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

• 1 minute = 60 seconds
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
Volumetric
MEASURING
flask
CYLINDER

• Burettes are the most accurate way of measuring • Volumetric pipettes are the most accurate way of measuring
a variable volume of liquid between 0 cm3 and 50 cm3  a fixed volume of liquid, usually 10 cm3 or 25 cm3.
• The tricky thing with burettes is to remember to read the • They have a scratch mark on the neck which is matched to the
scale from top to bottom as 0.00 cm3 is at the top of the bottom of the meniscus to make the measurement
column
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 be dissolved in the solution.
 SOLUBILITY AND TEMPERATURE
• FOR A SOLID SOLUTE, AS THE TEMPERATURE INCREASES SO DOES THE SOLUBILITY

Supersaturated solution
readily crystallizes
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 evaporation, Definition: Filtrate is a liquid or solution that has
distillation, filtration or any similar process 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
substances
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 solution
cools, indicating the
solution has reached its
crystallization point.
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
THINK!
3) After all the water is evaporated from the
Is the boiling point of solvent higher or lower than the boiling point of
solution, only the solid solute will be left behind
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
Thermometer Placed beside Ensures boiling
the arm of the point of the
flask, not dipped substance being
into solution distilled is
measured

Condenser Slopes Ensures pure

downwards solvent runs
downwards to
enter into the
conical flask

Cold water Ensures if water

enters jacket enters from the
from the bottom bottom, it fills
of the condenser the water jacket
completely for
efficient cooling
  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 R f 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 experimentally
determining its m.p and b.p and comparing to data tables
Which melting curve represents a
pure 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