Required Practical Tasks

1 – a) Making a standard solution

• Weigh the sample bottle containing the required mass of
solid on a 2 dp balance.
• Transfer to beaker and reweigh sample bottle.
• Record the difference in mass (this is called differential
weighing).
• Add 100cm3 of distilled water to the beaker. Use a glass
rod to stir to help dissolve the solid.
• Pour solution into a 250cm3 graduated flask via a funnel.
• Rinse beaker and funnel and add washings from the
beaker and glass rod to the volumetric flask.
• Make up to the mark with distilled water using a
dropping pipette for last few drops.
• Invert flask several times to ensure uniform solution.

Notes
• 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 meniscus sits on the line on the neck of the flask. With dark liquids
like potassium manganate it can be difficult to see the meniscus.

1 - b) Carrying out an acid-base titration

• Rinse equipment (burette with acid, pipette with alkali, conical
flask with distilled water).
• Pipette 25 cm3 of alkali into conical flask.
• Fill burette with acid.
• Make sure the jet space in the burette is filled with acid.
• Record initial burette reading.
• Add a few drops of indicator.
• Use a white tile underneath the flask to help observe the
colour change.
• Add acid to alkali whilst swirling the mixture and add acid
dropwise near endpoint.
• Stop adding acid when relevant colour change is observed.
• Record final burette reading.
• Repeat titration until at least 2 concordant results are
obtained (two readings within 0.1 of each other).

Notes
• If the jet space is not filled properly, you will obtain a larger than expected reading in your titration.
• Conical flasks are used in preference to beakers as it is easier to swirl.
• Indicators are usually weak acids so we just use a few drops. Adding too much will affect the titration result.
• 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]
2 – Measuring an enthalpy change
• Put polystyrene cup in a beaker for insulation and support.
• Clamp thermometer into place making sure the thermometer bulb
is immersed in liquid.
• Measure the initial temperatures of the solution (or both solutions
if 2 are used).
• Transfer reagents 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.
• Stir mixture.
• Measure highest/lowest temperature reached.

Notes
• If reaction is slow then then exact temperature rise can be hard to obtain as cooling occurs at the same time
as the reaction takes place – to counteract this, take readings at regular intervals, plot, and extrapolate the
temperature curve back
• Errors include: heat loss/gain, approximation of specific heat capacity of solution, neglecting specific heat
capacity of calorimeter, reaction incomplete, assuming density of solution the same as water

3 – Investigating how rate changes with temperature

e.g.
• Use a measuring cylinder to measure 10.0 cm3 of 0.05 mol dm-3 sodium thiosulfate solution into a conical
flask. Place this on a white tile with cross drawn.
• Record the initial temperature
• Add 1 cm3 of 1 mol dm-3 hydrochloric acid to the sodium thiosulfate solution and start timing.
• Record the time for the cross to disappear from view.
• Record the final temperature of the reaction mixture.
• Repeat (using water baths/ice) to obtain results for at least 5 different temperatures in total.
• Plot a graph of temperature v time, using the average temperature for each reaction.

Notes
• If the reaction is exothermic, you can only approximate the temperature of the reaction by taking a reading
of the initial temperature
4 – Carrying out test tube reactions to identify cations and anions in solution
Cation/Anion Reagent Result
Barium ion NaOH, dropwise NVC
until in excess NVC
Calcium ion NaOH, dropwise Slight white ppt.
until in excess Slight white ppt.
Magnesium ion NaOH, dropwise Slight white ppt.
until in excess White ppt.
Strontium ion NaOH, dropwise Slight white ppt.
until in excess Slight white ppt.
Barium ion Dilute H2SO4 dropwise White ppt.
until in excess White ppt.
Calcium ion Dilute H2SO4 dropwise Slight white ppt.
until in excess Slight white ppt.
Magnesium ion Dilute H2SO4 dropwise Slight white ppt.
until in excess Colourless solution
Strontium ion Dilute H2SO4 dropwise White ppt.
until in excess White ppt.
Ammonium NaOH, gently heat, hold damp red litmus over Production of ammonia gas, litmus turns blue
Hydroxide Red litmus paper / UI paper Turns blue
Carbonate HCl, test gas with calcium hydroxide solution Effervescence, CO2 gas produced, limewater
(limewater) turns cloudy
Sulfate HCl then barium chloride Production of white precipitate
Chloride (aq) Nitric acid, then silver nitrate Production of white precipitate
Add dilute ammonia solution Precipitate dissolves
Bromide (aq) Nitric acid, then silver nitrate Production of cream precipitate
Add concentrated ammonia solution Precipitate dissolves
Iodide (aq) Nitric acid, then silver nitrate Production of pale yellow precipitate
Add concentrated ammonia solution No visible change
Chloride (solid) Add concentrated H2SO4 Effervescence
Test gas evolved with damp blue litmus paper Litmus turns red (HCl produced)
Bromide (solid) Add concentrated H2SO4 Effervescence, brown gas produced (Br2),
Test gas evolved with filter paper dipped in solution turns red/brown
acidified potassium dichromate solution
Iodide (solid) Add concentrated H2SO4 Brown gas produced (Br2), solution turns
Test gas evolved with filter paper dipped in red/brown
lead nitrate solution Paper turns black
5 – Distilling a product from a reaction
6 – Testing for alcohols, aldehydes, alkenes and carboxylic acids
Functional group Reagent Result
Alkene Bromine water Orange colour decolourises
Aldehyde Fehlings solution Blue solution to red precipitate
Aldehyde Tollen’s reagent Silver mirror formed
Carboxylic acid Sodium carbonate / sodium Effervescence, CO2 made
hydrogencarbonate
10 and 20 alcohol, and aldehyde Sodium dichromate and sulphuric acid Orange to green colour change
Chloroalkane Warm with silver nitrate Slow formation of white precipitate
(AgCl)
Bromoalkane Warm with silver nitrate Slow formation of cream precipitate
(AgBr)
Iodoalkane Warm with silver nitrate Slow formation of pale yellow
precipitate (AgI)
Acyl chloride Silver nitrate Vigorous reaction, steamy fumes of
HCl, rapid production of white
precipitate (AgCl)

7 – a) Measuring the rate of reaction by initial rates method

e.g.
• Measure 50 cm3 of the 1.0 mol dm–3 hydrochloric acid and add to conical flask.
• Set up the gas syringe in the stand.
• Weigh 0.20 g of magnesium.
• Add the magnesium ribbon to the conical flask, place the bung firmly into the top of the flask and start the
stopwatch.
• Record the volume of hydrogen gas collected in 30 seconds.
• Repeat using different concentrations of HCl.

7 - b) Measuring the rate of reaction by continuous monitoring method

e.g.
• Measure 50 cm3 of the 1.0 mol dm–3 hydrochloric acid and add to conical flask.
• Set up the gas syringe in the stand.
• Weigh 0.20 g of magnesium.
• Add the magnesium ribbon to the conical flask, place the bung firmly into the top of the flask and start the
stopwatch.
• Record the volume of hydrogen gas collected every 15 seconds for until the reaction is finished.

8 – Measuring the EMF of an electrochemical cell

e.g.
• Clean a piece of copper and a piece of zinc using fine grade sandpaper.
• Degrease the metal using some cotton wool and propanone.
• Place the copper into a 100 cm3 beaker with about 50 cm3 of 1 mol dm-3 CuSO4 solution.
• Place the zinc into a 100 cm3 beaker with about 50 cm3 of 1 mol dm-3 ZnSO4 solution.
• Lightly plug one end of the plastic tube with cotton wool and fill the tube with the solution of 2 mol dm-3
NaCl provided.
• Plug the free end of the tube with cotton wool. Join the two beakers with the inverted U-tube so that the
plugged ends are in the separate beakers.
• Connect the Cu(s)|Cu2+(aq) and Zn(s)|Zn2+(aq) half-cells by connecting the metals (using the crocodile clips
and leads provided) provided to the voltmeter and read off the voltage.
9 – Investigating how pH changes in weak acid/strong base and strong
acid/weak base reactions
• Measure initial pH of the alkali
• Add acid in small amounts noting the volume added
• Stir mixture to equalise the pH
• Measure and record the pH
• When approaching endpoint add in smaller volumes of acid
• Add until acid in excess

Notes
• Calibrate pH meter first by measuring a known pH buffer solution (necessary
because pH meters can lose accuracy on storage)
• Improve accuracy by maintaining constant temperature

10 – a) Preparing a pure organic solid and testing its purity

Recrystallisation

Step Reason
1. Dissolve the impure compound in a minimum An appropriate solvent is one which will dissolve both
volume 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 This step will remove any insoluble impurities and
quickly. 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 The water pump connected to the Buchner flask
out crystals reduces 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

Notes
• Loss of yield from: losing crystals by filtering and washing, product staying in solution after recrystallization,
side reactions

Measuring melting point (to determine purity)

Melting point can be measured in an electronic melting point machine or by using a practical set up where the
capillary tube is strapped to a thermometer immersed in some heating oil.
• Put a small amount of the salt into a capillary tube.
• Heat up the tube, heating slowly near the melting point

Notes
• A pure sample will have a sharp melting point at the same value as that quoted in data books
• If impurities are present the melting point will be lowered and the sample will melt over a range of several
degrees Celsius.
10 – b) Preparing a pure organic liquid

Purifying the liquid

• Put the distillate of impure product into a separating funnel

• Wash product by adding either
o sodium hydrogencarbonate solution , shaking and releasing the pressure from CO2 produced.
o Saturated sodium chloride solution
• Allow the layers to separate in the funnel, and then run and discard the aqueous layer.
• Run the organic layer into a clean, dry conical flask and add three spatula loads of drying agent (anhydrous
sodium sulphate) to dry the organic liquid.
• Carefully decant the liquid into the distillation flask
• Distill to collect pure product

Notes
• Sodium hydrogencarbonate will neutralise any remaining acid
• Sodium chloride will help separate the organic layer from the aqueous layer
• The drying agent should:
o Be insoluble in the organic liquid
o Not react with the organic liquid
11 – Carrying out test tube reactions to identify transition metal ions in
solution
• Measure 3 samples of each unknown metal ion
• To the first test tube, add a few drops of sodium hydroxide solution
o add more sodium hydroxide solution until in excess
• To the second test tube, add a few drops of ammonia solution
o add more ammonia solution until in excess
• To the third test tube, add a few drops of sodium carbonate solution

Metal-aqua ion OH- (aq)/ NH3 (aq) XS OH-(aq) XS NH3 (aq) Na2CO3 (aq)
[Cu(H2O)6]2+ [Cu(H2O)4(OH)2] No visible change [Cu(H2O)2(NH3)4]2+ CuCO3
Blue solution Blue precipitate Deep blue solution Green-blue precipitate
[Fe(H2O)6]2+ [Fe(H2O)4(OH)2] No visible change No visible change FeCO3
Green solution Green precipitate Green precipitate
[Al(H2O)6]3+ [Al(H2O)3(OH)3] [Al(H2O)2(OH)4]- No visible change [Al(H2O)3(OH)3]
Colourless solution White precipitate Colourless solution White precipitate, bubbles
of CO2
[Fe(H2O)6]3+ [Fe(H2O)3(OH)3] No visible change No visible change [Fe(H2O)3(OH)3]
Yellow solution Brown precipitate Brown precipitate, bubbles
of CO2

12 – Separation of species by thin-layer chromatography

Step Reason
1. Wearing gloves, draw a pencil line 1 cm above the Gloves will prevent contamination from the hands.
bottom of a TLC plate and mark spots for each sample, The pencil line will not dissolve in the solvent
equally spaced along line.
2. Use a capillary tube to add a tiny drop of each Too big a drop will cause different spots to merge
solution to a different spot and allow the plate to air
dry.
3. Add solvent to a chamber or large beaker with a lid If the solvent is too deep it will dissolve the sample
so that is no more than 1cm in depth. spots from the plate
4. Place the TLC plate into the chamber, making sure A lid will prevent evaporation of toxic solvent
that the level of the solvent is below the pencil line.
Replace the lid to get a tight seal.
5. When the level of the solvent reaches about 1 cm You will get more accurate results if the solvent rises to
from the top of the plate, remove the plate and mark near the top of the plate, but this is not necessary; Rf
the solvent level with a pencil. Allow the plate to dry in values can be calculated regardless
the fume cupboard. A fume cupboard must be used as the solvent is toxic
6. Place the plate under a UV lamp. Draw around them The spots are colourless so UV is needed to see them
lightly in pencil.
7. Calculate the Rf values of the observed spots.

Notes
• Spraying ninhydrin and heating for 10 minutes will cause red-blue spots to appear
• Ninhidrin is necessary as amino acids are transparent. An alternative is to use a plate impregnated with
fluorescent dye.
• Each amino acid has its own Rf value