CORE PRACTICAL 1
Key Points
Experimental Obiective
• To find the volume of one mole of carbon dioxide gas
Method
Measure 30 cm3 of 1 mol dm-3 ethanoic acid
and transfer to a conical flask.
Attach conical flask to gas syringe or use collection
over water method
Measure the mass of a weighing bottle with approx
0.05 g of calcium carbonate
Add the calcium carbonate to the conical flask - quickly
resealing the bung so no gas escapes
Measure the final total volume of gas
Reweigh the empty weighing bottle test tube from
step 3
Repeat the experiment several more times, increasing
the mass of calcium carbonate by about 0.05 g each
time.
Exemplar Results
The results for this experiment are plotted into a
graph which should be a straight line (a line mass of
CaCOz can be found. of best fit may be needed)
From the graph, the volume of CO2 produced for a
specific
mass of CaCO3 can be found
Example:
0.25 g CaCOz = 61 cm3
n(CaCO3) = 0.25/100.1 = 0.0025
1:1 ratio .. 0.0025 moles of CO2
MV = 0.061/0.0025
MV = 24.4 dm3 mol-1
Conclusion
• The molar volume of carbon dioxide at room
temperature
(298 K) is 24.4 dm3 mol-1
Molar volume will change depending on the
temperature of the gas
However most molar volumes are determined at
standard temperature and pressure (STP) which are 100
kPa and 298 K
Wait until no effervescence is observed before
weighing flask containing acid and marble chips
(CaCOz) to minimise gas loss.
Don't use too much CaCO so you don't produce more
gas than the measuring cylinder can fit.
A weak acid is used so that the reaction is slower,
meaning there is less gas loss between adding
marble chips and attaching bung.
An alternative method could involve attaching
marble chips on a string to the bung, sealing the
test tube with a bung, and then tipping the test
tube so that the acid comes to the contact with
the marble chip.
This could reduce the loss of product.
Errors
For syringes, a plunger may not be free moving so
may need lubricant
CO, is slightly soluble in water, so the exact volume is
not measured.
Some gas escapes between addition of marble chips
and sealing the test tube.
Bung may not be airtight.
Transferring the solid - It is important to weigh the
tube containing marble chips before the
addition and reweigh after the addition. This
method is 'weighing by difference' and ensures
the amount of CaCO3 that ends up in the
reaction mixture is known..
Safety and Apparatus
Apparatus
Boiling tube
Stand and clamp
Bung with delivery tube
Water bath or gas syringe
100cm§ and 50cm§ measuring cylinders
Test tube
2 d.p. balance
1 mol dm 3 ethanoic acid
Powdered calcium carbonate
Safety
Wear eye protection
Remove the bung if the delivery tube gets blocked,
clear the blockage and restart the experiment
Avoid skin contact with the ethanoic acid
 CORE PRACTICAL 2
Experimental Objective
• To calculate the molar enthalpy change for two reactions and
use Hess's Law to determine the enthalpy change for the
reactions
Method
1. Place approximately 3 g of solid potassium carbonate in a test
tube Errors and Assumptions
Accurately weigh the test tube and its contents Energy can be transferred to the
Use a burette to add 30 cm3 of 2.0 mol dm-3 dilute surroundings
hydrochloric acid into a polystyrene cup which is supported Specific heat capacity of HCI (aq) assumed to
by a beaker be the same as water
Measure the temperature of the acid Ignore energy that is absorbed by the
Gradually add the potassium carbonate to the acid, stirring and polystyrene cup
continuously monitoring the temperature Density of the HCI (aq) assumed to be the
Reweigh the empty test tube same as water
Repeat steps 1-6 using approximately 3.5 g of potassium
hydrogencarbonate and record the lowest temperature Apparatus : 2.0mol dm-3 dilute hydrochloric
reached acid , Solid potassium carbonate , Solid potassium
Exemplar Results hydrogencarbonate , Thermometer , Polystyrene
• We can calculate the energy released in each reaction using: cup , 400 cm3 beakers , 2 × test tubes , Burette,
Q = mc t clamp stand , Stirring rod , 2 d.p. mass
• We can then determine the molar enthalpy using: balance , spatula
AH = Q/n
Safety
• Construct a Hess's cycle for the decomposition using the two
Wear eye protection and suitable chemical
equations:
resistant gloves
Reaction 1 - K,CO (s) + 2HCI (aq) -+ 2KCI (aq) + CO2 (g) + H2O (1)
Avoid skin contact with reactants and products
Reaction 2 - KHCO3 (s) + HCI (aq) - KCI (aq) + COz (g) + H2O (I)
Decomposition - KHCO3 (s) - K,CO; (s) + CO2 (g) + H20 (1)
CORE PRACTICAL 3
Experimental objective
* Finding concentration of a solution
Method
Wash out a 250 cm3 volumetric flask with distilled water
Use the pipette to add 25 cm3 hydrochloric acid in to the volumetric
flask and make the rest up with distilled water
Pour a 25 cm3 sample of the HCI solution in to the conical flask and add
a few drops of phenolphthalein indicator
Prepare your apparatus for the titration - sodium hydroxide in the
burette and the hydrochloric acid in the conical flask
Titrate the contents of the flask against the NaOH solution and record
the titre to the nearest 0.05 cm3 (when a permanent pink colour
appears)
Conduct additional titrations until you have concordant values Errors
Allow the titrant time to drain down the walls
Diagram and key points of the burette before reading the volume
Diluting the solutions may produce a reading
Rinse the pipette with the HCI solution before measuring out your
sample with a smaller percentage error
Calibrate the pipette by ensuring there are no air bubbles in the tip Phenolphthalein can turn back to colourless if
Rinse and fill the burette with the solution of your titrant using a left to stand because the NaOH reacts with the
funnel CO, in the air to make Na2co3
 Safety and Apparatus
Apparatus
0.08 mol dm-3 sodium hydroxide
Burette, clamp and stand
Hydrochloric acid of unknown concentration
Phenolphthalein indicator
250 cm3 conical flask
25 cm3 volumetric pipette and filler
100 cm3 beaker
Funnel
250 cm3 beaker
250 cm3 volumetric flask

Safety
Wear eye protection and suitable chemical resistant gloves , Avoid skin contact with acid, alkali and indicator
Always use a pipette filler; never use your mouth to suck the liquid up , Take care when clamping and filling the burette
that it does not crack or topple over

CORE PRACTICAL 4
objective : • To make a solution of a known concentration of an acid and use it to find the concentration of a
solution of sodium hydroxide
Method
Weigh an empty test tube and then add
approximately 2.5 g sulfamic acid in to it
Accurately reweigh the test tube and its contents
Dissolve the sulfamic acid in 100 cm3 of distilled
water
Transfer the solution and washings to a volumetric
flask and use distilled water to make it up to the
graduation mark
Prepare the apparatus for titrations and use a
pipette to measure out a 25.0 cm3 sample of the
acid solution into a conical flask with a few drops
of methyl orange indicator
Titrate the contents of the flask against the NaOH and
record the results to the nearest 0.05 cm3
Repeat the titration until you have concordant
results
key points
The acid used must have a high molar mass to reduce
weighing
errors
The sample must be pure and impurities can affect the
calculated concentration
The sample must not be air sensitive or react with any air
components (e.g. absorbing COz or H20)
Errors
Be careful not to lose any solid when transferring from the
weighing bottle to the beaker
When weighing out a solid, weight by difference and then
calculate the mass of a solid in a beaker
Mass of bottle + beaker - mass of empty bottle

Apparatus Safety
0.08 mol dm-3 sodium hydroxide Wear eye protection and suitable
Burette, clamp and stand chemical resistant gloves
Hydrochloric acid of unknown
Avoid skin contact with acid, alkali and
concentration
indicator
Phenolphthalein indicator
Always use a pipette filler; never use
250 cm3 conical flask
your mouth to suck the liquid up
25 cm3 volumetric pipette and
filler
Take care when clamping and filling the
100 cm3 beaker burette that it does not crack or
Funnel topple over
250 cm3 beaker
250 cm3 volumetric flask
 CORE PRACTICAL 5
Experimental Objective
• To investigate the relative rates of hydrolysis of primary, secondary, tertiary halogenoalkanes and of
chloro-, bromo- and iodoalkanes

Method
Set up a water bath using a 250 cm3 beaker with water around 50°C
Take three test tubes and add 5 cm3 of ethanol to each one
Add four drops of 1-iodobutane to the first test tube, 1-bromobutane to the second test tube and 1-
chlorobutane to the third test tube
Loosely place bungs in the test tubes and place them in a water bath
Take three clean test tubes and pour 5 cm3 of silver nitrate solution into each one and also place in the water
bath
When the halogenoalkane-ethanol solutions have reached the temp of the water bath, add a silver nitrate to
each test tube and measure the time taken for the precipitate to form
Repeat step 6 using the primary, secondary and tertiary
Key Points
This is a nucleophilic substitution reaction where
water acts as the nucleophile - it is also
known as hydrolysis
The equation for the formation of the
precipitation is:
RX + H2O -> ROH + H+ + X-
This is due to the relative strength of the C-X bond
X- (ag) + Ag* (ag) -› AgX (s) C-I is the weakest bond so it is the easiest one to break therefore the
The variables that are independentlv controlled precipitate forms the quickest.
are the nature of the halide (chloro-, bromo- or C-CI is the strongest bond so it is the hardest one to break therefore
iodo-) or the type of alkane (primary, secondary the precipitate forms the slowest.
or tertiary)

Errors
Ensure that the water bath is at the correct
temperature to control the temperature of the
halogenoalkane
Use lower temperatures to reduce the rates of
reaction as it makes the time difference • When different structural isomers are tested, the pattern is
between the halogenoalkanes larger, giving a tertiary is the quickest, followed by secondary and lastly
lower uncertainty primary Apparatus
250 cm3 conical flask 12 test tubes and bungs
Safety
[• 1-chlorobutane 1-bromobutane 1-iodobutane
Wear eye protection and suitable chemical resistant gloves 2-bromobutane )
Avoid skin contact with reactants and products 2-bromo-2-methylpropane
There must be no naked flames in the vicinity as halogenoalkanes and ethanol are flammable 0.05 mol dm-3 silver nitrate solution
15 cm3 ethanol Dropping pipettes
The laboratory needs to be well ventilated to prevent the inhalation of fumes
10 cm3 measuring cylinder Stop clock Kettle
 CORE PRACTICAL 6
Exerimental Obiective
• To produce and purify a sample of 2-chloro-2-methylpropane
Method
Diagram, Key Points and Errors
Pour 10 cm3 of 2-methylpropane-2-ol and 35 cm3 of
A weaker base is used to prevent hydrolysis of the
concentrated hydrochloric acid in to a large conical
halogenoalkane
flask and swirl
If sodium hydroxide was used, it could react with the
Place the bung in the mouth of the flask and swirl again.
product via nucleophilic substitution
Remove the bung to release the pressure.
The equation for this reaction is:
Continue this for approx. 20 minutes until two layers
(CHs) COH + HCI -> (CHs) CCI + H2O
begin to appear
Be aware that some product may be lost when
Add approx. 6 g of anhydrous calcium chloride and swirl
transferring liquids between the different vessels
until dissolved - this will ensure all unreacted alcohol
used
goes in to the bottom aqueous layer and not the top
organic layer Safety
Transfer the reaction to a separating funnel and allow it This procedure requires the use of a working fume
to settle in to two layers. Run off and discard the cupboard
lower layer but keep the upper layer Wear eye protection - goggles are preferred
Add approx. 10 cm° sodium hydrogencarbonate solution to Avoid skin contact with the reactants and products -
the separating funnel and swirl whilst releasing the wear gloves
pressure. Run off and discard the lower aqueous Avoid inhaling vapours
layer and repeat. The product of the distillation process is flammable
Run off the organic layer in to a small conical flask and The fumes from the concentrated hydrochloric acid are
add a spatula of anhydrous sodium sulfate. Swirl and toxic and corrosive and must not be inhaled, especially
leave until the mixture looks completely clear by anyone with a respiratory problem
Decant the organic liquid in to a 50 cm3 pear-shaped
flask and set up for distillation
Collect the fraction boiling between 50 °C and 52 °C
Analyse the sample by adding 5 cm§ ethanol and 1 cm?
sodium hydroxide and warm in a water bath
Add excess nitric acid and a few drops of silver nitrate
and record the observations

CORE PRACTICAL 7

Experimental Objective
To oxidise propan-1-ol to produce propanal by heating and distillation
To oxidise propan-1-ol to produce propanoic acid by heating under reflux and distillation

Background
Primary alcohols, such as propan-1-ol can be oxidised to aldehydes which can then be oxidised further to produce
carboxylic acids
Each can then be analysed using chemical tests.and/or spectroscopy to be identified

Safety
Wear goggles and chemical resistant gloves
Propan-1-ol and propanal are flammable
Avoid skin contact with reactants and products
Method - Propanal
Add 20 cm3 acidified potassium dichromate(VI) to a pear-shaped flask and cool using an ice water bath
Set the the flask for distillation and add some anti-bumping granules (for smoother boiling)
Measure 1.5 cm3 propan-1-ol in to a measuring cylinder and add 5 ст3 distilled water
Using a pipette, add the propan-1-ol solution slowing in to the pear shaped flask
When the propan-1-ol is added, cool the flask to room temperature
Light a burner under the flask and gently heat
Collect the colourless liquid given off in a test tube that is immersed in cold water

Method - Propanoic Acid

Add 20 cm3 acidified potassium dichromate (VI) to a pear-shaped flask and cool using an ice water bath
Set the the flask for reflux and add some anti-bumping granules (for smoother boiling)
Measure 1.5 cm3 propan-1-ol in to a measuring cylinder and add 5 cm3
distilled water
Using a pipette, add the propan-1-ol soliton slowing in to the pear shaped flask
When the propan-1-ol is added, cool the flask to room temperature
Light a burner under the flask and gently heat under reflux for 30 mins
Distil the product using the distillation apparatus. Collect the colourless liquid given off in a test tube that is
immersed in cold water
Method - Testing for Propanoic Acid
Silver Mirror - Tollens Reagent
Add 5 drops of sodium hydroxide solution to 2 cm3 of silver nitrate solution
Add just enough ammonia solution to dissolve the precipitate
Add 10 drops of this to the distillate, if propanoic acid has been made a silver mirror will not appear on the walls of
the test tube
* Magnesium Ribbon
Add a small piece of magnesium ribbon to the distillate
Propanoic acid will react with magnesium to produce effervescence
* Sodium hydrogencarbonate
Add a spatula of sodium hydrogencarbonate to the distillate
Propanoic acid will react with sodium hydrogencarbonate to produce effervescence
Fehling's Solution
Add 1 cm' Fehling's solution to 1 cm3 of the distillate and place in hot water
If no colour change is seen, propanoic acid has been formed

Key Points
When oxidising alcohols, it is important to control the conditions as these will dictate the products that are formed
The equation for these reactions is:
CH CH2CH2OH + [O] -> CH CH2CHO + H20
CH CH,CHO + [0] -> CH CH2COOH
Carboxylic acids are weak acids however they still react in the same way as other acids such as hydrochloric acid
CORE PRACTICAL 8
Results - Inorganic Tests
Objectives Flame tests
Experimental Obiective Flame tests may be carried out by using a clean
• To identify several unknown colourless liquids and nichrome wire to mix a sample of a solid compound
inorganic solids with a few drops of concentrated hydrochloric
acid. The wire is then held at the edge of a hot
Background Bunsen flame and the colour observed.
Chemical tests can be used to identify different
molecules or functional groups within a molecule
Further analvsis such as spectroscopy will usually follow
these tests for organic substances

Safety
Wear eye protection
Avoid skin contact with reactants and products
Ammonia solution gives off ammonia gas which should
not be inhaled by anyone, especially those with
respiratory problems
Ethanol is flammable
Silver nitrate solution
Method Chemical Tests Aqueous silver nitrate is used to test for the presence of
Flame test to identify cations halide ions in solution.
Sodium hydroxide test to identify cations Anions such as carbonate that would form precipitates
Silver nitrate test to identify halide ions with silver nitrate are removed by adding dilute nitric
Barium nitrate test to identify sulfate ions acid before the silver nitrate.
Hydrochloric acid test to identify carbonate ions The identity of the halide may be confirmed by adding
Use the results to identify each unknown inorganic aqueous ammonia to the silver halide.
substance
Bromine water test for alkenes
Tollens/Fehling's/Potassium dichromate(VI) for aldehydes
Hydrochloric acid or ethanol test for carboxylic
acids
Use the results to identify each unknown organic
Barium chloride solution
Aqueous barium chloride forms precipitates with a number of anions but is usually used as the
test for the sulfate(VI), SO4?- anion.
When dilute hydrochloric acid is added to the anion solution before the addition of aqueous
barium chloride then only the sulfate(VI) anion will form a precipitate.

Concentrated sulfuric acid

When a few drops of concentrated sulfuric acid are added to a solid halide the observed products may be used
to identify the halide ion.
The test must be carried out on a small scale and in a fume cupboard.
The gaseous products in brackets will not be observed since they are colourless.

Displacement of halide ions

When aqueous chlorine is added to a solution of a bromide or an iodide then bromine or iodine is displaced.
When aqueous bromine is added to a solution of an iodide then iodine is displaced.
The formation of aqueous solutions of bromine or iodine may be used as a test for the bromide and iodide ions.
If an organic solvent such as hexane is added to the reaction mixture the bromine or iodine dissolves in the
organic layer.
 HEAT

Gases or vapours may be given off on heating a solid inorganic compound.

Ignition
Igniting an organic compound on a crucible lid in a fume cupboard may provide evidence for the identity of
the compound.