Measurement and Experimental Techniques

1. Measurement
Physical
S.I. Unit Other Common Units Apparatus and Accuracy
Quantity

Gram(g), Tonne(t).
1
Mass Kilogram(kg) Electronic Balance(+- 0.01g)
tonne=1,000kg=1,000,000
g

Time Second(s) Minute(min), Hour(h) Stopwatch(+- 0.01s)

Thermometer(+-0.5℃)
Temperature Kelvin(k) Degree Celsius(℃)
Datalogger with temperature sensor

Measuring Cylinder(nearest 0.5cm³)

Cubic Centimetre(cm³),
Volume of Cubic Pipette (fixed volume of 20.0cm³ or
Cubic Decimetre(dm³)
Liquid Metre(m³) 25.0 cm³)
1 dm³=1000cm³
Burette(nearest 0.05cm³)

Cubic Centimetre(cm³),
Volume of Cubic Graduated Gas Syringe (Maximum
Cubic Decimetre(dm³)
Gasses Metre(m³) 100cm³)
1 dm³=1000cm³
2. Collection of Gases
 Measurement and Experimental Techniques
1. Separating Solids
● Using a Magnet
○ To separate a solid that is magnetic from those that are not
○ Magnetic Material
■ Iron, Steel, Cobalt, Nickel

● Sublimation
○ Definition
■ Change in Physical State from solid to gas without passing
through the liquid phase
○ Solids that can sublime
■ Iodine crystals, dry ice, ammonium chloride
○ Example: Obtain Iodine from a mixture of sand and iodine
○ Steps:
■ Heat the Mixture, Black solid iodine turns into purple vapour
directly
■ The vapour changes back to solid directly on a cold surface
 ■ Sand which does not sublime remains in the evaporating
dish

● When one solid is soluble in a particular solvent, such as water

● Evaporation to Dryness
○ The mixture containing the 2 substances that would be separated
must be thermally stable and not decompose upon heating
■ Potassium Chloride and Sodium Chloride
○ Example: Obtain Sodium Chloride from a mixture of sand and
sodium chloride
○ Steps
■ Add Excess distilled water to the mixture to dissolve sodium
chloride
■ Filter the mixture to remove sand as a residue
■ Evaporate salt solution (filtrate) to dryness to obtain sodium
chloride
● Crystallisation
○ The mixture containing the 2 substances that would be separated
are generally thermally unstable and will decompose readily upon
heating
○ Example: Obtain Copper (II) Sulfate from a mixture of sand and
Copper (II) Sulfate

○ Steps:
■ Add Excess distilled water to the mixture to dissolve sodium
chloride
■ Filter the mixture to remove sand as a residue
■ Heat the filtrate to obtain a saturated solution of copper(II)
sulfate
■ Cool the saturated solution for crystals to form
■ Filter the Mixture to obtain crystals and dry it between sheets
of filter paper
2. Separating a Solid from a Liquid
● Filtration

3. Separating a Liquid from a Solution

● Simple Distillation
○ Example: Obtaining pure water from salt solution
○ Steps:
■ Heat the mixture in the distilling flask. A few pieces of boiling
chips are added to ensure smooth boiling
■ Ensure that the thermometer is placed at the opening of the
sidearm of the distillation flask
 ■ The vapour will condense to a pure liquid called the distillate
in the cold condenser and is collected in the receiver
○ Precautions for Distillation
■ The bulb of the thermometer is to be positioned at the
opening of the sidearm of the distillation flask. Why?
● This is to ensure accurate measurement of the
temperature of the vapour passing into the condenser
■ The cooling water should enter the condenser jacket through
the lower tube and leave by the upper tube. Why?
● Water enters at the lower end of the condenser to
ensure that the water is at a lower temperature than
the vapours. This is to ensure complete condensation
of the vapours to take place more efficiently

4. Separating Liquids
● Fractional Distillation
○ Miscible Liquids are separated by fractional distillation
■ Miscible liquids are liquids that can dissolve in each other to
form a solution. These liquids have different boiling points
○ Example: Separating Ethanol (Boiling Point:78℃) and water
(Boiling Point:100℃)
○ Steps:
■ Heat the mixture of ethanol and water in the round bottom
flask
■ Ethanol vapour and water vapour rise up the column as the
solution is heated
■ The water vapour condenses in the fractionating column and
falls back into the flask
■ Ethanol, which has a lower boiling point than water, reaches
the upper part of the column and is distilled over
■ At this stage, the thermometer shows a constant
temperature of 78℃, which is the boiling point of ethanol
■ In this condenser, hot ethanol vapour condenses as running
water cools it; liquid ethanol flows down the inner tube of the
condenser and into the receiver
■ Ethanol is collected as the distillate in the receiver
■ When all the ethanol has distilled over, the temperature
rapidly rises to 100℃, which is the boiling point of water.
Replace the distillation flask such that the distilled water can
be collected

○ How does a fractionating column work?

■ Packed with glass beads which greatly increases the surface
area to volume ratio for evaporation and condensation
 ■ When heated, a mixture of vapour passes up the column. As
the temperature in the column is lower, the vapour starts to
condense
■ Vapour of the higher boiling point condenses more readily
than that of the lower boiling point
■ Liquid that has condensed on the column is warmed by the
rising hot vapours and the more volatile liquid (lower boiling
point) evaporated more readily
■ As a result of many repeated evaporations and
condensations, the vapours moving up the column become
richer in the more volatile liquid
■ Hence the vapour with the lower boiling point will be able to
reach the top first and be distilled over into the receiver
■ In short, a fractionating column provides a surface for
continuous condensation and evaporation of the vapours

Precaution Purpose

1. Addition of boiling To ensure smooth boiling by reducing bumping of

chips to the liquid
mixture

2. It is placed near the opening of the condenser to

Position of the measure the temperature of the vapour accurately.
thermometer bulb This also helps to determine the identity and purity of
the distillate

3. ● Cooling water should enter the condenser

jacket through the lower tube and leave by the
The direction of upper tube
water flow in the ● The direction of water flow is opposite to the
condenser direction that vapour moves in the condenser
to ensure efficient cooling and complete
condensation of vapour

4. Receiving Flask A Conical Flask is used because the narrow neck

can reduce loss of distillate through splashing

● Separating Funnel
○ Immiscible Liquids are separated by using a Separating Funnel
 ■ Immiscible liquids are liquids that do not dissolve in each
other
○ Example: Separating oil from water
○ Steps:
■ Pour the mixture into the separating funnel
■ Support the separating funnel using a retort stand. Then
place a clean beaker below the separating funnel
■ Open the tap of the funnel to allow the bottom layer to drain
into the beaker. Close the tap before the top layer of liquid
run out
■ Place another beaker below the funnel. Open the tap to
allow a little of the top layer of liquid into the beaker.

5. Chromatography
● A technique used for separating and identifying small amounts of solutes
by dissolving them in a solvent and allowing them to move along a filter
paper at different speeds
○ Solutes to be separated must be soluble in the solvent
○ Solutes which are more soluble travel further while less soluble
solutes appear nearer to the base of the paper
○ Identical solutes travel the same distance on the filter paper
● Steps:
 ○ Draw a straight pencil line along one end of the chromatography
paper (about 2 cm away from the edge)
○ Label a cross in the middle of the pencil line and place a small spot
of the sample onto the cross
○ Secure the chromatography paper using a glass rod and place the
paper into a beaker containing a solvent. The solvent has to be
below the pencil line
○ Allow the solvent to move up the paper to separate the sample into
its corresponding components
○ When the solvent reaches close to the other end of the paper,
remove the paper from the beaker
○ Leave the chromatography paper to dry for a few minutes. The
result is known as the chromatogram
● Precautions:
Precautions Explanation

The starting line has to be drawn in pencil, not The ink consists of a mixture of colors which might
in ink dissolve in the solvent and interfere with the results

The start line must be above the solvent level

To prevent the spots from dissolving in the solvent
at the start of the experiment

Only a small spot of the sample must be To prevent overlapping and smudging of
placed at the start line components

The solvent front must be allowed to reach

To ensure complete separation of the mixture
near the top of the chromatography paper
● Identification of substances by paper chromatography is carried out in 2
ways:
○ Comparing with ‘Known’ standards
○ Rf value is a constant for a particular solute in a given solvent. It
acts as a fingerprint and can be used to identify the substance
○ Rf value
■ Is a ratio that is expressed in the form of decimals
■ Has no units
■ always smaller than 1
■ Working should always be shown clearly

𝐷𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑓𝑟𝑜𝑚 𝑠𝑡𝑎𝑟𝑡 𝑙𝑖𝑛𝑒 𝑡𝑜 𝑠𝑝𝑜𝑡

Rf = 𝐷𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑓𝑟𝑜𝑚 𝑠𝑡𝑎𝑟𝑡 𝑙𝑖𝑛𝑒 𝑡𝑜 𝑠𝑜𝑙𝑣𝑒𝑛𝑡 𝑓𝑟𝑜𝑛𝑡
To locate and identify colourless spots of the sample, the chromatogram is sprayed with
a locating agent that can react with the substances on the chromatogram to produce a
coloured product. This coloured product can then be easily observed

6. Purity
Pure Impure

Only one type of substance Two or more substances

Fixed Proportion Any Ratio

Fixed M.P and B.P. Range of M.P. (decreased) and B.P. (increased)

Single spot on Chromatogram Multiple spots on Chromatogram

● Method 1: Paper Chromatography
○ Chromatography is carried out if
■ The substance cannot be melted or boiled very easily
■ The amount of substance is very small
● Method 2: Measure Melting / Boiling Point