CHEMISTRY/GRADE 9

EXPERIMENTAL TECHNIQUES

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EXPERIMENTAL DESIGN

Apparatus used to measure Time, Temperature, Mass & Volume

Time

 Time can be measured using a stopwatch or stopclock which are usually

accurate to one or two decimal places.
 The units of time normally used are seconds or minutes although other units
may be used for extremely slow reactions (e.g. rusting).
 1 minute = 60 seconds

Stopwatch
Temperature

 Temperature is measured with a thermometer which can normally give readings

to the nearest degree Celsius.
 The units of temperature are degrees Celsius (ºC).

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Mass

 Mass is measured using a digital balance which normally give readings to two
decimal places.
 The standard unit of mass is kilograms (kg) but in chemistry grams (g) are most
often used.
 1 kilogram = 1000 grams.

Weighing balance

Volume-liquids

 The volume of a liquid can be determined using several types of apparatus,

depending on the level of accuracy needed.
 For approximate volumes where accuracy isn´t an important factor, measuring
cylinders are used. These are graduated (have a scale so can be used to
measure) and are available in 25 cm3, 50 cm3, 100 cm3 and 250 cm3.
 Pipettes are the most accurate way of measuring a fixed volume of liquid,
usually 10 cm3 or 25 cm3
 Burettes are the most accurate way of measuring a variable volume of liquid
between 0 cm3 and 50 cm3 (e.g. in a titration).

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Volume-gases

 The volume of a gas sometimes needs to be measured and is done by

collecting it in a graduated measuring apparatus.
 A gas syringe is usually the apparatus used.
 A graduated cylinder inverted in water may also be used, provided the gas isn’t
water-soluble.
 If the gas happens to be heavier than air and is colored, the cylinder can be
used upright.

Diagrams of the set-up for experiments involving gas collection

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Advantages and disadvantages of experimental methods and
apparatus

 While measuring volumes, use pipette / burette in place of a measuring cylinder

since they are more accurate and precise than that of a measuring cylinder.
 Experimental data collection processes can be repeated to get an accurate
result by comparing data and converting the values into an average value.
 Experiments involving measuring temperature can use insulators such as
polystyrene objects to prevent loss of heat to the surrounding.

Acid–base titrations

 Titration is a technique used that can be used to analyse the concentrations of
substances in solution using a standard solution.

 One type of titration is acid-base titrations.

 Acid-base titration is a process that is used to find the amount of acid needed
to neutralize a known amount of alkali- or vice versa.
 The reaction is carried out in a carefully controlled way. The volumes are
measured using a pipette and a burette. Just sufficient acid is added to the
alkali to neutralize it and the end point is found using an indicator.

Indicator Colour in acid Colour in alkali

Phenolphthalein colourless pink
Methyl orange red yellow

Thymolphthalein indicator

Between pH of 9.3-10.5, its colorless and above this range, it is blue.

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Apparatus needed

1. Pipette: 2. Burette:

it is calibrated to measure
fixed It is calibrated to measure accurately a range of
volumes.
volumes such as 10cm3,
25cm3
3. volumetric flask 4. conical flask 5. pipette filler

Titration flask
To take liquid into a pipette
Used to prepare a
standard solution

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PROCEDURE
Using the pipette

 Wash 2 or 3 conical flasks with distilled water.

 Using a pipette filler suck some alkali into the pipette and
washes the inside by allowing it to drain out.
 Now using the pipette filler take alkali into the pipette up
to the graduation mark.
 Slowly allow the alkali to flow into one of the cleaned
conical flasks and hold the pipette in contact with the flask and
its tip for about 3seconds. This will allow proper amount of alkali
to be drawn out into the flask.

Using the burette

 Close the tap allow acid to wash the inside of the burette and
then run the acid out.
 Close the tap and clamp the burette with the stand.
 Pour the acid into the burette using a filter funnel up to 0 cm3 marked.
 Make sure there are no air bubbles trapped inside and the burette is ready for
use.

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Performing the titration

 Add few drops of indicator to the alkali in the conical flask.

 Place the flask under the tip of the burette and should be placed
under a white tile so that the colour change of the indicator
would be clear.
 Note the initial reading of the burette.

 Allow to flow the acid into the alkali and the shake the flask.

 Notice the change in colour of the indicator until you reach the
endpoint. The endpoint is where the indicator is just changing
from its colour in alkali to its colour in acid.

 Note the final reading of the burette in a table of results.

 Fill the burette and repeat the procedures to take 3 or 4 readings and then find
the average reading.

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Separation and purification

Terminologies involving separation and purification

 Solvent: a substance that dissolves a solute.
 Solute: a substance that is dissolved in a solvent.
 Solution: a mixture of one or more solutes dissolved in a solvent.
 Saturated solution: a solution containing the maximum concentration of a
solute dissolved in the solvent at a specified temperature.
 Residue: a substance that remains after evaporation, distillation, filtration or
any similar process.
 Filtrate: a liquid or solution that has passed through a filter.
Methods of Purification

The choice of the method of separation depends on the nature of the substances being
separated. All methods rely on there being a difference of some sort, usually in a
physical property such as b.p., between the substances being separated.

Mixtures of solids

 Differences in density, magnetic properties, sublimation and solubility can be

used
 For a difference in solubility, a suitable solvent must be chosen to ensure the
desired substance only dissolves in it and not other substances or impurities

Mixtures of liquids

 Immiscible liquids can be separated using

a separating funnel or by decanting (pouring
carefully)
 Examples include oil and water mixture.

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Crystallisation

 Used to separate a dissolved solid from a solution, when the solid is much
more soluble in hot solvent than in cold (e.g. copper sulphate from a solution of
copper (II) sulphate in water).
 The solution is heated, allowing the solvent to evaporate to leave a saturated
solution behind.
 Test if the solution is saturated by dipping a clean, dry, cold glass rod into the
solution. If the solution is saturated, crystals will form on the glass rod.
 The saturated solution is allowed to cool slowly and solids will come out of the
solution as the solubility decreases, and crystals will grow.
 Crystals are collected by filtering the solution.
 They are then washed with cold, distilled water to remove impurities and
allowed to dry.

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Simple Distillation

 Used to separate a liquid and soluble solid from a solution (e.g. water from a
solution of saltwater) or a pure liquid from a mixture of liquids.
 The solution is heated, and pure water evaporates producing a vapour which
rises through the neck of the round-bottomed flask.
 The vapour passes through the condenser, where it cools and condenses,
turning into pure liquid H2O which is collected in a beaker.
 After all the water is evaporated from the solution, only the solid solute will be
left behind.

Fractional distillation

 Used to separate two or more liquids that are miscible with one another (e.g.
ethanol and water from a mixture of the two).
 The solution is heated to the temperature of the substance with the lowest
boiling point.
 This substance will rise and evaporate first, and vapours will pass through a
condenser, where they cool and condense, turning into a liquid that will be
collected in a beaker.
 All of the substance is evaporated and collected, leaving behind the other
components(s) of the mixture.
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  For water and ethanol: ethanol has a boiling point of 78 ºC and water of 100 ºC.
The mixture is heated until it reaches 78 ºC, at which point the ethanol boils and
distils out of the mixture and condenses into the beaker.
 When the temperature starts to increase to 100 ºC heating should be stopped.
Water and ethanol are now separated.

Important points to remember in distillation and fractional distillation

1. Thermometer has to be placed such that the tip of the thermometer is exactly at
the entrance of the condenser (in order to measure boiling point correctly)
2. If the solution used is flammable, a water bath should be used.
3. The apparatus that collects the distillate should not be closed tightly, to prevent
the build up of pressure. This may send back the vapours into the heated mixture
instead of it being liquefied and collected.
 Condenser is placed in such a way that the ‘water in’ is at the bottom and
furthest from the reactor to ensure the condensation of any uncondensed gas
left near the out let at the distillate collector.

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Paper Chromatography

 This technique is used to separate substances that

have different solubilities in a given solvent (e.g. different coloured inks that
have been mixed to make black ink).
 A pencil line is drawn on chromatography paper and spots of the sample are
placed on it. Pencil is used for this as ink would run into the chromatogram
along with the samples.
 The paper is then lowered into the solvent container, making sure that the pencil
line sits above the level of the solvent so the samples don´t wash into the
solvent container.
 The solvent travels up the paper by capillary action, taking some of the coloured
substances with it.
 Different substances have different solubilities so will travel at different rates,
causing the substances to spread apart. Those substances with higher
solubility will travel further than the others.
 This will show the different components of the ink / dye.

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Interpret Simple Chromatograms

 If two or more substances are the same, they will produce identical
chromatograms. 
 If the substance is a mixture, it will separate on the paper to show all the
different components as separate spots.
 An impure substance will show up with more than one spot, a pure substance
should only show up with one spot.

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Assessing Purity

 Pure substances melt and boil at specific and sharp temperatures. Eg water
has a boiling point of 100°C and a melting point of 0°C.
 Mixtures have a range of melting and boiling points as they consist of different
substances that melt or boil at different temperatures.
 Melting and boiling points data can therefore be used to distinguish pure
substances from mixtures.
 An unknown pure substance can be identified by experimentally determining its
m.p and b.p and comparing to data tables.
 Mixtures melt over a range of temperatures as they contain two or more
substances.

Importance of Purity

 A pure substance consists of only one substance and contains nothing else.
 To have a pure substance for food and drugs is very important as impurities
could be dangerous even in small amounts.
 Melting and boiling point analysis is routinely used to assess the purity of food
and drugs.
 For example, if a sample of water melts at exactly 0°C and boils at exactly
100°C then the water is pure.
 If the melting and boiling points of the water aren’t these exact values then the
water must be impure and contain other substances i.e. it must be a mixture.

Retention Factor (Rf) Values

 These values are used to identify the components of mixtures.

 The Rf value of a particular compound is always the same
 Calculating the Rf value allows chemists to identify unknown substances
because it can be compared with Rf values of known substances under the
same conditions.

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Calculation

 Retention factor = distance moved by the substance ÷ distance moved by the

solvent
 The Rf value is a ratio and therefore has no units.

Locating Agents

 For chromatography to be useful the chemist needs to be able to see the

components move up the paper, which is not the case for invisible samples
such as proteins.
 Locating agents are substances which react with the sample and produce a
coloured product which is then visible.
 The chromatogram is treated with the agent after the chromatography run has
been carried out, making the sample runs visible to the naked eye.

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