
b) Acidify the contents of the test tube by adding 2 cm3 of dilute nitric acid and then add about
1 cm3 of silver nitrate solution.
c) Record your observations.

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A-level Chemistry exemplar for required practical No. 7 part a

Measuring the rate of reaction by an initial rate method:


An Iodine Clock experiment: To investigate the reaction of iodide(V) ions with hydrogen
peroxide in acidic solution and to determine the order of the reaction with respect to
iodide ions.

Student sheet

The Iodine Clock experiment can be used to determine the effect of a change in concentration of
iodide ions on the reaction between hydrogen peroxide and iodide ions.

Introduction

Hydrogen peroxide reacts with iodide ions to form iodine and the thiosulfate ion immediately reacts
with iodine as shown below.

H2O2(aq) + 2H+(aq) + 2I (aq) I2(aq) + 2H2O(l)

2S2O32(aq) + I2(aq) 2I (aq) + S4O62(aq)

When the I2 produced has reacted with all of the limited amount of thiosulfate ions present, excess
I2 remains in solution. Reaction with the starch then forms a dark blue-black colour.

By varying the concentration of I, you can determine the order of reaction with respect to I ions.

Requirements

You are provided with the following:

0.25 mol dm3 dilute sulfuric acid


0.10 mol dm3 potassium iodide solution
0.05 mol dm3 sodium thiosulfate solution (in a shared burette)
0.10 mol dm3 hydrogen peroxide solution (in a shared burette)
starch solution
50 cm3 burette
funnel suitable for filling a burette
stand and clamp
white tile
plastic dropping pipette
25 cm3 measuring cylinder
50 cm3 measuring cylinder
100 cm3 beaker
250 cm3 beaker
stirrer
stopwatch
paper towels to dry beakers
plentiful supply of distilled or deionised water.

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Suggested method

Experiment 1

a) Rinse a 50 cm3 burette with potassium iodide solution. Fill the burette with potassium iodide
solution.
b) Transfer 10.0 cm3 of hydrogen peroxide solution from the shared burette provided to a clean,
dry 100 cm3 beaker. You will use this in step (h).
c) Use a 50 cm3 measuring cylinder to add 25 cm3 of sulfuric acid to a clean, dry 250 cm3
beaker.
d) Use a 25 cm3 measuring cylinder to add 20 cm3 of distilled or deionised water into the 250 cm3
beaker.
e) Use a plastic dropping pipette to add about 1 cm3 of starch solution to this beaker.
f) Use your burette to add 5.0 cm3 of potassium iodide solution to the mixture in the 250 cm3
beaker.
g) Finally, add 5.0 cm3 of sodium thiosulfate solution from the shared burette provided to the
mixture in the 250 cm3 beaker. Make sure this sodium thiosulfate solution is added last.
h) Stir the mixture in the 250 cm3 beaker. Pour the hydrogen peroxide solution from the 100 cm3
beaker into the 250 cm3 beaker and immediately start the timer. Stir the mixture.
i) Stop the timer when the mixture in the 250 cm3 beaker turns blue-black. Record the time to an
appropriate precision in a table of your own design. This experiment could take several
minutes.
j) Rinse the 250 cm3 beaker with distilled or deionised water and dry it with a paper towel.

Experiments 25
k) Repeat steps (b) to (j) in four further experiments using the volumes shown in the following
table.

Volume in
Volumes of solutions added to 250 cm beaker 3 100 cm3
beaker
Sulfuric Potassium Hydrogen
Sodium
acid iodide peroxide
Experiment Starch Water thiosulfate
0.25 M 0.10 M 0.10 M
/ cm3 / cm3 0.05 M / cm3
/ cm3 / cm3 / cm3
1 25 1 20 5.0 5.0 10.0
2 25 1 15 10.0 5.0 10.0
3 25 1 10 15.0 5.0 10.0
4 25 1 5 20.0 5.0 10.0
5 25 1 0 25.0 5.0 10.0

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A-level Chemistry exemplar for required practical No. 7 part b

Measuring the rate of reaction by a continuous monitoring method:


The reaction between magnesium and hydrochloric acid

Student sheet

Requirements

You are provided with the following:

magnesium ribbon
0.8 mol dm3 hydrochloric acid
50 cm3 measuring cylinder
100 cm3 conical flask
rubber bung and delivery tube to fit conical flask
100 cm3 gas syringe OR trough/plastic container with 100 cm3 measuring cylinder
stand, boss and clamp
stopwatch or timer
distilled or deionised water.

Suggested method

a) Measure 50 cm3 of the 0.8 mol dm3 hydrochloric acid and add to conical flask.
b) Set up the gas syringe in the stand (or alternative gas collection method as shown by your
teacher).

Using a gas syringe

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Using a trough

c) Add one 6 cm strip of magnesium ribbon to the conical flask, place the bung firmly into the top
of the flask and start the timer.
d) Record the volume of hydrogen gas collected every 15 seconds for 2.5 minutes.

Repeat steps (a) to (d) using 0.4 mol dm3 hydrochloric acid, made by mixing 25 cm3 of the
0.8 mol dm3 hydrochloric acid with 25 cm3 of distilled or deionised water.

Analysis

a) Plot a graph of volume of hydrogen produced on the y-axis against time in seconds for each
hydrochloric acid concentration. Draw a line of best fit.
b) Draw a tangent to each line of best fit at time, t = 0 s
c) Calculate the gradient of each tangent in order to deduce the rate of each reaction.
d) Compare the two rate values obtained.

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A-level Chemistry exemplar for required practical No. 8

Measuring the EMF of an electrochemical cell

Student sheet

Requirements

You are provided with the following:

pieces of copper and zinc foil (about 2 cm 5 cm)


propanone
2.0 mol dm3 NaCl solution
1.0 mol dm3 CuSO4 solution
1.0 mol dm3 ZnSO4 solution
emery paper or fine grade sandpaper
two 100 cm3 beakers
plastic or glass U-tube
cotton wool soaked in sodium chloride solution
voltmeter (digital or high impedance)
two electrical leads with connectors for the voltmeter at one end and crocodile clips at the
other end
samples of metals.

Suggested method for setting up a standard cell

a) Clean a piece of copper and a piece of zinc using emery paper or fine grade sandpaper.
b) Degrease the metal using some cotton wool and propanone.
c) Place the copper into a 100 cm3 beaker with about 50 cm3 of 1 mol dm3 CuSO4 solution.
d) Place the zinc into a 100 cm3 beaker with about 50 cm3 of 1 mol dm3 ZnSO4 solution.
e) Lightly plug one end of the plastic tube with cotton wool and fill the tube with the solution of
2 mol dm3 NaCl provided.
f) Plug the free end of the tube with cotton wool which has been soaked in sodium chloride. Join
the two beakers with the inverted U-tube so that the plugged ends are in the separate beakers.
g) Connect the Cu(s)|Cu2+(aq) and Zn(s)|Zn2+(aq) half-cells by connecting the metals (using the
crocodile clips and leads provided) provided to the voltmeter and read off the voltage.

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Suggested method for measuring comparative electrode potentials of different metals

a) Clean a piece of copper using emery paper or fine grade sandpaper.


b) Connect the positive terminal of the voltmeter to the copper using a crocodile clip and one of
the leads.
c) Cut a piece of filter paper to about the same area as the copper, moisten the filter paper with
the sodium chloride solution and place on top of the copper.
d) Connect the second lead to the voltmeter and use the crocodile clip on the other end of the
lead to grip a piece of another metal.
e) Hold the metal against the filter paper and note the voltage reading and sign.

f) Repeat steps (d) and (e) with different metals and record your results in a table.
g) Write the conventional representation for each of the cells that you have constructed
h) Suggest how you could construct the cell with the largest EMF from the metals provided.

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A-level Chemistry exemplar for required practical No. 9

To investigate how pH changes when a weak acid reacts with a strong base:
Investigation of how the pH of a solution of ethanoic acid changes as sodium
hydroxide solution is added.
Student sheet

This experiment investigates how the pH of a solution of ethanoic acid changes as sodium
hydroxide solution is added.

The results are plotted in a graph which shows the general pattern of how the pH changes
when a weak acid reacts with a strong base.

It is necessary initially to calibrate a pH meter so as to give accurate pH values for each pH


reading.

Requirements

You are provided with the following:

two 50 cm3 burettes


two funnels
100 cm3 beaker
deionised (or distilled) water in a wash bottle
stand and clamp
pH meter/probe
0.100 mol dm3 sodium hydroxide solution
0.100 mol dm3 ethanoic acid solution
standard pH buffer solutions at pH 4.00, 7.00 and 9.20
stirring rod
graph paper.

Suggested method

Part 1 Calibrate the pH meter

a) Rinse the pH probe thoroughly with deionised water, and shake it gently to remove excess
water. Place the probe in the standard pH 7.00 buffer solution provided, ensuring that the bulb
is fully immersed. Record the pH reading in a suitable table.
b) Repeat this process using the standard pH 4.00 and 9.20 buffer solutions. Rinse the pH probe
thoroughly with deionised water before taking each reading. Record the pH readings in your
table.
c) Plot a graph of your recorded pH reading (x-axis) against the pH of the buffer solution. Your
graph may be a straight line or a curve.This calibration graph will be used in the next part of
the experiment to convert pH readings into more accurate pH values.

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Part 2 The measurement of the pH of the mixture of acid and alkali

a) Rinse a burette with the 0.100 mol dm3 solution of ethanoic acid provided and then fill the
burette with this solution, ensuring that it is filled below the tap. Label this burette so that you
do not confuse it with the second burette.
b) Use the burette to transfer exactly 20.0 cm3 of ethanoic acid to a clean 100 cm3 beaker.
c) Rinse a second burette with the 0.100 mol dm3 NaOH solution provided and then fill this
second burette with this solution, ensuring that it is filled below the tap.
d) Rinse the pH probe with distilled or deionised water and clamp it so that its bulb is fully
immersed in the ethanoic acid solution in the beaker. Use a rod to stir the solution gently and
record the pH reading in a suitable table.

e) Using the second burette, add exactly 2.0 cm3 of the NaOH solution to the beaker containing
the ethanoic acid. Stir the mixture gently with the glass rod and measure the pH of the
mixture. Record the pH reading.
Add the NaOH solution in 2.0 cm3 portions from the second burette to the ethanoic acid in the
beaker until 18 cm3 of the NaOH solution have been added. Take a pH reading after each
addition of NaOH solution, and in each case record the pH reading in your table.
Then add the NaOH solution in 0.20 cm3 portions until 22.0 cm3 is reached.
Then add the NaOH solution in 2.0 cm3 portions again until 40 cm3 have been added.
f) Rinse the pH probe with distilled or deionised water when you have taken all of your readings.

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Analysing the data

a) Use your calibration graph from Part 1 to adjust, as appropriate, the pH readings obtained in
your experiment in Part 2. These corrected pH values should be entered into a new column in
your table of results.
b) Plot a graph of the corrected pH values from Part 2 (y-axis) against volume of
sodium hydroxide solution added.
c) Join the points in the most appropriate way.
d) Comment on the shape of the curve.

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A-level Chemistry exemplar for required practical No. 10 part a

Preparation of an organic solid and a test of its purity:


To prepare a sample of aspirin

Student sheet

Aspirin is prepared by the acylation of salicylic acid (2-hydroxybenzenecarboxylic acid)


using ethanoic anhydride as the acylating agent.
The reaction can be represented as follows.

HOOCC6H4OH + (CH3CO)2O HOOCC6H4OCOCH3 + CH3COOH


salicylic acid ethanoic aspirin ethanoic acid
anhydride

Aspirin (2-ethanoylhydroxybenzenecarboxylic acid) is an antipyretic drug (reduces fever by


lowering body temperature) and an analgesic (relieves pain).

Aspirin does not react in the acidic conditions in the stomach, but is hydrolysed in the
alkaline conditions found in the intestines to produce ethanoate ions and salicylate
(2-hydroxybenzencarboxylate) ions. Salicylates lower the body temperature of feverish
patients and have a mild analgesic effect relieving headaches and other pain. The toxic dose
is relatively high, but symptoms of poisoning can occur with quite small quantities.

Requirements

You are provided with the following:

Part 1

salicylic (2-hydroxybenzenecarboxylic) acid


100 cm3 conical flask
10 cm3 measuring cylinder
ethanoic anhydride
concentrated sulfuric acid in a dropping bottle
400 cm3 beaker
tripod, gauze and Bunsen burner
thermometer
250 cm3 beaker
reduced pressure filtration apparatus
filter paper
stirring rod
deionised or distilled water in a wash bottle
spatula.

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Part 2

25 cm3 measuring cylinder


boiling tube
ethanol
thermometer
deionised or distilled water in a wash bottle
250 cm3 beaker
100 cm3 conical flask
stirring rod
kettle
access to a digital mass balance (reading to 2 decimal places).

Suggested method
Part 1 Preparation

a) Weigh out approximately 6.00 g of salicylic acid directly into a 100 cm3 conical flask.
b) Record the mass of salicylic acid used.
c) Using a 10 cm3 measuring cylinder, add 10 cm3 of ethanoic anhydride to the flask and swirl
the contents.
d) Add 5 drops of concentrated sulfuric acid to the flask and swirl the mixture in the flask for
a few minutes to ensure thorough mixing.
e) Warm the flask for about 20 minutes in a 400 cm3 beaker of hot water at approximately
60 C. The temperature in the flask should not be allowed to rise above 65 C.

f) Allow the flask to cool and pour its contents into 75 cm3 of water in a beaker, stirring well
to precipitate the solid.
g) Filter off the aspirin under reduced pressure, avoiding skin contact.

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h) Collect the crude aspirin on a double thickness of filter paper and allow it to dry

Part 2 Purification

a) Using a 25 cm3 measuring cylinder, measure out 15 cm3 of ethanol into a boiling tube.
b) Prepare a beaker half-filled with hot water at a temperature of approximately 75 C. The
safest way to do this is to use a kettle of boiling water and add water from the kettle to cold
water in the beaker until the temperature is at approximately 75 C.
NB The boiling point of ethanol is 78 C and the temperature of the water in the beaker should
not be allowed to go above this.
c) Use a spatula to add the crude aspirin to the boiling tube and place the tube in the
beaker of hot water. Do not scrape the filter paper.
d) Stir the contents of the boiling tube until all of the aspirin dissolves into the ethanol.
e) Pour the hot solution containing dissolved aspirin into approximately 40 cm3 of water in
a 100 cm3 conical flask. If a solid separates at this stage, gently warm the contents of
the flask in the water bath until solution is complete. You should avoid prolonged
heating, since this will decompose the aspirin.
f) Allow the conical flask to cool slowly and white needles of aspirin should separate.
g) If no crystals have formed after the solution has cooled to room temperature, you may
need to scratch the insides of the flask with a glass stirring rod to obtain crystals. Cool the
whole mixture in an ice bath.
h) Filter off the purified solid under reduced pressure and allow it to dry on filter paper.
i) Record the mass of the dry purified solid.

Analysing the effectiveness of this method of preparation of aspirin

a) Calculate the theoretical yield of aspirin which should be formed from 6.00 g of salicylic
acid.
b) Calculate the percentage yield of aspirin from your experiment and comment on the
reasons for the losses that have occurred during the preparation and the purification of
the solid.
c) Calculate the atom economy for the preparation of aspirin by this method.
d) Consider the reasons why the alternative preparative method which uses ethanoyl
chloride rather than ethanoic anhydride, is not favoured by industry even though this
alternative method has a higher atom economy.

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To test the purity of an organic solid by measuring its melting point

The purity of an organic solid can be determined in part by measuring its melting point and
comparing the value with the known Data Book value of the melting point for that compound.
A pure dry solid will melt at a precise temperature whereas an impure solid will melt over a
range of temperatures which are lower than the melting point of the pure solid.

Melting point apparatus varies in type from the most simple using an oil bath to the more
sophisticated electrothermal devices. In every case, the same general principle applies that
the heating of a small quantity of the solid in a thin-walled melting point tube should be
undertaken slowly and with care. When melting occurs, the solid should collapse into a liquid
without any change in temperature and the way in which this occurs can give a clue to the
purity of the solid. Repeat measurements should be taken with further samples of the
organic solid to verify the reliability of the value obtained.

The method will not work if the solid decomposes on heating.

Requirements

You are provided with the following:

pure benzenecarboxylic acid


other pure organic solids as desired by the centre
thermometer (0 C to 250 C range)
melting point apparatus to include either:
an electrothermal melting point apparatus or oil bath (Thiele tube or small beaker half-
filled with mineral oil)
tripod, gauze and Bunsen burner
rubber ring to attach melting point tube to thermometer (if needed)
melting point tubes
watch glass
spatula.

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Suggested method

a) Powder a sample of the organic solid by crushing it gently with a spatula onto the surface
of a filter paper.
b) Fill three melting point tubes with the organic solid to a depth of approximately 0.5 cm.
c) Set up the melting point apparatus provided and mount one of the melting point tubes
ready for taking a measurement.

d) Heat the apparatus gently and observe the temperature at which the solid collapses
into a liquid. The melting point will be in the range 100 C to 200 C.
e) Allow the melting point apparatus to cool and repeat the measurement of the melting
point of the solid with the other two samples. If the first reading is taken as an
approximate value, then the subsequent heating of the other two samples can be done
much more slowly as this approximate value is approached.
f) On the basis of the three measurements that you have taken, record the melting
point of the organic solid.
g) Ask your teacher for the Data Book value of the melting point for the solid that you
have tested and compare this value with your own.

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A-level Chemistry exemplar for required practical No. 10 part b
Preparation of a pure organic liquid:
The preparation of ethyl ethanoate

Student sheet

An ester is a chemical compound that is formed when an organic acid reacts with an alcohol.
Esters frequently have distinctive odours and are naturally occurring flavour and fragrance
chemicals in many fruits and plants. In this practical, the ester ethyl ethanoate is prepared and
purified by distillation.

Requirements

Stage 1: Preparation of ethyl ethanoate

12 cm3 glacial ethanoic acid


10 cm3 ethanol
15 drops concentrated sulfuric acid
anti-bumping granules
disposable dropping pipette
10 cm3 measuring cylinder
25 cm3 measuring cylinder
250 cm3 beaker
50 cm3 pear-shaped flask
condenser (with rubber tubing)
clamp stand
clamps and bosses
heatproof mat
Bunsen burner
tripod and gauze.

Stage 2: Isolation of ethyl ethanoate

4.5 g sodium carbonate


15 cm3 distilled or deionised water
100 cm3 beaker
50 cm3 beaker
separating funnel and stopper
anhydrous sodium sulfate
boiling tube
50 cm3 pear-shaped flask.

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Stage 3: Purification of the ethyl ethanoate

thermometer (0100 oC) and adapter


three-way adapter
condenser (with rubber tubing)
receiver adapter
anti-bumping granules
joint clips
250 cm3 beaker
clamp stand
clamps and bosses
heatproof mat
Bunsen burner
tripod and gauze
access to a balance.

Suggested method

Stage 1: Preparation of ethyl ethanoate

a) Put a few anti-bumping granules in a 50 cm3 pear-shaped flask.


b) In a fume-cupboard, add 10 cm3 ethanol, 12 cm3 glacial ethanoic acid and 15 drops of
concentrated sulfuric acid to the flask.
c) Place a 250 cm3 beaker containing some water on a tripod and gauze over a Bunsen burner.
d) Clamp the pear-shaped flask in the beaker of water so that the reaction mixture is below the
water line.
e) Add a condenser so that it is set up for heating with reflux. Clamp the condenser. Do not insert
a stopper.
f) Light the Bunsen burner to heat the hot water bath. Raise the temperature of the hot water
until the mixture in the flask is gently boiling. Continue the gentle boil of the reaction mixture
for about 15 minutes. Turn off the Bunsen burner and cool the mixture by removing the hot
water bath.

Stage 2: Isolation of ethyl ethanoate

g) Prepare a saturated solution of sodium carbonate by combining 4.5 g of sodium carbonate


with 15 cm3 of distilled water in a 100 cm3 beaker.
h) In a fume cupboard, transfer the reaction mixture from the pear-shaped flask to the beaker and
stir.
i) Transfer the mixture to a separating funnel. Stopper it and turn it upside down gently and then
open the stopcock to vent the system. Invert at least 1520 times, opening the stopcock each
time.
j) Allow the two layers to separate. Ethyl ethanoate is less dense than water, therefore the top
layer is ethyl ethanoate.
k) Remove the stopper, open the stopcock and slowly drain off the waste aqueous layer into a
50 cm3 waste beaker, then close the stopcock.
l) Transfer the remaining ethyl ethanoate into a dry boiling tube containing about 1 g of
anhydrous sodium sulfate. Agitate the tube so that any water is absorbed into the anhydrous
solid.
m) Decant the ethyl ethanoate into a clean, dry 50 cm3 pear-shaped flask.

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Stage 3: Purification of the ethyl ethanoate

n) Add a few anti-bumping granules to the pear-shaped flask.


o) Set up the apparatus for distillation.
p) Place the flask in the 250 cm3 beaker and clamp it so the crude ethyl ethanoate is below the
water line.
q) Weigh a clean, dry 100 cm3 conical flask on an analytical balance. Record the mass in your
Data Table.
r) Place the conical flask under the receiver.
s) Light the Bunsen burner and heat the flask in the hot water bath. Heat until the ethyl ethanoate
is gently boiling.
t) As the ethyl ethanoate vapours start to carry over and condense, record the temperature of
the vapours in a suitable table. Record this temperature at the beginning and end of the
distillation.
u) Distil the ethyl ethanoate until no more distillate comes over. There should be some liquid
remaining in the round-bottom flask. Never distil to dryness.
v) Turn off the Bunsen burner.
w) Reweigh the conical flask with the distilled ethyl ethanoate.

Stage 4: Yield calculation

Which is the limiting reagent - ethanoic acid or ethanol?

What is the percentage yield from the limiting reagent?

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A-level Chemistry exemplar for required practical No. 11

Carry out simple test-tube reactions to identify transition metal ions in aqueous solution:
An investigation of some transition metal compounds

Most transition metal compounds are coloured. Some of them are used as dyes and pigments.
A dye is a soluble coloured compound. A pigment is an insoluble coloured compound. Both dyes
and pigments have to be resistant to chemical change.

Four solutions, labelled P, Q, R and S, have been provided by a supplier as possible dyes.

You will carry out tests on these solutions.


You will record what you observe for each test.
You should ensure that you record observations on dropwise addition, on addition to excess
and on standing.
Where no visible change is observed, write no visible change.

In this task, you are not required to identify any of the solutions or any of the reaction products.

Requirements

You are provided with the following:

four solutions labelled Solution P, Solution Q, Solution R and Solution S


sodium hydroxide solution
sodium carbonate solution
silver nitrate solution
12 test tubes
7 dropping pipettes
test-tube rack
250 cm3 beaker
access to hot water
plentiful supply of distilled or deionised water.

Suggested method

Test 1(a)

a) Place about 10 drops of solution P in a test tube.


b) Add sodium hydroxide solution, dropwise with gentle shaking, until in excess.
c) Do not discard this mixture.
d) Repeat this test with solution Q and then solution R and then solution S.

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Test 1(b)

a) Half fill a 250 cm3 beaker with the freshly boiled water provided.
b) Allow the four test tubes containing the mixtures from Test 1(a) to stand in the beaker of hot
water for about 10 minutes.
c) While you are waiting, begin Test 2.

Test 2

a) Place about 10 drops of sodium carbonate solution in a test tube.


b) Add about 10 drops of solution P and shake the mixture gently.
c) Repeat this procedure with solution Q and then with solution R and then solution S.

Test 3

a) Place about 10 drops of solution P in a test tube.


b) Add about 10 drops of silver nitrate solution and shake the mixture gently.
c) Repeat this procedure with solution Q and then with solution R and then solution S.
d) Allow the four test tubes to stand for about 10 minutes.

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Spare supplies of all reagents specified in these notes should be available for student use (if
needed).

Sample results

Test 1(a) and (b)

P Q R S
pale green
Initial blue solution yellow solution light blue solution
solution
orange/brown deep blue grey/green
Add NaOH white precipitate
precipitate precipitate precipitate
On standing in
green solution no visible change no visible change no visible change
hot water

Test 2

P Q R S
Addition of orange/brown
blue/green grey/green
sodium grey precipitate precipitate and
precipitate precipitate
carbonate effervescence

Test 3

P Q R S
Addition of light brown
no visible change white precipitate white precipitate
silver nitrate precipitate

Photographs of an exemplar set-up of this practical can be found in our mini-guide for each
practical, which are available on our practical resources page

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A-level Chemistry exemplar for required practical No. 12

Separation of species by thin-layer chromatography:


Analysis of the composition of some common medicines

Student sheet

Requirements

You are provided with the following:

ethanol or other solvent


ethyl acetate
ibuprofen tablet
paracetamol tablet
caffeine tablet
aspirin tablet
Anadin Extra tablet (or equivalent containing aspirin, paracetamol and caffeine)
pestle and mortar
weighing boat or bottle
TLC plate
capillary tubes
developing chamber (or suitable container with lid)
access to UV lamp.

Suggested method

Preparation of samples

a) Use a pestle and mortar to crush the aspirin tablet and transfer to a weighing boat or bottle.
b) Dissolve approximately 0.1 g of the powdered tablet in 0.5 cm3 of ethanol.
c) Repeat steps (a) and (b) with the ibuprofen tablet and the paracetamol tablet.
d) Use a pestle and mortar to crush the caffeine tablet and transfer to a weighing boat or bottle.
e) Dissolve approximately 0.1 g of the powdered tablet in 7.0 cm3 of ethanol.
f) Repeat steps (d) and (e) with the Anadin Extra tablet.

Thin-layer chromatography

a) Carefully use a pencil to draw a faint line 1 cm above the bottom of a TLC plate and mark five
spots, equally spaced along this line.
b) Use a capillary tube to apply a tiny drop of each solution to a different origin spot and allow the
plate to air dry.
c) Add approximately 10 cm3 of ethyl acetate to a development chamber (or suitable container
with a lid)
d) Place the TLC plate into the developing chamber, making sure that the level of the solvent is
below the spotting line. Replace the lid and make sure it is a tight seal.

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e) When the level of the solvent reaches about 1 cm from the top of the plate, remove the plate
and mark the solvent front with a pencil. Allow the plate to dry in the fume cupboard.
f) Place the plate under a UV lamp in order to visualise the spots. Draw around them lightly in
pencil.
g) Calculate the Rf values of the observed spots.

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