Practical Guide International Edexcel

Practical Guide International 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
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 lid improves the accuracy of the

The water of crystallisation in calcium sulfate crystals can be removed experiment as it prevents loss of solid
as water vapour by heating as shown in the following 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 sulfate 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
CORE PRACTICAL 2: 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.
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
limited
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 0.20M
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 calorimeter.
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 2.0 mol dm-3 HCl was neutralised by 25.0cm3 of 2.0 mol dm-3 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 can be called the enthalpy change of neutralisation
= 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
5
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
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)
= 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
Core practical 3+4. 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
Titrations Core Practical 3+4: 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 titrating A with B:
--> finding conc.
conical flask and B should be in the burette. of A using B
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.
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 ] unknown - alkali
known - acid point. unknown - acid
known - alkali
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
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.
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.
Core practical 5: 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 haloalkanes in a substitution
reaction
CH3CH2X + H2O  CH3CH2OH + X- + H+
Aqueous silver nitrate is added to a haloalkane 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
haloalkane and so the rate of formation of the precipitate can be silver nitrate first as the C-I bond is weakest
used to compare the reactivity of the different haloalkanes. and so it hydrolyses the quickest
The quicker the precipitate is formed, the faster the substitution

reaction and the more reactive the haloalkane 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.
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 sulphate, 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 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 The collection flask can be
with a naked flame. cooled in ice to help improve
yield of distillate
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. dehydrating/eliminating alcohol --> alkene
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
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.
Core practical 7. 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 sulfuric 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.
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
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
CORE PRACTICAL 8 + 15: Analysis of some inorganic unknowns
Testing for cations metal ions (positive)
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 dilute NaOH 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.
2+ Ion Summary
[MCl4]2-
[Zn(OH)4]2- colourless sol
[CuCl4]2- green sol
[CoCl4]2- blue sol
excess OH-
water Conc Cl-
Few drops OH -
or NH3 excess NH3 [Cu(NH3)4(H2O)2]2+
[M(H2O)6]2+ M(OH)2 (H2O)4 deep blue solution
H+ [Co(NH3)6]2+
[Cu(H2O)6]2+ blue sol Cu(OH)2(H2O)4 blue ppt yellow/light brown solution
[Co(H2O)6]2+ pink sol Co(OH)2(H2O)4 blue ppt [Ni(NH3)6]2+ blue sol
[Fe(H2O)6]2+ green sol Fe(OH)2(H2O)4 green ppt [Zn(NH3)4]2+ colourless sol
[Ni(H2O)6]2+ green sol Ni(OH)2(H2O)4 green ppt
[Mn(H2O)6]2+ very pale pink sol Mn(OH)2(H2O)4 light brown ppt
[Zn(H2O)6]2+ colourless sol Zn(OH)2(H2O)4 white ppt Air or H2O2
Air or H2O2 [Co(NH3)6]3+ brown sol
M(OH)3 (H2O)3
Fe(OH)3(H2O)3 brown ppt

Co(OH)3(H2O)3 brown ppt
Mn(OH)3(H2O)3 dark brown ppt
3+ Ion Summary Cr2O72- orange sol
H+ OH-
H2O2
[Cr(OH)6]3- green sol CrO42- yellow sol
excess OH-
Few drops
OH- or NH3 excess NH3
[M(H2O)6]3+ M(OH)3 (H2O)3 [Cr(NH3)6]3+ violet sol
H+
[Cr(H2O)6]3+ green sol
[Fe(H2O)6]3+ yellow sol Cr(OH)3(H2O)3 green ppt
Fe(OH)3(H2O)3 brown ppt
N Goalby chemrevise.org
21
CORE PRACTICAL 8+15: Analysis of some inorganic unknowns
Testing for anions: – Group 7 (halide ions), OH– , CO32– , SO42– negative ions
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 both dilute + concentrated
AgCl(s) + 2NH3(aq) [Ag(NH3)2]+ (aq) + Cl- (aq)
Colourless solution
Silver bromide dissolves in concentrated ammonia to form a complex ion only concentrated
AgBr(s) + 2NH3(aq) [Ag(NH3)2]+ (aq) + Br - (aq)
Colourless solution
Silver iodide does not react with ammonia – it is too insoluble. non
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
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 chocking
smell
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 sulfur
Ox ½ equation 2I -  I2 + 2e- H2S (Hydrogen sulfide), a gas with a bad egg smell.
Re ½ equation H2SO4 + 2 H+ + 2 e-  SO2 + 2 H2O
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
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 draw filter paper 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
CORE PRACTICAL 8+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 excess NH3 + AgNO3
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 silver mirror due to reduction
of Ag+ ions into Ag(s)
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.
ketones cannot be
CH3CHO + 2Cu2+ + 2H2O  CH3COOH + Cu2O + 4H+ further oxidized
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
primary alcohols produced
Alcohols, phenols, Sodium metal Efferevesence 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
Investigating rates of reaction
Techniques to investigate rates of reaction
There are several different methods for measuring reactions rates. Some reactions can be measured
in several ways
measurement of the change in volume of a gas
This works if there is a change in the number of moles of
gas in the reaction. Using a gas syringe is a common
way of following this.
(CH3)2C=CH2(g) + HI(g) (CH3)3CI(g)
HCOOH(aq) + Br2(aq)  2H+(aq) + 2Br - (aq) + CO2(g)
Measurement of change of mass
This works if there is a gas produced which is allowed to

escape. Works better with heavy gases such as CO2
HCOOH(aq) + Br2(aq)  2H+(aq) + 2Br - (aq) + CO2(g)
Titrating samples of reaction mixture with acid, alkali, sodium thiosulfate etc
1. Small samples are removed from the reaction mixture
2. quench (which stops the reaction)- can be done by
• by dilution with water
• by cooling
• by adding a reagent that reacts with one of the reactants
3. then titrate with a suitable reagent.
HCOOCH3(aq) + NaOH(aq)  HCOONa(aq) + CH3OH(aq) The NaOH could be titrated with an acid
BrO3 –(aq) + 5Br –(aq) + 6H+(aq)  3Br2(aq) + 3H2O(l) The H+ could be titrated with an alkali
CH3COCH3(aq) + I2(aq) → CH3COCH2I(aq) + H+(aq) + I–(aq) The I2 could be titrated with sodium
thiosulfate
Colorimetry.
If one of the reactants or products is coloured H2O2(aq) + 2I- (aq) + 2H+(aq)  2H2O(l) + I2(aq)
then colorimetry can be used to measure the
change in colour of the reacting mixtures The I2 produced is a brown solution
Measuring change in electrical conductivity

Can be used if there is a change in the number HCOOH(aq) + Br2(aq)  2H+(aq) + 2Br - (aq) + CO2(g)
of ions in the reaction mixture
Measurement of optical activity.

If there is a change in the optical activity through
the reaction this could be followed in a CH3CHBrCH3 (l) + OH−(aq)  CH3CH(OH)CH3 (l) + Br−(aq)
polarimeter
General: Measuring the rate of reaction: by an continuous monitoring method
When we follow one experiment over time recording the change in

concentration it is the continuous rate method.
concentration
The gradient represents the rate of reaction. The reaction is
fastest at the start where the gradient is steepest. The rate
drops as the reactants start to get used up and their
concentration drops. The graph will eventual become
horizontal and the gradient becomes zero which represents
the reaction having stopped.
time
Measurement of the change in volume of a gas

This works if there is a change in the number of moles of gas
in the reaction. Using a gas syringe is a common way of
following this. It works quite well for measuring continuous
rate but a typical gas syringe only measures 100ml of gas so gas syringe
you don’t want at reaction to produce more than this volume.
Quantities of reactants need to be calculated carefully.
Mg + HCl  MgCl2 +H2
Typical Method
The initial rate is the rate at the start of the • Measure 50 cm3 of the 1.0 mol dm–3 hydrochloric acid
reaction, where it is fastest. It is obtained by taking and add to conical flask.
the gradient of a continuous monitoring conc vs • Set up the gas syringe in the stand
time graph at time = zero. A measure of initial rate • Weigh 0.20 g of magnesium.
is preferable as we know the concentrations at the • Add the magnesium ribbon to the conical flask, place the
start of the reaction bung firmly into the top of the flask and start the timer.
• Record the volume of hydrogen gas collected every 15
seconds for 3 minutes.
Large Excess of reactants

In reactions where there are several reactants, if the
concentration of one of the reactant is kept in a large excess
then that reactant will appear not to affect rate and will be
pseudo-zero order . This is because its concentration stays
virtually constant and does not affect rate.
Continuous rate experiments

Continuous rate data
0.060 This is data from one experiment where the concentration of a
substance is followed throughout the experiment.
If half-lives are constant
[A]
then the order is 1st order

This data is processed by plotting the data and calculating
0.030 successive half-lives.
0.015 The half-life of a first-order reaction

0.0075 is independent of the concentration and is constant
If half-lives rapidly increase then the order is

t½ t½ t½ 2nd order
Time (min)
end of U3
CORE PRACTICAL 9a: Rates of reaction: Following the rate of the iodine propanone
reaction by a titrimetric method
Propanone reacts with iodine in acidic solution (the acid is a catalyst) as shown in the equation
below.
CH3COCH3(aq) + I2(aq) → CH3COCH2I(aq) + H+(aq) + I–(aq)
This reaction can be followed by removing small samples from the reaction mixture with a
volumetric pipette. The sample is then quenched by adding excess sodium hydrogencarbonate to
neutralize acid catalyst which stops the reaction. Then the sample can be titrated with sodium
thiosulphate using a starch catalyst
2S2O32-(aq) + I2 (aq)  2I- (aq) + S4O62-(aq)

yellow/brown sol colourless sol
[I2] This reaction is zero order with respect to I2 but 1st order
with respect to the propanone and acid catalyst
The rate equation for the reaction is

Rate = k[CH3COCH3(aq)][H+(aq)]
If there is a zero order reactant there must

be at least two steps in the mechanism
because the rate determining step will not
involve the zero order reactant
Time (min)
The rate determining step of this reaction must therefore contain one propanone molecule and one H+ ion
forming an intermediate. The iodine will be involved in a subsequent faster step.
Detailed Method
1. To a beaker add 25 cm3 of 1 mol dm−3 aqueous propanone and 25 cm3 of 1 mol dm−3 sulfuric acid.
2. Add 50 cm3 of 0.02 mol dm− 3 iodine solution. Start the clock swirl the beaker well to mix.
3. Using a 10cm3 pipette, withdraw a sample of the mixture and transfer it to a conical flask.
4. Add a spatula measure of sodium hydrogencarbonate (This stops the reaction). Record the time at which the sodium
hydrogencarbonate is added.
5. Titrate the iodine present in the conical flask with 0.01 mol dm − 3 sodium thiosulfate solution. When the colour
turns a pale yellow add the starch indicator. The end point is then when the mixture goes from blue to colourless.
6 Every 5 minutes withdraw another 10 cm3 sample and repeat steps 4 and 5
This method allows the order with respect to Iodine to be calculated because the propanone and
acid are in large excess so their concentrations do not change during the reaction
Core practical 9b: Rates of reaction: clock reaction
The initial rate can be calculated from taking the Initial rate can also be calculated from clock reactions
gradient of a continuous monitoring conc vs time where the time taken to reach a fixed concentration is
graph at time = zero measured.
A Common Clock Reaction (no need to learn details)

In clock reactions there are often two
Hydrogen peroxide reacts with iodide ions to form iodine. The thiosulfate
successive reactions and an end point is
ion then immediately reacts with iodine formed in the second reaction as
achieved when one limited reactant runs
shown below.
out, resulting in a sudden colour change
H2O2(aq) + 2H+(aq) + 2I–(aq) → I2(aq) + 2H2O(l)

By repeating the experiment several times,
2S2O32–(aq) + I2(aq) → 2I–(aq) + S4O62–(aq) varying the concentration of a reactant e.g.
I–, ( keeping the other reactants at constant
When the I2 produced has reacted with all of the limited amount of concentration )you can determine the
thiosulfate ions present, excess I2 remains in solution. Reaction with the order of reaction with respect to that
starch then suddenly forms a dark blue-black colour. reactant
A series of experiments is carried out, in which the concentration of iodide
ions is varied, while keeping the concentrations of all of the other reagents
the same. In each experiment the time taken (t) for the reaction mixture to The initial rate of the reaction can be
turn blue is measured. represented as (1/t )
Detailed method
• Put each of the chemicals in the table in separate burettes.
• In each experiment, measure out required volumes of the potassium iodide, sodium thiosulfate, starch and
water into a small conical flask from the burettes
• Measure the hydrogen peroxide into a test tube
• Pour the hydrogen peroxide from the test tube into the conical flaks and immediately start the timer. Stir the
mixture.
• Time until the first hint of blue/ black colour appears
Sulfuric Potassium Sodium Hydrogen

Experiment peroxide ml
acid (H+) ml Starch ml Water ml iodide(I-) ml Thiosulfate S2O32- ml
1 25 1 20 5 5 10
10
2 25 1 15 10 5
3 25 1 10 15 5 10
4 25 1 5 20 5 10
5 25 1 0 25 5 10
Normally to work out the rate equation we do a series of experiments where the initial concentrations of reactants are
changed (one at a time) and measure the initial rate each time.
Working out rate order graphically
In an experiment where the concentration of one of
log (rate)
the reagents is changed and the reaction rate measured

it is possible to calculate the order graphically
gradient = n
Taking rate equation
Rate = k [I- ]n = change in y
y intercept = log K
change in x
Log both sides of equation
Log rate = log k + n log [Y]
log [I- ]
Y= c + mx
In this experiment high concentrations with quick
A graph of log rate vs log [I- ] will yield a straight line where the
times will have the biggest percentage errors.
gradient is equal to the order n
Core practical 10: Finding the activation energy of a reaction
Experiment Determine the activation energy for the reaction between bromide ions and bromate(V) ions
BrO3– + 5Br– + 6H+  3Br2 + 3H2O The Bromine produced in the first reaction reacts with the phenol. When
the phenol is used up, the bromine is no longer removed. The bromine
C6H5OH + 3Br2 → C6H2Br3OH + 3HBr then bleaches the methyl red indicator at the ‘end of the reaction’
Detailed Method
1. Pipette 10 cm3 of phenol solution and 10 cm3 of bromide/bromate solution into a boiling tube.
2. Add a few drops of methyl red indicator to the mixture.
3. Into a second boiling tube pipette 5 cm3 of sulfuric acid.
4. Place the two boiling tubes in a water bath at temperature 20oC.
5. When the substances have reached the water temperature, mix the contents into one of the boiling tubes and
swirl. Start the stop clock.
6. Place the boiling tube containing the reaction mixture in the water bath.
7. Stop the clock when the methyl red indicator disappears.
8. Repeat the experiment at 30,40 50 60oC
In this experiment rate is 1/time where the time is the time taken for the indicator to change colour.
This is an approximation for initial rate of reaction as it does not include the change in concentration term. We can use
this because we can assume the amount of phenol used in each experiment is the same and constant. The change in
concentration is therefore the same for each experiment so only the time taken to reach this concentration is relevant.
Analysis of results to calculate activation energy 1/T

The Arrhenius equation can be rearranged
ln k = constant – EA/(RT)
ln (Rate)
Gradient = - EA/ R
k is proportional to the rate of reaction so ln k can be
replaced by ln(rate)
EA = - gradient x R
From plotting a graph of ln(rate) or ln k against 1/T the
activation energy can be calculated from measuring the
gradient of the line
Example 9 1/T
0.0029 0.003 0.0031 0.0032 0.0033 0.0034
Temperature time t -1.6
T (K) 1/T (s) 1/t Ln (1/t) x1,y1
297.3 0.003364 53 0.018868 -3.9703 -2.1
310.6 0.00322 24 0.041667 -3.1781
ln (Rate)
317.2 0.003153 16 0.0625 -2.7726 -2.6
323.9 0.003087 12 0.083333 -2.4849

-3.1
335.6 0.00298 6 0.166667 -1.7918
-3.6
x2,y2
gradient = y2-y1 The gradient should
x2-x1 always be -ve -4.1
In above example gradient =-5680 use a line of best fit

EA = - gradient x R (8.31) use all graph paper
= - -5680 x8.31 choose points far apart on the graph to
= 47200 J mol-1 calculate the gradient
The unit of EA using this equation will be J mol-1 . Convert

into kJ mol-1 by dividing 1000
EA = +47.2 kJ mol-1
Core practical 11: Finding the Ka value for a weak acid – titration curves
Constructing a pH curve
1. Transfer 25cm3 of acid to a conical flask with a volumetric Calibrate meter first by measuring known pH of a
pipette buffer solution. This is necessary because pH meters
2. Measure initial pH of the acid with a pH meter can lose accuracy on storage.
3. Add alkali in small amounts (2cm3) noting the volume Most pH probes are calibrated by putting probe in a
added set buffer (often pH 4) and pressing a calibration
4. Stir mixture to equalise the pH button/setting for that pH. Sometimes this is
5. Measure and record the pH to 1 d.p. repeated with a second buffer at a different pH
6. Repeat steps 3-5 but when approaching endpoint add in
Can also improve accuracy by maintaining
smaller volumes of alkali
constant temperature
7. Add until alkali in excess
Strong acid – Strong base e.g. HCl and NaOH
pH
13
Long steep part from

The equivalence point lies
around 3 to 9
at the mid point of the
7 extrapolated vertical
pH at equivalence
portion of the curve.
point = 7
25 cm3 of base
Weak acid – Strong base e.g. CH3CO2H and NaOH Half neutralisation volume
At the start the pH rises quickly and then levels off. The For weak acids
flattened part is called the buffer region and is formed because [H+ (aq)][A- (aq)]
a buffer solution is made Ka=
[HA (aq)]
pH
At ½ the neutralisation volume
13 the [HA] = [A-]
Equivalence point >7 So Ka= [H+] and pKa = pH
7 If we know the Ka we can then work out the pH

at ½ V or vice versa.
pH starts Steep part of curve >7 (around
near 3 7 to 9) If a pH curve is plotted then the pH of a weak
acid at half neutralisation (½ V) will equal the pKa
1
½V V cm3 of base
Weak acid – Weak base

pH Strong acid – Weak base
e.g. HCl and NH3 pH
e.g. CH3CO2H and NH3
13
13
No Steep part of the curve
Steep part of curve <7

7
(around 4 to 7)
7
Equivalence point < 7

1
1
25 cm3 of base
3
25 cm of base
Core practical 12: Investigating some electrochemical cells
Electron
flow
Method
• Clean the zinc and copper foils with emery before use. Salt bridge
Degrease the metal using some cotton wool and copper
propanone. electrode
Zinc
• Place the copper strip into a 100 cm3 beaker with
electrode
about 50 cm3 of 1 mol dm–3 CuSO4 solution.
• Place the zinc strip into a 100 cm3 beaker with about
1M
50 cm3 of 1 mol dm–3 ZnSO4 solution. 1M zinc copper
• Use a strip of filter paper soaked in saturated sulphate sulphate
potassium nitrate solution for the salt bridge solution solution
• Connect the Cu(s)|Cu2+ (aq) and Zn(s)|Zn2+ (aq) half-
cells by connecting the metals using the crocodile clips
and leads provided to the voltmeter
Salt Bridge
The salt bridge is used to connect up the circuit. The free moving ions conduct the charge.
A salt bridge is usually made from a piece of filter paper (or material) soaked in a salt solution, usually potassium nitrate.
It can also be a glass U tube containing a salt solution plugged with cotton wool
The salt should be unreactive with the electrodes and electrode solutions.. E.g. potassium chloride would not be suitable
for copper systems because chloride ions can form complexes with copper ions.
A wire is not used because the metal wire would set up its own electrode system with the solutions.
Pt electrode
Salt bridge
Method copper KNO3 (aq)
If one or both of the half cells do not contain a electrode
conducting metal, we must use an inert platinum
electrode.
Set up a copper half cell using a similar
arrangement to the previous one. Combine it
with a Fe2+/Fe3+ half-cell with a platinum 1M
electrode. copper
The half cell should have a mixture of acidified sulphate
solution
1.0M iron(II) sulphate solution and an equal
volume of 0.5M iron(III) sulphate solution as the 1M FeSO4 and 0.5 M Fe2(SO4)3
electrolyte. Use a fresh salt bridge.
Note: in the electrode system containing two solutions it is
A platinum electrode is used because it is necessary to use a platinum electrode and both ion solutions must
unreactive and can conduct electricity be of a 1M concentration so [Fe2+] = 1M and [Fe3+] = 1M .
Core practical 13a: Redox titration
Manganate Redox Titrations The purple colour of manganate can make it
The redox titration between Fe2+ with MnO4– (purple) is a very common difficult to see the bottom of meniscus in
exercise. This titration is self indicating because of the significant colour the burette.
change from reactant to product. If the manganate is in the burette then the end
point of the titration will be the first permanent
MnO4-(aq) + 8H+ (aq) + 5Fe2+ (aq)  Mn2+ (aq) + 4H2O (l) + 5Fe3+ (aq) pink colour.
Purple colourless Colourless  purple
Detailed Procedure : how much iron is in iron tablets
• Weigh accurately two 'ferrous sulfate' tablets.

• Grind up the tablets with a little 1M sulfuric acid, using a pestle and mortar.
• Through a funnel, transfer the resulting paste into a 100cm3 volumetric flask. Use further small volumes of 1 M
sulfuric acid to rinse the ground-up tablets into the flask.
• Then add sufficient 1M sulfuric acid to make up the solution to exactly 100cm3. Stopper the flask and shake it to
make sure that all the contents are thoroughly mixed. They will not all be in solution although the Fe 2+ ions which
were present in the tablets will be dissolved.
• Titrate 10.0 cm3 portions of the solution with 0.0050 M potassium manganate(VII). The end-point is marked by the
first permanent purple colour.
Choosing correct acid for manganate titrations.

The acid is needed to supply the 8H+ ions. Some acids are not suitable as they set up alternative redox reactions and
hence make the titration readings inaccurate.
Only use dilute sulfuric acid for manganate titrations.
Insufficient volumes of sulfuric acid will mean the solution is not acidic enough and MnO 2 will be produced instead of
Mn2+.
MnO4-(aq) + 4H+(aq) + 3e-  MnO2 (s) + 2H2O
The brown MnO2 will mask the colour change and lead to a greater (inaccurate) volume of manganate being used in
the titration.
Using a weak acid like ethanoic acid would have the same effect as it cannot supply the large amount of hydrogen
ions needed (8H+).
It cannot be conc HCl as the Cl- ions would be oxidised to Cl2 by MnO4- as the Eo MnO4-/Mn2+ > Eo Cl2/Cl-
MnO4-(aq) + 8H+(aq) + 5e–  Mn2+ (aq) + 4H2O(l) E+1.51V
Cl2(aq) +2e–  2Cl–(aq) E +1.36V
This would lead to a greater volume of manganate being used and poisonous Cl 2 being produced.
It cannot be nitric acid as it is an oxidising agent. It oxidises Fe 2+ to Fe3+ as Eo NO3-/HNO2> Eo Fe3+/Fe2+

NO3- (aq) + 3H+(aq) + 2e–  HNO2(aq) + H2O(l) Eo +0.94V
Fe3+ (aq)+e–  Fe2+ (aq) Eo +0.77 V
This would lead to a smaller volume of manganate being used.
Example 6 Manganate titration Step1 : find moles of KMnO4

A 2.41g nail made from an alloy containing iron is moles = conc x vol
dissolved in 100cm3 acid. The solution formed contains 0.02 x 9.8/1000
Fe(II) ions. = 1.96x10-4 mol
10cm3 portions of this solution are titrated with Step 2 : using balanced equation find moles Fe2+ in 10cm3
potassium manganate (VII) solution of 0.02M. 9.80cm3
= moles of KMnO4 x 5
of KMnO4 were needed to react with the solution
= 9.8x10-4 mol
containing the iron.
Step 3 : find moles Fe2+ in 100cm3
Calculate the percentage of iron by mass in the nail.
= 9.8x10-4 mol x 10
MnO4-(aq) + 8H+(aq) + 5Fe2+  Mn2+(aq) + 4H2O + 5Fe3+ = 9.8x10-3 mol
Step 4 : find mass of Fe in 9.8x10-3 mol
mass= moles x RAM = 9.8x10-3 x 55.8 = 0.547g
Step 5 : find % mass
%mass = 0.547/2.41 x100
= 22.6%
Other useful manganate titrations
With hydrogen peroxide
Ox H2O2  O2 + 2H+ + 2e-
Red MnO4-(aq) + 8H+(aq) + 5e-  Mn2+ (aq) + 4H2O The reaction between MnO4- and
Overall 2MnO4-(aq) + 6H+(aq) + 5H2O2  5O2 + 2Mn2+ (aq) + 8H2O C2O42- is slow to begin with (as the
With ethanedioate reaction is between two negative
ions). To do as a titration the conical
Ox C2O42-  2CO2 + 2e-
flask can be heated to 60o C to
Red MnO4-(aq) + 8H+(aq) + 5e-  Mn2+ (aq) + 4H2O
speed up the initial reaction.
Overall 2MnO4-(aq) + 16H+(aq) + 5C2O42-(aq)  10CO2(g) + 2Mn2+(aq) + 8H2O(l)
With Iron (II) ethanedioate both the Fe2+ and the C2O42- react with the MnO4-
1MnO4- reacts with 5Fe2+ and 2 MnO4- reacts with 5C2O42-
MnO4-(aq) + 8H+(aq) + 5Fe2+  Mn2+ (aq) + 4H2O + 5Fe3+

2MnO4-(aq) + 16H+(aq) + 5C2O42-  10CO2 + 2Mn2+ (aq) + 8H2O
So overall
3MnO4-(aq) + 24H+(aq) + 5FeC2O4  10CO2 + 3Mn2+ (aq) + 5Fe3+ + 12H2O
So overall the ratio is 3 MnO4- to 5 FeC2O4
Example 7 Step1 : find moles of KMnO4

A 1.412 g sample of impure FeC2O4.2H2O was moles = conc x vol
dissolved in an excess of dilute sulphuric acid 0.0189 x 23.45/1000
and made up to 250 cm3 of solution. 25.0 cm3 = 4.43x10-4 mol
of this solution decolourised 23.45 cm3 of a
Step 2 : using balanced equation find moles FeC2O4.2H2O in 25cm3
0.0189 mol dm–3 solution of potassium
manganate(VII). = moles of KMnO4 x 5/3 (see above for ratio)
What is the percentage by mass of = 7.39x10-4 mol
FeC2O4.2H2O in the original sample? Step 3 : find moles FeC2O4.2H2O in 250 cm3
= 7.39x10-4 mol x 10
= 7.39x10-3 mol
Step 4 : find mass of FeC2O4.2H2O in 7.39x10-3 mol
mass= moles x Mr = 7.39x10-3 x 179.8 = 1.33g
Step 5 ; find % mass
%mass = 1.33/1.412 x100
= 94.1%
CORE PRACTICAL 13b: Redox titration

Thiosulfate redox titration A starch indicator is added near the end
The redox titration between I2 and thiosulfate S2O32- is a point when the iodine fades a pale yellow
common exercise. to emphasise it.
With starch added the colour change is
2S2O32-(aq) + I2 (aq)  2I- (aq) + S4O62-(aq) from blue/black to colourless
yellow/brown sol colourless sol
The starch should not be added until nearly all the iodine has
reacted because the blue complex formed with high
concentrations of iodine is insoluble and does not re-dissolve as
more thiosulfate is added
Core practical 14: Prepare a transition metal complex
1. Add 1.5 g of hydrated copper(II) sulfate to weighing The mass of the copper(II) sulfate is the
bottle and measure the combined mass. difference between the two masses.
2. Transfer the copper (II) sulfate to a test tube and
measure the mass of the empty weighing bottle.
3. Add 4 cm3 of water to the test tube
4. Place the test tube in the water bath (a beaker with
freshly boiled water).
5. Stir gently to dissolve the copper(II) sulfate.
6. Remove the test tube containing copper(II) sulfate
solution from the water bath
7. In a fume cupboard, add 2 cm3 of concentrated
ammonia solution to the copper(II) sulfate solution Concentrated ammonia is corrosive.
8. Pour the contents of the test tube into a beaker Use in a fume cupboard and wear
containing 6 cm3 of ethanol. Stir well and cool the gloves
mixture in an ice bath.
9. Using a Buchner funnel and flask, filter the crystals.
Wash the test tube with some cold ethanol and add
the washings to the Buchner funnel. Finally, rinse the
crystals with a little cold ethanol.
10. Scrape the crystals onto a fresh piece of filter paper
and cover with a second piece of filter paper and Buchner
press to dry the crystals. funnel
11. Measure the mass of the dry crystals Filter paper
Buchner flask (has
Air outlet to
thicker glass walls than
water pump
a normal flask to cope
with the vacuum )
This is vacuum filtration. The apparatus is

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

CuSO4•5H2O + 4NH3 → Cu(NH3)4SO4•H2O + 4H2O
Loss of yield in this process

• Crystals lost when filtering or washing
• Some product stays in solution after recrystallisation
• other side reactions occurring
If the crystals are not dried properly the mass will be larger
than expected which can lead to a percentage yield >100%
Preparation of a pure organic solid and test of its purity
Purifying an organic solid: Recrystallisation Used for purifying aspirin
Step Reason
1. Dissolve the impure compound in a minimum volume An appropriate solvent is one which will dissolve both
of hot (near boiling) solvent. compound and impurities when hot and one in which the
compound itself does not dissolve well when cold.
The minimum volume is used to obtain saturated
solution and to enable crystallisation on cooling
2. Hot filter solution through (fluted) filter paper quickly. This step will remove any insoluble impurities and heat
will prevent crystals reforming during filtration
3. Cool the filtered solution by inserting beaker in ice Crystals will reform but soluble impurities will remain in
solution form because they are present in small quantities
so solution is not saturated. Ice will increase the yield of
crystals
4. Suction filtrate with a Buchner flask to separate out The water pump connected to the Buchner flask reduces
crystals the pressure and speeds up the filtration.
5 Wash the crystals with distilled water To remove soluble impurities
6. Dry the crystals between absorbent paper
Loss of yield in this process

• Crystals lost when filtering or washing
• Some product stays in solution after recrystallisation
• other side reactions occurring
If the crystals are not dried properly the mass will be larger Buchner flask
than expected which can lead to a percentage yield >100%
16. Core activity: The preparation of aspirin
Detailed method for Preparation of Aspirin Aspirin is made from 2-hydroxybenzoic
O acid which contains a phenol group. In the
CO2H
CO2H CH3 C O
reaction the phenol group is turned into an
ester by reacting it with the reactive
OH
+ O  O C CH3 + CH CO H
3 2
ethanoic anhydride
CH3 C
O Aspirin Ethanoic anhydride is used instead of
Add to a 50 cm3 pear-shaped flask 2.0 g of 2-hydroxybenzoic acid and acid chlorides because it is cheaper, less
4 cm3 of ethanoic anhydride. corrosive, less vulnerable to hydrolysis,
To this mixture add 5 drops of 85% phosphoric(v) acid and swirl to and less dangerous to use.
mix, Fit the flask with a reflux condenser and heat the mixture on a
The excess ethanoic anhydride will
boiling water bath for about 5 minutes. Without cooling the mixture,
hydrolyse and the contents of the flask
carefully add 2 cm3 of water in one portion down the condenser.
will boil.
When the vigorous reaction has ended, pour the mixture into 40 cm 3
of cold water in a 100 cm3 beaker, stir and rub the sides of the beaker
with a stirring rod necessary to induce crystallisation and, finally,
allow the mixture to stand in ice bath to complete crystallisation.
Collect the product by suction filtration and wash it with a little water.
Purification stage: recrystallisation

Using a measuring cylinder, measure out 15 cm3 of ethanol into a
boiling tube.
Prepare a beaker half-filled with hot water from a kettle at a Avoid naked flames due to
temperature of approximately 75 °C. flammability of ethanol
Use a spatula to add the crude aspirin to the boiling tube with ethanol
and place the tube in the beaker of hot water.
Stir the contents of the boiling tube until all of the aspirin dissolves
into the ethanol.
Pour the hot solution containing dissolved aspirin through a warmed This step will remove any insoluble
filter funnel and fluted filter paper to hot filter impurities and heat will prevent crystals
Then pour filtrate into 40 cm3 of water in a conical flask. reforming during filtration
Allow the conical flask to cool slowly and white needles of aspirin
should separate. Soluble impurities will remain in solution form
Cool the whole mixture in an ice bath. because they are present in small quantities
Filter off the purified solid under reduced pressure and allow it to dry so solution is not saturated. Ice will increase
on filter paper. the yield of crystals
Record the mass of the dry purified solid
Detailed method for Nitration Procedure

Conc acids are corrosive- wear
Measure 2.5 cm3 of methyl benzoate into a small conical flask and then gloves
dissolve it in 5 cm3 of concentrated sulfuric acid. When the liquid has The acids react together to make
dissolved, cool the mixture in ice. the NO2+ ion
Prepare the nitrating mixture by adding drop by drop 2 cm3 of This reaction is exothermic so acids
concentrated sulfuric acid to 2 cm3 of concentrated nitric acid. Cool this are kept cool and acid is added
mixture in ice as well. dropwise
Now add the nitrating mixture drop by drop from a dropping pipette to
the solution of methyl benzoate. Stir the mixture with a thermometer and The temperature is kept low at this
keep the temperature below 10 °C. When the addition is complete, allow stage to prevent multiple
the mixture to stand at room temperature for another 15 minutes. substitution of nitro groups on the
After this time, pour the reaction mixture on to about 25 g of crushed ice benzene ring
and stir until all the ice has melted and crystalline methyl 3-nitrobenzoate
has formed.
Then use same purification method as in aspirin above
Measuring melting point
One way of testing for the degree of purity is to determine the melting
“point”, or melting range, of the sample.
Thermometer with
If the sample is very pure then the melting point will be a capillary tube
sharp one, at the same value as quoted in data books. strapped to it
containing sample
If impurities are present (and this can include solvent from the
recrystallisation process) the melting point will be lowered and the Heating oil- needs to
sample will melt over a range of several degrees Celsius have boiling point
higher than samples
melting point and low
Melting point can be measured in an electronic melting point machine or flammability
by using a practical set up where the capillary tube is strapped to a
thermometer immersed in some heating oil.
In both cases a small amount of the sample is put into a capillary tube. The
tube is heated up and is heated slowly near the melting point
Heat
Comparing an experimentally determined melting point value
with one quoted in a data source will verify the degree of Sometimes an error may occur if the
purity. temperature on the thermometer is not the
same as the temperature in the actual sample
tube.
steam
Steam distillation in
In steam distillation steam is passed into

the mixture and the product vapour is
distilled off with the water and condensed
Advantage of steam distillation:

The product distils at a lower temperature
which can prevents decomposition of the
product if it has a high boiling point
Water
out
Water
in
Solvent extraction
Mix organic solvent and oil-water mixture in a

separating funnel then separate the oil layer.
Distil to separate oil from organic solvent
Add anhydrous CaCl2 to clove oil to dry oil
Decant to remove CaCl2
Separating funnel
Separation of species by thin-layer chromatography
Method: Thin-layer chromatography

Wear plastic gloves to prevent contamination
a) Wearing gloves, draw a pencil line 1 cm above the bottom of a from the hands to the plate
TLC plate and mark spots for each sample, equally spaced along
line. pencil line –will not dissolve in the solvent
b) Use a capillary tube to add a tiny drop of each solution to a tiny drop – too big a drop will cause different
different spot and allow the plate to air dry. spots to merge
c) Add solvent to a chamber or large beaker with a lid so that is no
more than 1cm in depth Depth of solvent– if the solvent is too deep it will
d) Place the TLC plate into the chamber, making sure that the level dissolve the sample spots from the plate
of the solvent is below the pencil line. Replace the lid to get a
lid– to prevent evaporation of toxic solvent
tight seal.
e) When the level of the solvent reaches about 1 cm from the top Will get more accurate results if the solvent is
of the plate, remove the plate and mark the solvent level with a allowed to rise to near the top of the plate but the
pencil. Allow the plate to dry in the fume cupboard. Rf value can be calculated if the solvent front does
f) Place the plate under a UV lamp in order to see the spots. Draw not reach the top of the plate
around them lightly in pencil.
g) Calculate the Rf values of the observed spots. dry in a fume cupboard as the solvent is toxic
UV lamp used if the spots are colourless and not

visible
Rf value = distance moved by amino acid

distance moved by the solvent
If the stationary phase was polar and the moving

Separation by chromatography depends on the
phase was non- polar e.g. Hexane. Then non-polar
balance between solubility in the moving phase and
compounds would pass through the plate more quickly
retention in the stationary phase.
than polar compounds as they would have a greater
solubility in the non-polar moving phase.
A solid stationary phase separates by adsorption, (Think about intermolecular forces)
A liquid stationary phase separates by relative solubility
Rf values are used to identify different substances.
Practical: Working out equilibrium constant Kc
A common experiment is working out the equilibrium constant for an esterification reaction. Ethanol and
ethanoic acid are mixed together with a sulfuric acid catalyst.
CH3CO2H + CH3CH2OH CH3CO2CH2CH3 + H2O

Ethanoic acid Ethanol Ethyl Ethanoate
Method
Part 1 Preparing the equilibrium mixture
1 Use burettes to prepare a mixture in boiling tube of carboxylic acid, alcohol, and dilute sulfuric acid.
2 Swirl and bung tube. Leave the mixture to reach equilibrium for one week
Part 2 Titrating the equilibrium mixture

1 Rinse a 250 cm3 volumetric flask with distilled water.
Use a funnel to transfer the contents of the boiling tube into the flask. Rinse the boiling tube with water and add
the washings to the volumetric flask.
2 Use distilled water to make up the solution in the volumetric flask to exactly 250 cm 3.
Stopper the flask, then invert and shake the contents thoroughly.
3 Use the pipette to transfer 25.0 cm3 of the diluted equilibrium mixture to a 250 cm3 conical flask.
4 Add 3 or 4 drops of phenolphthalein indicator to the conical flask.
5 Set up the burette with sodium hydroxide solution..
6 Add the sodium hydroxide solution from the burette until the mixture in the conical flask just turns pink. Record
this burette reading in your table.
7 Repeat the titration until you obtain a minimum of two concordant titres.
The sodium hydroxide will react with the sulfuric acid catalyst and any unreacted carboxylic acid in the
equilibrium mixture
There are many different calculations that can be based on this experiment. Let’s
look at general stages. Not all calculations will use all the stages.
Working out initial amount of moles of reactants

The amount of moles of alcohol and carboxylic acid can be calculated from the densities
and volumes of liquids added
Mass = density x volume
then
Moles = mass / Mr
The initial amount of moles of acid catalyst used is usually determined by titrating a
separate sample of catalyst with sodium hydroxide
Working out equilibrium amount of moles of acid present from the titre results
39.0 cm3 of 0.400 mol dm-3 sodium hydroxide was used in the above titration. The initial moles of sulphuric acid
was 5x10-4 mol. Calculate the moles of ethanoic acid present at equilibrium
Amount of NaOH = vol X conc

= 0.039 x 0.400
= 0.0156 mol
So total amount of H+ present in 25cm3 = 0.0156 mol
So total amount of H+ present in 250cm3 = 0.156 mol
Total mol acid present = moles of carboxylic acid + moles of acid catalyst
So X 2 because H2SO4
Amount of carboxylic acid at equilibrium = 0.156 – (5x10-4 x 2) has 2 H+
= 0.155 mol
The pink colour of the phenolphthalein in the titration can fade after the end-point of the titration has been reached
because the addition of sodium hydroxide may make the equilibrium shift towards the reactants
Working out equilibrium amount of moles of other substances
Calculate the equilibrium amount of ethanol, ethyl ethanoate and water if there were initially 0.400 mol of
ethanol and 0.500 mol of ethanoic acid and at equilibrium there were 0.155 mol of ethanoic acid.
Amount of ethanoic acid that reacted = initial amount – equilibrium amount

= 0.5 – 0.155
= 0.344mol
Amount of ethanol at equilibrium = initial amount - amount that reacted
= 0.400 – 0.344
= 0.056 mol
Amount of ethyl ethanoate at equilibrium = initial amount + amount that formed
= 0 + 0.344
= 0.344 mol
Amount of water at equilibrium = initial amount + amount that formed The amount of water at
= 0 + 0.344 equilibrium would not really be
= 0.344 mol 0 as there would be water
present in the acid catalyst
Calculating the equilibrium constant

Finally calculate the equilibrium constant.
To work out equilibrium concentrations divide the equilibrium amounts by the total volume. Then put in Kc
expression
Kc = [CH3CO2CH2CH3 ] [H2O]
[CH3CO2H] [CH3CH2OH]
In order to confirm that one week was sufficient time for equilibrium to be established in the mixture
from Part 1, several mixtures could be made and left for different amount of time. If the resulting Kc is
the same value then it can be concluded the time is sufficient
Spectrophotometry
If visible light of increasing frequency is passed through a Absorption of visible light is used in spectrometry to
sample of a coloured complex ion, some of the light is determine the concentration of coloured ions.
absorbed.
The amount of light absorbed is proportional to the method
concentration of the absorbing species (and to the distance •Add an appropriate ligand to intensify colour
travelled through the solution). •Make up solutions of known concentration
Some complexes have only pale colours and do not absorb •Measure absorption or transmission
light strongly. In these cases a suitable ligand is added to •Plot graph of absorption vs concentration
intensify the colour. •Measure absorption of unknown and compare
Spectrometers contain a coloured filter. The colour of the filter is chosen to only allow the wavelengths of light
through that would be most strongly absorbed by the coloured solution.
Detailed method- measuring absorption of copper solutions

• Take nine 100cm3 graduated flasks and pipette 20cm3 of 2 mol dm-3 ammonia solution into each one.
Use the 0.05M solution of aqueous copper sulfate to make up solutions which are concentrations of 0.005 to 0.04
mol dm-3 of [Cu(NH3)4(H2O)2 ]2+
• Mix each solution thoroughly.
• Insert the red filter into the colorimeter.
• Use a cuvette with distilled water to zero the colorimeter
• Then put each prepared solution in cuvette and measure the absorbance of each solution.
• Plot graph of absorption vs concentration
• Measure absorption of unknown solution and determine its concentration from the calibration curve
0.005 to 0.04 mol dm-3 solutions of [Cu(NH3)4(H2O)2 ]2+
Calibration curve
1.8
1.6
1.4
1.2
absorption
1
0.8
0.6
0.4
0.2
0
0 0.01 0.02 0.03 0.04 0.05
concentration in mol dm-3
colorimeter
Autocatalytic Reaction between Ethanedioate and Manganate ions
Potassium manganate(VII) will oxidise ethanedioic acid (oxalic acid) to carbon
dioxide and water, in the presence of an excess of acid:
2MnO4-(aq) + 6H+ (aq) + 5(CO2H)2 (aq) 2Mn2+ (aq) +10CO2 (g) + 8H2O (I)
Detailed method
1. Prepare a reaction mixture according to the table, using Solution Mixture 1 Mixture 2
measuring cylinders. 0.2 M ethanedioic acid 100cm3 100cm3
2. Some members of your group should use mixture 1 and some 0.2 M manganese(ll)
-- 15cm3
mixture 2. The results should then be shared. sulfate
3. Add 50 cm3 of 0.02 M potassium manganate(VII) and start timing. 1 M sulfuric acid 10 cm3 10cm3
Shake the mixture for about half a minute to mix it well. Water 90 cm3 75 cm3
4. After about a minute use a pipette to withdraw a 10.0 cm3
portion of the reaction mixture and empty into a conical flask.
5. Note the time and add about 10cm3 of 0.1 M potassium iodide
solution. This stops the reaction and releases iodine equivalent to
the remaining manganate(VII) ions.
6. Titrate the liberated iodine with 0.01 M sodium thiosulfate,
adding a little starch solution near the end-point. Record the titre
of sodium thiosulfate.
7. Remove further portions every 3 or 4 minutes and titrate them in
the same way. Continue until the titre is less than 3 cm3.
Explanation of results
The autocatalysis by Mn2+ in titrations of C2O4 2- with MnO4- This is an example of autocatalysis where one of
the products of the reaction can catalyse the
overall 2 MnO4- + 5 C2O42- + 16 H+  2Mn2+ + 10 CO2 + 8 H2O reaction.
Catalysed alternative route Mixture with only

Step 1 4Mn2+ + MnO4- + 8 H+  5Mn3+ + 4 H2O reactants showing
Step 2 2Mn3+ + C2O42-  2Mn2+ + 2 CO2 effect of autocatalysis
The initial uncatalysed reaction is slow because the reaction is a

collision between two negative ions which repel each other
leading to a high activation energy. Mixture with
The Mn2+ ions produced act as an autocatalyst and therefore the added catalyst
reaction starts to speed up because they bring about the Mn2+ at start
alternative reaction route with lower activation energy.
The reaction eventually slows as the MnO4- concentration drops.
Alternative method for following the reaction rate

This experiment can be done by removing samples at set times and titrating to work out the concentration of MnO 4- .
It could also be done by use of a spectrometer measuring the intensity of the purple colour. This method has the
advantage that it does not disrupt the reaction mixture, using up the reactants and it leads to a much quicker
determination of concentration.

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Safety and hazards

Measuring gas volumes

Potential errors in using a gas syringe

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

Moles of gas can be calculated from gas

Volume of CO2 in cm3

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

moles = PV/RT 100 kPa = 100 000 Pa

The lid improves the accuracy of the

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

Calculate ratio of mole of 0.0122 = 0.085

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

To counteract this we take readings at regular time intervals and

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

Errors in this method Read question carefully. It

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

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

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

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

Enthalpies of combustion can be calculated by using calorimetry.

Errors in this method

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

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

moles of propan-1-ol = mass/ Mr

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

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

Measuring mass accurately:

Titrations are done often to find out the concentration of one

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

However, the standard phrase: titrate solution A

A conical flask is used in preference to a beaker because

Detailed Method for Titration

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

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

Read the bottom of the meniscus on the burette

This is reading 9.00cm3

note burette reading before and after addition of solution

Working out average titre results

Titre (cm3 ) 24.00 24.50 24.40

Calculate the percentage error for each piece of equipment used by

Reducing uncertainties in a titration To decrease the apparatus uncertainties

Weighing sample before and after addition and then calculating

Testing for halogenoalkanes method

Comparing the rate of hydrolysis of halogenoalkanes reaction

The quicker the precipitate is formed, the faster the substitution

Distillation It’s important to be able to

Note the bulb of the thermometer should be Liebig condenser

Note the water goes in the bottom of the Water

Detailed method for preparing and purifying a halogenoalkane from an alcohol

Detailed method for preparing and purifying Cyclohexene from cyclohexanol

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

Measuring boiling point

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

Reaction: primary alcohol  aldehyde

Observation: the orange

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

Distillation It’s important to be able to

Note the bulb of the thermometer should be Liebig condenser

Note the water goes in the bottom of the Water