Experimental techniques

and chemical analysis

Unit 14
Measurement

Variable Common apparatus for Common units of measurement

measurement

Time stopwatch s
mass Electronic balance Kg, g
volume Measuring cylinder, Cm3, dm3
pipette, burette
Temperature thermometer
Time - measurement
•Time is measured with a clock or digital stopwatch
•SI unit of time is the second (s)
•Other units are the hour (h) and the minute (min)
•1h = 60min=3600s
Temperature - measurement
•
Temperature -
measurement
Measurement of mass
Volume -
measurement
 Volume of liquids- measurement
3
• SI unit for volume is cubic metre (m ) – large unit
• Hence, we measure volume of liquids in cubic centimetres (cm3)
• Larger volumes are occasionally measured in cubic decimetres (dm3)
• 1dm3 = 1000cm3
Volume of liquids - measurement
apparatus accuracy
Measuring cylinder Approximately measures the volume of
the liquid to the nearest 0.5 cm3, ex:
24.0 or 32.5cm3
burette Accurately measures the volume of the
liquid to the nearest 0.05cm3 , ex: 23.00
or 35.45 cm3
pipette Accurately measures a fixed volume of
liquid, ex: 20.0 or 25.0 cm3
Volume of gases
- measurement
• Volume of gas is produced
in a chemical reaction is
measured with a gas
syringe
• Gas syringe measures gas
on a graduated scale
Collecting and measuring volumes of gases
• The method to collect a gas depends on

• (a) the solubility of the gas in water

• (b) the density of the gas compared to air

Collecting and measuring volume of gases
Collecting and measuring volumes of gases
1. Displacement of water: This method can be used for gases that
are insoluble or slightly soluble in water. Examples are hydrogen,
oxygen, and carbon dioxide
2. Downward delivery: This method is used to collect gases that are
soluble in water and denser than air. An example is chlorine. The
collection of chlorine gas should preferably be carried out in a
fume cupboard.
3. Upward delivery: This is used to collect gases that are soluble in
water and less dense than air. Ex: ammonia and hydrogen
4. Using a gas syringe: Gases can also be collected in gas syringe. This
is particularly useful when we want to collect and measure the
volume of gas over a period of time. Gas produced from the
reaction of substances in the conical flask is collected in the gas
syringe. This apparatus is useful in experiments on speed of
reaction.
Mixtures and pure substance
• Pure substance: is a single substance not mixed with anything else
• Ex: white sugar, copper (II) sulphate crystals

• Mixture: consists of 2 or more substances that are not chemically

combined together
• Ex: seawater is a mixture as it contains water, salt, and other
dissolved solids
• Milk is a mixture of fats and other solids in water
How are pure substances obtained?
• Mixtures can be easily separated into pure substances.
• This process is called purification.
• It is done by various physical methods without chemical reactions.
Separation of solid
–liquid mixture
• 1. Decanting: decanting separates an
insoluble solid from a liquid by pouring
off the liquid from the container
• Example: removal of big stones from a
container of water
• In cooking, we often pour off water
from the boiled vegetables by
decanting
Separation of solid - liquid mixture
• 2. Filtration: when we want to separate small solid particles such
as sand, from water, we use this method
• Filtration is used to separate an insoluble solid from a liquid
• The mixture is poured into a filter paper which is placed on a
funnel.
• The liquid passes through the small holes in the filter paper
• The insoluble solid particles cannot pass through and is trapped in
the filter paper
• Residue: solid collected on the filter paper
• Filtrate: the liquid passing through the filter paper
Filtration method
 Uses of filtration
• Water filtration: Much of Singapore’s drinking water comes from
rainwater collected in local reservoirs and from rivers in Johor,
Malaysia. At water purification plants, large filters are used to
remove sand and mud from water. The filters in these plants do
not use filter paper, but consists of layers of sand, gravel and
pebbles.
• Nose : the nose filters particles from the air to ensure that the air
we breathe is clean
• Kidneys: our kidneys use filtration to separate wastes (and extra
water) from our blood. The waste and water then passes out of the
body as urine.
Separation of solid – liquid mixture
• 3) Evaporation: is used to separate dissolved solids from a solution
• Ex: separation of common salt from a salt solution
• Common salt dissolves in water to form a salt solution
• We cannot use filtration to separate salt from its solution as the
dissolved salt passes through the filter paper
• We use evaporation, where the solution is heated, and water
changes into steam
• When all the water has evaporated, solid salt remains as a residue
• In some countries, salt is obtained by evaporating seawater in large
open areas called ‘salt pans’. Heat from the Sun slowly evaporates
the water in the pans, leaving behind solid salt
Separating solid – liquid mixture
• 4) Crystallisation: best method to obtain a pure solid from a solution
• Crystallisation separates a dissolved solid from a solution, forming
pure crystals of the substance
• The process involves heating a solution to evaporate off the solvent
until a saturated solution is obtained
• The hot saturated solution is allowed to cool
• As it cools, pure crystals of the dissolved solid (solute) form
• You can test if the solution is saturated by dipping a clean, dry, glass
rod into the solution
• If the solution is saturated, crystals will form on the glass rod, when it
is removed and allowed to cool
• Pure sugar is obtained in this method
Separation of solid – liquid mixture by
centrifugation
• 6) Centrifugation: Methods
for separating out particles
of different densities in a
substance – heavier
particles settle down and
lighter particles float above
• The separation of an
insoluble solid from a liquid
by rapid spinning in a
centrifuge
• During the rapid spinning,
the solid collects at the
bottom of the sample
• The liquid can be decanted
carefully
 Separating soluble solid from a liquid

• 7) Simple distillation: separates a pure liquid from a

75

solution
• Ex : water from a solution of saltwater
• The solution is heated, the liquid is changed into a vapour by
boiling
• The vapour rises the neck of the round-bottomed flask
• The vapour passes through the condenser ( this apparatus
removes heat from the system by continual pumping in
water. The hot vapours condense as they come in contact
with the cold glass of the condenser)
• Thus, pure water is collected in a beaker
• After all the water is evaporated, only the solid solute will
be left in the flask
Separation of two miscible liquids

• 8) Fractional distillation: separates a mixture of miscible liquids

with widely differing boiling points
• Miscible – if two liquids form a completely uniform mixture when
added together, they are said to be miscible
• Ex: alcohol and water
 Fractional distillation - method
•
Fractional
distillation
 Separating two solids in a mixture
• 9) Sublimation – separates a mixture of solids, one of which
sublimes
• Sublimation – substances change directly from a solid state to the
vapour state on heating without going through the liquid state
• Iodine is a solid that sublimes
• Mixture of sand and iodine – heated in a beaker, the iodine
sublimes into its vapour form
• The vapour changes into solid form when it settles directly on a cold
surface
• The sand is not affected by the heat and remains in the beaker
• As only few solids sublime, this method is limited
Separating two
immiscible liquids
• Two immiscible liquids are separated using a
10)

separating funnel
• Ex: separate oil and water
• The mixture is placed in a separating funnel and allowed
to stand
• The oil and water form two different layers – less dense
oil on top
• The stopper is removed, and the tap is opened
• The bottom layer of water is collected in a beaker
• Then the tap is opened again, and the layer of oil can be
collected in a separate beaker
Chromatography
• Chromatography is a method of separating and identifying
mixtures
• Paper chromatography is used to separate coloured substances in
a dye/ink
 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
Paper chromatography - process
Paper chromatography
• Interpret simple chromatograms:
• If two or more substances are the same, they will produce the same
chromatograms
• It is a common practice to include a known compound as a reference
spot – this can match up to an unknown spot or set of spots in order
to identify it
• 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 spot, a pure
substance will show up with one spot
Locating agents – paper chromatography
• 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
colourless substances such as amino acids or sugars
• 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
• Locating agents – a compound that reacts with invisible, colourless
spots separated by chromatography to produce a coloured product
which can be seen. Amino acids and other biological substances need
locating agents
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
• Retention factor = Distance travelled by substance/distance travelled
by solvent
• The retention factor is a ratio and has no units
Measuring Rf value
Summary
 Assessing Purity
•
Criteria for purity
•