CAIE IGCSE Chemistry

12.1 Experimental design

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Name appropriate apparatus for the measurement of time, temperature,
mass and volume

Measuring time
Stopwatches- The time taken for a reaction to occur can be measured or controlled
by a stopwatch. The user can set a certain fixed time in experiments where time
intervals are a controlled variable, e.g. 30s. This apparatus is more accurate than
use of a analogue clock as most have a more precise measurement, e.g. to the
nearest millisecond

Measuring temperature
Thermometer- Temperature can be measured using a thermometer, liquid-in-glass
thermometers are commonly used in school laboratories due to their ease of use and
low expense. They usually have an uncertainty of ±0.5°C.

Measuring mass
Measuring balance- The mass of an object or a substance can be measured using
a digital balance, commonly giving readings to 2 decimal places. Before every use,
the balance should be tared (set to zero) and once the object is placed on the centre
of the balance, it should be given time for the reading to settle on a stable
measurement before it is recorded

Measuring volume of liquids

Burettes- The volume of a liquid is measured using a burette, commonly used in
titrations. 0.00cm3 is at the top of the burette column so when a measurement is
taken, the scale is read from top to bottom.

Volumetric pipettes- A specific, fixed volume of a liquid can be measured using a

volumetric pipette. A pipette filler is used to draw the liquid into the volumetric
pipette. Commonly used in titrations, 10cm3 and 25cm3 can be measured and
delivered using the volumetric pipette that has this volume marked.

Measuring cylinder- An approximate volume of a liquid can be measured using a

measuring cylinder. They are less accurate than volumetric pipettes, but measuring
cylinders come in a range of sizes (from 10cm3 to 1L) and are simpler and quicker to
use.

Measuring volume of gases

Gas syringe- Gas syringes can be used to collect gas produced from a chemical
reaction, measuring volumes of gas or for delivering a gas to a closed system.

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Suggest advantages and disadvantages of experimental methods and
apparatus

Advantages and disadvantages of apparatus

Apparatus Advantages Disadvantages

Stopwatch Can measure time intervals Accuracy of stopwatch reading

to a high level of precision depends on the reaction time of the
as some can measure to a user so human error is introduced
hundredth of a second

Thermometer Ease of use and cheap to Liquid-in-glass thermometers

acquire (commonly used in school labs)
have limited temperature ranges,
lower precision compared to digital
temperature probes and parallax
error can occur

Measuring Speed of readings to a high Sensitive to environmental factors

Balance level of accuracy, e.g. to such as air currents and fluctuations
micrograms in temperature in the lab

Burette Wide range of burettes so Meniscus reading errors can occur if

can measure accurate user does not view the
volumes and a range measurement at eye level

Volumetric Can accurately measure a Limited to measuring only one fixed

pipettes specified volume volume, e.g. 25cm3 volumetric
consistently pipettes

Gas syringe Can measure volumes of Gases in the closed system can
gas to a high level of become sensitive to environmental
accuracy factors such as temperature or
pressure changes

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Experimental methods

To comment on the advantages and disadvantages of an experimental method, you

must access and comment on the following questions:

- The advantages and disadvantages of the apparatus used, e.g. ‘a measuring

cylinder has a less accuracy than a volumetric pipette’
- How many repeats have been done? Were the answers similar or different?
The closer the repeat readings are, the more precise the result.
- Were there any controlled variables to ensure that the independent variable is
the only factor causing a change? For example, if temperature is the
independent variable, examples of controlled variables can include volumes
and concentrations of any solution, pressure or pH of a solution.

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 CAIE IGCSE Chemistry

12.2 Acid–base titrations

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Describe an acid–base titration to include the use of a: (a) burette (b)
volumetric pipette (c) suitable indicator

Titrations are carried out to calculate the concentration of an acid or an alkali by

determining how much acid is needed to neutralise an alkali (or vice versa).
Titrations can also be done to prepare a soluble salt from the reaction between an
acid and dilute solution of alkali

Apparatus required
● 50cm3 burette
● 25cm3 volumetric pipette
● Pipette filler
● 250cm3 conical flask
● Suitable indicator, e.g. phenolphthalein
● Sodium hydroxide solution of concentration 0.1mol/dm3
● Sulfuric acid of unknown concentration
● Clamp stand
● White tile
● Funnel

Method
1. Use the pipette filler to draw up 25cm3 of sodium hydroxide solution into the
volumetric pipette and add this to the conical flask.
2. With the burette clamped onto the stand, use the funnel to fill the burette with
sulfuric acid.
3. Place an empty beaker underneath the tap and release a small amount of the
acid to prevent any air bubbles.
4. Record the initial volume on the burette to the nearest 0.05cm3, taking care to
ensure that you are eye-level to the meniscus.
5. Place the conical flask underneath the tap on top of a white tile to allow any
colour changes to be more visible.
6. Add 3 drops of the phenolphthalein indicator into the conical flask and swirl
gently to mix (phenolphthalein is pink when alkaline and colourless when
acidic).
7. Run the acid from the burette into the alkali, whilst swirling the solution. As the
endpoint is approached (the colour of the solution becomes pale pink), reduce
the increments and quickly stop the titration when it is reached.
8. Record the final volume on the burette in your table to the nearest 0.05cm3.
9. Calculate the rough titre using the following equation:
Final volume - Initial volume = Titre volume
10. Repeat the experiment until 2 concordant titres are found (results that are
within 0.1cm3 of each other excluding the rough titration).

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 11. Calculate the mean titre volume using the 2 concordant titre volumes.

Example table of results

Titration Initial volume /cm3 Final volume /cm3 Titre /cm3

Rough 0.20 24.65 24.45

1 0.35 25.20 24.85

2 1.10 25.70 24.60

3 0.90 25.85 24.95

Mean titre: (24.85 + 24.95) / 2 = 24.9 cm3

Describe how to identify the end-point of a titration using an indicator

Indicators are used to identify the end-point of a titration as a sudden colour change
will occur when the solution goes from acid to alkali (or vice versa). The two most
commonly used acid-base indicators are:

1. Phenolphthalein: pink in alkali -> colourless in acid

2. Methyl orange: yellow in alkali -> red in acid

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 CAIE IGCSE Chemistry

12.3 Chromatography

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Describe how paper chromatography is used to separate mixtures of
soluble coloured substances, using a suitable solvent

- Paper chromatography is a separation technique used to separate mixtures of

soluble substances depending on their different solubilities
- Chromatography involves 2 different phases: the stationary phase and the
mobile phase
- The stationary phase is usually the chromatography paper
- The mobile phase is the solvent that carries the different substances with it,
e.g. ethanol
- A more soluble substance will be more attracted to the mobile phase so will
travel further than a less soluble substance

Apparatus needed
● Chromatography paper
● Pencil
● Ruler
● Suitable solvent e.g. ethanol
● Suitable sized beaker
● Soluble coloured substance e.g. 2 coloured pens

Method
1. Draw a straight pencil line across, 1 cm from the base of the chromatography
paper
*Pencil is used since pen ink would dissolve along with the substance being
tested and disrupt the chromatogram.*
2. Mark evenly spaced spots of the coloured pens along the line
3. Add a small volume of solvent into the beaker, roughly less than 1 cm.
4. Place the chromatography paper into a beaker so it is stood upright, ensuring
the pencil line sits above the solvent.
5. Wait for the solvent to travel up the paper, carrying the different substances in
the pigments with it
6. Remove the paper and mark a line where the solvent went up to, this is
known as the solvent front and allow the chromatogram to dry

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Interpret simple chromatograms to identify:

Unknown substances by comparison with known substances

- When setting up the chromatography paper, place a spot of the unknown
substance alongside spots of known substances, evenly spacing them.
- Once the chromatogram has dried, the unknown substance will have
separated into its separate components if it is a mixture
- Identify the unknown substance by comparing its separate components with
the reference substances, as the spots that have the same solubility will be in
line with each other

Pure and impure substances

- An impure substance will show up with more than one spot on the
chromatogram
- A pure substance will show up with only one spot on the chromatogram

(Extended only) Describe how paper chromatography is used to separate

mixtures of soluble colourless substances, using a suitable solvent and a
locating agent

- Colourless mixtures of chemicals can be analysed if the ‘spots’ can be

coloured by a chemical or light treatment
- Examples include:
● Ninhydrin used with proteins – breaks them down into amino acids and
colours them purple
● UV light – fluoresce many colourless organic molecules

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NB: The knowledge names of specific locating agents is not required
- These are all known as locating agents, allowing Rf values to be taken and
(previously colourless) molecules to be identified

(Extended only) State and use the equation for Rf :

- To find the Rf value of a substance, use the following equation:

𝑑𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑡𝑟𝑎𝑣𝑒𝑙𝑙𝑒𝑑 𝑏𝑦 𝑠𝑢𝑏𝑠𝑡𝑎𝑛𝑐𝑒

𝑅𝑓 = 𝑑𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑡𝑟𝑎𝑣𝑒𝑙𝑙𝑒𝑑 𝑏𝑦 𝑠𝑜𝑙𝑣𝑒𝑛𝑡

- The distance travelled by the solute should be measured to the centre of the
solute spot
- Different compounds have different Rf values in different solvents, which can
be used to help identify the compounds
- Compounds in a mixture may separate into different spots depending on the
solvent but a pure compound will produce only one spot in all solvents

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 CAIE IGCSE Chemistry

12.4 Separation and purification

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Describe and explain methods of separation and purification using:

(a) A suitable solvent

- A solvent is a substance that dissolves a solute
- The type of solvent must be carefully chosen depending on the type of solute
that needs to be separated to ensure:
- No other impurities or components dissolve in the solvent
- Only the desired substance is dissolved in the solvent

(b) Filtration
- Filtration separates an insoluble solute, such as a precipitate, from a solution
- Filter paper is placed into a funnel, the small pores only allow liquids to pass
through
- The mixture is poured into a beaker through the funnel, leaving the solute
behind

(c) Crystallisation
- Crystallisation separates a soluble salt from the solution it is dissolved in
- Method:
- Heat the solution in a evaporating dish over a bunsen burner until
boiling
Specify that no more than half of the solution is boiled off before it is
removed from the heat
- Remove from the heat and allow the solution to cool and evaporate
- The saturated solution will leave behind crystals of the salt as it cools
- The crystals will grow and can be collected and allowed to dry

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(d) Simple distillation
- Simple distillation separates a solvent from a solution, e.g. producing water
from a salt solution
- Simple distillation works because the dissolved solute has a much higher
boiling point than the solvent, e.g. salt has a higher boiling point than the
water so the water will boil and evaporate first and the salt stays behind
- The water vapour will cool and condense as it travels through the condenser,
collecting in a separate flask
- The remaining solution becomes more concentrated in solute as the amount
of solvent in it decreases.

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(e) Fractional distillation
- Fractional distillation separates a pure liquid from a mixture of liquids, e.g.
separating water and ethanol.
- Fractional distillation works because the liquids have different boiling points,
e.g. pure ethanol boils at 78°C whereas water boils at 100°C.
- The mixture is heated to the boiling point of the liquid with the lowest boiling
point, which will evaporate first, pass through the condenser and collect in its
fraction. This process is repeated, until every component of the mixture has
evaporated in its associated boiling point and separated into its individual
fractions
- The many hydrocarbons in crude oil are separated using fractional distillation:
- Heated crude oil is piped in at the bottom of the fractionating column.
- The vaporised oil rises up the column and the various fractions are
constantly tapped off at the different levels where they condense.
- The fractions can be processed to produce fuels and feedstock for the
petrochemical industry.

Separating a mixture of gases

- To separate a mixture of gases, one method would be to cool the mixture to
convert the state from gaseous to liquid, then use fractional distillation to
separate the different gases into their individual components

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Suggest suitable separation and purification techniques, given information
about the substances involved

Method of What is separated

separation

Filtration Insoluble solute from a solution

Crystallisation Soluble solute from a solution (e.g. dissolved salt)

Simple distillation Solvent from a solution

Fractional Mixture of miscible (dissolved) liquids

distillation

Identify substances and assess their purity using melting point and boiling
point information

- Pure substances melt and boil at specific temperatures

- This melting and boiling points data can be used to distinguish pure
substances from mixtures (which melt over a range of temperatures due to
them consisting of 2 or more elements or compounds)
- To identify an unknown substance, the melting point or boiling point of the
substance can be tested experimentally and the value can be compared to
a database of the values of known substances
- To assess the purity of a substance, the melting point or boiling point of the
substance can be tested experimentally and the value is compared to the
database value. The more similar the value, the higher the purity of the
substance.

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 CAIE IGCSE Chemistry

12.5 Identification of ions and gases

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Describe tests to identify the anions:

Carbonates: CO3 2 –
- Carbonates react with dilute acids, i.e. nitric acid, to create carbon dioxide.
- This gas can be bubbled through limewater
- If the limewater goes cloudy, the gas is CO2 so a carbonate is present

Halides: Chlorides (Cl –) Bromides (Br –) Iodides (I –)

- First add dilute nitric acid to the sample, followed by silver nitrate solution
- Chlorides produce a white precipitate
- Bromides produce a cream precipitate
- Iodides produce a yellow precipitate

Nitrates: NO3 –
- Firstly, add aqueous sodium hydroxide to your unknown sample
- Then add aluminium powder or foil, and proceed to heat the mixture strongly.
- If nitrate ions are present, they will be reduced to ammonia, giving off
ammonia gas.
- This can be identified by testing it with damp red litmus paper, which will turn
blue in its presence.

Sulfates: SO4 2 –
- First add dilute hydrochloric acid, followed by barium chloride solution
- A white precipitate will form if sulfate ions are present in this solution

Sulfite: SO3 2–
- Add a dilute acid and heat gently
- Sulfur dioxide gas is given off
- Bubble this gas through aqueous potassium manganate(VII)
- There will be a colour change from purple to colourless if the sulfite ion is
present.

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Describe tests using aqueous sodium hydroxide and aqueous ammonia to
identify the aqueous cations:

Using aqueous dilute sodium hydroxide

Ions Observation after a few Observation after

drops of NaOH is added excess NaOH is added

Aluminium, Al 3+ White precipitate forms Precipitate redissolves

Ammonium, NH4 + Ammonia gas given off (how No change

to test is further below)

Calcium, Ca2+ White precipitate forms No change

Chromium(III), Cr3+ Grey-green precipitate forms Dark green solution forms

Copper(II), Cu2+ Blue precipitate forms No change

Iron(II), Fe2+ Green precipitate forms No change

Iron(III), Fe3+ Orange-brown precipitate No change

forms

Zinc, Zn2+ White precipitate forms Precipitate redissolves

Using aqueous ammonia

Ions Observation after a few Observation after

drops of ammonia is added excess ammonia is
added

Aluminium, Al 3+ White precipitate forms No change

Calcium, Ca2+ Very faint precipitate forms No change

Chromium(III), Cr3+ Grey-green precipitate forms No change

Copper(II), Cu2+ Light blue precipitate forms Precipitate dissolves to

form a dark blue solution

Iron(II), Fe2+ Green precipitate forms No change

Iron(III), Fe3+ Orange-brown precipitate No change

forms

Zinc, Zn2+ White precipitate forms Precipitate dissolves to

form a colourless solution

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 - Testing with both solutions can differentiate between the different cations, i.e.
there are 3 cations which all produce white precipitates:

1. Aluminium ions, Al 3+
2. Calcium ions, Ca2+
3. Zinc ions, Zn2+

- To distinguish Calcium ions (Ca2+)

The white precipitate formed when NaOH is added does not dissolve in
excess NaOH, whereas the hydroxide precipitates of aluminium and zinc do

- To distinguish Zinc ions (Zn2+)

The white precipitate formed when a few drops of ammonia is added to zinc
dissolves into a colourless solution when excess ammonia is added, but the
white precipitate of aluminium doesn’t dissolve

Describe tests to identify the gases:

Ammonia: NH3
- Turns damp red litmus paper blue

Carbon dioxide: CO2

- Bubble the gas through the limewater (calcium hydroxide)
- If carbon dioxide is present, the limewater will turn cloudy

Chlorine: Cl2
- When damp litmus paper is put into chlorine gas the litmus paper is bleached
and turns white

Hydrogen: H2
- Hold a burning splint at the open end of a test tube of the gas sample
- Creates a ‘squeaky pop’ sound if hydrogen gas is present

Oxygen: O2
- Insert a glowing splint into a test tube of the gas sample
- Splint relights if oxygen gas is present

Sulfur dioxide: SO2

- Bubble the gas through aqueous potassium manganate(VII)
- If sulfur dioxide gas is present, there will be a colour change from purple to
colourless

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Describe the use of a flame test to identify the cations:

A flame test could be used to identify the cations by distinguishing the colour of the
flame they produce

Cation Flame colour

Lithium, Li+ Crimson

Sodium, Na+ Yellow

Potassium, K+ Lilac

Calcium, Ca2+ Red

Barium, Ba2+ Yellow-green

Copper(II), Cu2+ Blue-green

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