EXPERIMENTAL

TECHNIQUES
AND CHEMICAL
ANALYSIS
EXPERIMENTAL
DESIGN
 MEASUREMENT

TIME
• Time can be measured using a stopwatch or stopclock
which are usually accurate to one or two decimal places
(0.01 s)

• The units of time normally used are seconds or minutes

although other units may be used for extremely slow
reactions (e.g. rusting)

• 1 h= 60 min
CALCULATION

Express both
the times in
seconds
 TEMPERATURE
• Temperature is measured with a thermometer or digital probe

• Laboratory thermometers usually have a precision of a half

(0.5oC) or one degree (very small changes can be observed. )

• Digital temperature probes are available which are

more precise than traditional thermometers and can often read to
0.1 oC

• Traditional thermometers rely upon the uniform expansion and

contraction of a liquid substance with temperature (alcohol or
mercury); digital temperature probes can be just as, if not,
more accurate than traditional thermometers

• The units of temperature are degrees Celsius (ºC) or Kelvin (K)

• Temp in K = Temp in oC + 273

 MASS
• Mass is measured using a
digital balance/electronic
which normally give readings to
two decimal places (0.01 g)

• Balances must be tared (set

to zero) before use

• The standard unit of mass is

kilograms (kg) but in
chemistry grams (g) are most
often used

• 1 kilogram = 1000 grams

 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 high accuracy is not an important factor, measuring
( or graduated) cylinders are used
• These are graduated (have a scale so can be used to measure) and are available
typically in a range of sizes from 10 cm3 to 1 litre (1 dm3)

Whichever apparatus you use, you may see

markings in ml(millilitre) which is the same as a
cm3
• 1 mL= 1 cm3
• 1 m3= 1000 dm3
• 1 dm3 = 1000 cm3
 VOLUME-LIQUIDS
Volumetr
MEASURING
ic flask
CYLINDER

• Burettes are the most accurate way of • Volumetric pipettes are the most accurate way of
measuring a variable volume of liquid between measuring a fixed volume of liquid, usually 10
0 cm and 50 cm
3 3
cm3 or 25 cm3.
• The tricky thing with burettes is to remember to • They have a scratch mark on the neck which is
read the scale from top to bottom as 0.00 matched to the bottom of the meniscus to make
Measuring Volume of Liquids
READING THE MENISCUS IN A BURETTE
 VOLUME-GASES

• The volume of a gas is measured 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 coloured, the cylinder can be used upright

 Collecting Gases and Measuring
Volume of gases
The gas syringe measures a
maximum volume of 100 cm3
 THINK

Volumetric pipette
Burette
SOLVE
 DISSOLVING
• solvent as a substance that dissolves a solute
• solute as a substance that is dissolved in a solvent
• solution as a mixture of one or more solutes dissolved in a solvent
 SATURATED SOLUTION
• During dissolving, particles of solvent
collide and surround the particles of
solute, gradually moving them away
until the particles are evenly spread
through the solvent.
• For each solute and solvent, there is a
limit to the mass of solute that will
dissolve in a particular volume of the
solvent. When no more solute will
dissolve, we say that the solution is
a saturated solution.
Definition: Saturated solution as a solution
containing the maximum concentration of
a solute dissolved in the solvent at a
specified temperature. No more solute can
 SOLUBILITY AND TEMPERATURE
• FOR A SOLID SOLUTE, AS THE TEMPERATURE INCREASES SO DOES THE SOLUBILITY

Supersaturated
solution readily
PURITY
Impurity: An
unwanted
substance,
mixed with the
substance you
want, is called
an impurity.
 SEPARATION AND
PURIFICATION
Separating:
• a solid from a liquid
• Solids
• A liquid from a
solution
• liquids
 SEPARATING MIXTURES
• A mixture consists of two or more different substances, not chemically
joined together
• The substances in a mixture can be elements, or compounds, or both.
Being part of a mixture does not change the chemical properties of the
substances that are in it.
• Mixtures can be separated by physical processes. These processes do not
involve chemical reactions, and no new substances are made.
• A pure substance is made up of one single element or compound.
 FILTRATION
• Used to separate an insoluble solid from a
mixture of a liquid solution (e.g. sand from a
mixture of sand and water, chalk from a mixture of
chalk and water).
• Filter paper is placed in a filter funnel above another
beaker
• The mixture of insoluble solid and liquid is poured
into the filter funnel
• Filter paper will only allow small liquid particles to
pass through in the filtrate
• Solid particles are too large to pass through the filter
paper so will stay behind as a residue
Definition: Residue is a substance that remains after Definition: Filtrate is a liquid or solution
evaporation, distillation, filtration or any similar process that has passed through a filter
 CRYSTALLISATION
• Used to separate a soluble solid from a solution, when the solid is more soluble in hot
solvent than in cold (e.g. copper sulphate crystals from a solution of copper (II) sulphate in
water)
• The solution is heated, allowing the solvent to evaporate leaving a saturated solution
behind
• The saturated solution is allowed to cool slowly and dissolved solid will come out of the
solution as the solubility decreases, and crystals will grow
• Crystals are collected by filtering the solution and are then washed with distilled water to
remove any impurities and then allowed to dry
 CRYSTALLISATION PROCESS

Cooling
decreases
the
solubility
of most
substance
s
How do we test for
a saturated
solution?

A clean glass rod

can be used to test
whether a solution
is saturated. If
dipped into the
solution, small
crystals will form
on the rod as the
FLOW CHART FOR STEPS IN OBTAINING COPPER (II)
SULPHATE CRYSTALS
 EVAPORATION TO DRYNESS
• For some substances, their solubility changes very little with temperature e.g. salt

• It is more suited to separate: Solutes that are thermally stable, which do not decompose under high heat e.g. sugar turns

into caramel upon heating. Separating salt and water can be done using this method.

• Sugar and ethanol mixture can also be separated in this way

• Solid(solute) used in this case will be less volatile than the solvent (higher boiling point than the solvent) and will remain

as a crystalline residue (sodium has a very high boiling point than water)

• Copper sulfate is an example of a solute which cannot be separated using the evaporation to dryness method. The blue

crystals easily break down to give a dull white-grey powder.

CRYSTALLISATION-COPPER SULFATE
SUBLIMATION OF IODINE
 SEPARATING IODINE FROM SAND USING
SUBLIMATION

• This method is used to separate a substance

that sublimes from the one that a high
melting point e.g. sand or sodium chloride
SEPARATING MIXTURES USING SUBLIMATION
AMMONIUM CHLORIDE AND CHALK
 SEPARATING SOLIDS-USING A SUITABLE
SOLVENT
• 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 boiling point between the substances being separated
• To separate a mixture of two solids, we use a solvent in which only one
solid is soluble
Mixtures of solids
• 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, e.g. to separate a
mixture of sand and salt, water is a suitable
solvent to dissolve the salt, but not the sand
 SEPARATION- MIXTURES OF LIQUIDS
• Immiscible liquids can be separated using
a separating funnel or by decanting (pouring carefully)
• Immiscible liquids are those which do not dissolve in each
other e.g. oil and water, kerosene and water, milk and
cream
SEPARATING A LIQUID FROM A SOLUTION-
SIMPLE DISTILLATION
Used to separate a pure solvent (liquid)
from a solution (e.g. drinking water from
a solution of saltwater) or a pure liquid
from a mixture of liquids with large
difference in their boiling points
1) The solution is heated and pure water
evaporates producing a vapour which
rises through the neck of the round-
bottomed flask
2) The vapour passes through
the condenser, where it cools and
condenses, turning into pure water which
is collected in a beaker as a distillate
3) After all the water is evaporated from THINK!
the solution, only the solid solute will be Is the boiling point of solvent higher or lower than
left behind the boiling point of the solute?
 THOUGHT PROCESS!
Q. In distillation set up, why is water inlet at the bottom
of the condenser and water outlet at the top?

This is so in order to provide longer

contact time of cold water in the
condenser with the inner tube
containing vapour. Hence, it provides
efficient cooling.
SIMPLE
DISTILLATI
ON
Apparatus Placement Reason
Thermomete Placed Ensures
r beside the boiling point
arm of the of the
flask, not substance
dipped into being
solution distilled is
measured
Condenser Slopes Ensures pure
downwards solvent runs
downwards
to enter into
the conical
flask

Cold water
enters jacket Ensures if
from the water enters
bottom of from the
the bottom, it
condenser fills the
water jacket
completely
 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)
• A more effective separation where the liquids are
closer in boiling points and a higher degree of
purity is required
• For example: water and ethanol where ethanol has a
boiling point of 78 ºC and water of 100 ºC.
• An additional column called a fractionating column is
attached and filled with glass beads to increase the
surface area for vapor to condense on
• 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
 FRACTIONAL DISTILLATION
• 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
 FRACTIONAL OR SIMPLE DISTILLATION?

WHICH TYPE OF DISTILLATION IS BEST TO

SEPARATE A MIXTURE OF TWO LIQUIDS?
• A mixture of two liquids can be separated by
either distillation method. However, simple
distillation requires very careful control of
the temperature.
• Fractional distillation is better if the two
liquids have very similar boiling points. If
simple distillation is used instead, the
distillate is likely to be a mixture of the two
liquids as both will evaporate when heated.
• An electric heater is safer to use when there
are flammable liquids present
• The separation of the components in
petroleum is achieved by fractional distillation
on an industrial scale
 PAPER CHROMATOGRAPHY
• This technique is used to separate a mixture of substances that have different solubilities in a
given solvent (e.g. different coloured inks that have been mixed to make black ink). To check the
purity of a substance
• 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 (1 cm) so the samples don´t wash into the solvent container
 PAPER CHROMATOGRAPHY

• 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
PAPER CHROMATOGRAPHY
 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
 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
• The Rf value is a ratio and therefore has
no units
Calculate the Rf values of the substance?

The Rf value of a
substance remains
constant as long as
the experiment is
carried out in the
same conditions
e.g. temperature
IDENTIFICATION OF AN UNKNOWN SUBSTANCE

• A paper chromatogram can also be used to identify substances by comparing them with
known substances. Two substances are likely to be the same if:
• they produce the same number of spots, and these match in colour
• the spots travel the same distance up the paper compared to reference spots (have
the same Rf value)
 LOCATING AGENTS

• Locating agents are substances

which react with an invisible sample

(proteins) 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

USES OF CHROMATOGRAPHY

• Separate the components in a sample e.g. dyes in ink, pigments in

plants etc
• Identify the components present in a sample
• Identify substances such as poisons, pesticides and drugs
• Determine whether a sample is pure
ASSESSING PURITY OF FOOD COLOURING
 IMPORTANCE OF PURITY
• A pure substance consists of only one substance.
• To have a pure substance for food (preservatives and dyes) 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

How can be sure that a

sample of water is
pure?
If the melting and boiling points of
the water aren’t these exact
values i.e. 0oC and 100oC then the
water must be impure and contain
other substances i.e. it must be a
mixture
 ASSESSING PURITY

• Pure substances melt and boil at specific and

sharp temperatures e.g. 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
Which melting
experimentally determining its m.p curve
and b.p and
represents a pure
comparing to data tables
substance?
EFFECTS OF IMPURITIES ON MELTING AND BOILING
POINT
• Impurities lower the melting point of a solid (range of temperatures)
• Impurities increase the boiling point of a liquid
THINK!
SEPARATING TECHNIQUES- A SUMMARY
 MORTAR AND PESTLE

Usage: to grind, mesh or crush

various ingredients. One of the key
applications and use of mortar and
pestle is to transform ingredients into
fine powder and paste
PAST PAPER PRACTICE
PAST PAPER PRACTICE
LABEL THE
DIAGRAM

WHAT IS THE
PURPOSE OF THE
FRACTIONATING
COLUMN?

WHY IS THE WATER

INLET PLACED AT THE
BOTTOM OF THE
CONDENSER?