Core Practicals

Gas syringe potential errors:
- Gas escapes before bung inserted

- Syringe sticks
- Some gases like carbon dioxide or sulphur dioxide are soluble in water so the true
amount of gas is not measured
CP1: Measure the molar volume of a gas

Heating in a crucible
- Large amounts of hydrated calcium carbonate should not be used in this experiment
as the decomposition is likely to be incomplete
- Crucible needs to be dry – wet crucible would give an inaccurate result. Would cause
mass loss to be too large as the water would be lost when heating
- Lid = improves accuracy of the experiment as it prevents loss of solid from the
crucible but should be loose fitting to allow gas to escape
CP2: Make up a volumetric solution and carry out a simple acid-base titration
Dilutions
- Using a volumetric pipette is more accurate than a measuring cylinder because it has
a smaller uncertainty
CP3: Make up a volumetric solution and carry out a simple acid-base titration
- Substance that we don’t know the concentration of is put in the conical flask, other
substance is in the burette
Burette
- 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
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
o Doesn’t affect the titration reading as water does not react with the reagents
or changes the number of moles of acid added
Reducing uncertainties in a titration
- Make 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
CP4: Investigation of the rates of hydrolysis of some halogenoalkanes

Nucleophile
- Water is a poor nucleophile but it can react slowly with haloalkanes in a substitution
reaction
CP5: Oxidation of an alcohol

Distillation:
- Water goes in the bottom of the condenser to go against gravity – allows more
efficient cooling and prevents backflow of water
- Electric mantle – used to heat organic chemicals (highly flammable)
Reflux:
- No stopper should be placed – build-up of pressure
- Anti-bumping granules – promote smooth boiling, making small bubbles form
instead of large bubbles
- Making sure that the apparatus is sealed – otherwise gas will escape
Purifying an organic liquid:
- The layer with lower density will be the upper layer – usually the organic layer
- Sodium hydrogencarbonate added – reacts with HCl (neutralises it)
- Shake the mixture in the separating funnel, open the tap – release CO2 (prevent
build-up of pressure)
- Adding a drying agent (eg/anhydrous sodium sulphate) – remove water
CP6: Chlorination of 2-methylpropan-2-ol using concentrated HCl

Preparing and purifying an ester:
- Sulfuric acid is a catalyst – adding conc. H2SO4 is an exothermic reaction – to prevent
uncontrolled boiling over add drop by drop (or put in water bath ๗
- In reflux the reactant vapours of volatile compound are condensed and returned to
the reaction mixture.
- Sodium carbonate – reacts with unreacted acid and remaining catalyst still present
after distillation
- Calcium chloride – drying agent therefore the liquid will appear clean when dry
- Anti-bumping granules
CP7 + 15: Analysis of some inorganic unknowns

Testing for NH4+:
- Alkaline ammonia gas is released which turns the red litmus paper blue
Testing for SO4 2-:
- Simplest ionic equation
Ba2+ (aq) + SO42-(aq)  BaSO4 (s)
Reaction with 2,4-DNPH:
- 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-DNPH.
Compare melting point with known values in database.
CP8: To determine the enthalpy change of a reaction using Hess’s Law

Errors:
- Energy loss from surroundings
- Approximation in specific heat capacity of solution
- Neglecting the specific heat capacity of the calorimeter
- Reaction or dissolving may be incomplete
- Density of solution is taken up to be the same as water
Errors from measuring enthalpies of combustion using flame calorimetry:
- 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
CP9: Finding the Ka value for a weak acid – titration curves

Calibrate:
- Calibrate meter first by measuring known pH of a buffer solution. This is necessary
because pH meters can lose accuracy on storage
CP12: Prepare a transition metal complex

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%
Purifying an organic solid: Recrystallisation

Step Reason
1. Dissolve the solid in the minimum An appropriate solvent is one which will
volume of hot solvent dissolve both 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. Filter the solution while hot To remove any insoluble impurities, heat
will prevent crystals reforming during
filtration
3. Cool the filtrate So that, as solubility drops on cooling, the
solid will crystallise out.
4. Filter at the pump and wash with a To separate the crystals from the solvent;
little cold solvent any soluble impurities remain dissolved,
washing removes traces of the solvent with
dissolved impurities in it
5. Blot the crystals dry between filter
papers
Loss of yield in this process:
- Crystals lost when filtering or washing
- Some product stays in solution after recrystallisation
- Other side reactions occurring
CP16: The preparation of aspiring

Measuring melting point:
- If impurities are present the melting point will be lowered and the sample will melt
over a range of several degrees
- Comparing an experimentally determined melting point value with one quoted in a
data source will verify the degree of purity
Separation of species by TLC:
- Pencil line: will not dissolve in the solvent
- Tiny drop – too big a drop will cause different spots to merge
- Depth of solvent – if the solvent is too deep it will dissolve the sample spots from the
plate
- Lid – to prevent evaporation of toxic solvent
- Dry in a fume cupboard as the solvent is toxic
- UV lamp used if the spots are colourless and not visible
Separation by chromatography depends on the balance between solubility in the moving
phase and retention in the stationary phase
- If the stationary phase was polar and the moving phase was non-polar. Then the non-
polar compounds would pass through the plate more quickly than polar compounds
as they would have a greater solubility in the non-polar moving phase.
-

Core Practicals

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Gas syringe potential errors:

- Gas escapes before bung inserted

CP1: Measure the molar volume of a gas

CP4: Investigation of the rates of hydrolysis of some halogenoalkanes

CP5: Oxidation of an alcohol

CP6: Chlorination of 2-methylpropan-2-ol using concentrated HCl

CP7 + 15: Analysis of some inorganic unknowns

CP8: To determine the enthalpy change of a reaction using Hess’s Law

CP9: Finding the Ka value for a weak acid – titration curves

CP12: Prepare a transition metal complex

Purifying an organic solid: Recrystallisation

CP16: The preparation of aspiring

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