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Separating Techniques

Separating Mixtures of Solid/Liquid


There are three methods for separating mixtures of solid/liquid: Filtration, Evaporation to
Dryness and Crystallisation.

Filtration

- Method used for separating a mixture of insoluble solid and liquid (e.g. sand and water)
- Mixture is poured through filter paper
o Filter paper contains many tiny holes
o Water/liquid is able to pass through, big particles are trapped
- Solid trapped in filter paper = Residue
- Liquid passed through filter paper = Filtrate (usually a solution)

Evaporation to Dryness

- Method used for separating a solution (with substances dissolved in it)


- Used to recover the solute from a solution
- Water is evaporated off completely
- Criteria for using evaporation to dryness method:
o solute must be stable at high temperature
o it must not contain water of crystallisation

Crystallisation

- Recovery of a crystalline solid from its saturation solution by allowing the hot solution to
cool to its saturation point
o Example: When a solid, e.g. Copper (II) sulphate dissolves in a liquid, a solution is
formed. When the solution is heated, most of the liquid is evaporated off until a
saturated solution is cooled; the dissolved solute will reappear and can be
obtained easily by filtration.
- Main steps in crystallisation:
o Impure solid is dissolved in a solvent
o Solution is heated to saturation
o Solution is cooled, pure crystals appeared
o Filter out the crystals
o Dry the crystals between two sheets of paper
- If impurities are present,
o if the impurities are insoluble in the solvent, remove them by filtration first before
crystallisation
o if the impurities are soluble in the solvent, it will remain dissolved in the solution
after crystallisation
- Criteria for using crystallisation method:
o Solubility of the solute must vary a lot with temperature e.g. for potassium nitrate,
solubility at 20˚C is 15g/100g of water but solubility at 100˚C is 250g/100g of
water
o If the solubility does not vary appreciably with temperature, the crystallisation
method is not suitable e.g. for sodium chloride, the solubility at 20˚C is 36g/100g
of water and the solubility at 100˚C is only 39g/100g of water

Separating Mixtures of Solids


There is only one method for separating mixtures of solids: Sublimation.

Sublimation

- Definition : Sublimation refers to change of state of a substance from solid to gaseous


state without going through the liquid state on heating
- Examples of substances which can sublime include naphthalene, dry ice, iodine, ammonium
salts
- To separate a mixture of ammonium chloride, NH4Cl and sodium chloride, NaCl
o the mixture is first gently heated.

o ammonium chloride will condense on the cooler side of the furnace


Separating Mixtures of Liquids/Solution
There are two methods for separating mixtures of liquids/solution: Distillation and Fractional
Distillation.

- Definition: a process used to recover a solvent from a solution where the solution is boiled
and the vapour of the solvent condenses by cooling
- Used to purify liquids by converting the liquid into a gas then condensing it into its pure
form.
o The liquid collected is called the distillate

Simple Distillation

- Used to obtain a pure solvent from a solution of a solute (e.g. pure water from sea water)
- To achieve even boiling and preventing too much bumping (frothing and bubbling) in the
flask, anti-bumping granules or boiling chips is added.
- The set-up is as shown in the diagram below:
Fractional Distillation

- Definition: A process used to separate a mixture of miscible liquids using a fractionating


column.
- This method separates liquids in order of boiling points i.e. liquid with lowest boiling point
distilled first, while liquid with highest boiling point distilled last.
- When the flask is heated, the vapour will contain a higher proportion of lower boiling point
ethanol. The upper part of the column is cooler than the lower part. As the vapour moves up, it
repeatedly condenses and boils. Each time it boils, a higher percentage of ethanol is in the vapour.
(The large surface area [of the glass beads present in the fractional distillation column] causes
vaporisation followed by condensation of vapour to occur many times resulting in effective
separation of the vapours).

- By the time it reaches the top, almost pure ethanol is obtained. Ethanol vapour will be
condensed by the cool water as it enter the condensor. The thermometer also registers a
constant temperature of 78oC (bpt of ethanol) when the ethanol is being distilled.
- Water remains in the flask until almost all the ethanol has distilled. The temperature then
rises from 78oC to 100oC. The water starts to boil and passes into the condenser and is
collected as the second distillate.
Separating Immiscible Liquids
There is only one method to separate immiscible liquids: Separating Funnel.

Separating Funnel

- Two or more immiscible liquids with different densities can be separated using separating funnel.
- A typical set-up of the technique is shown below:

- Procedures:
o The mixture of immiscible liquids is poured in
o It settles into two layers as the liquids do not mix
o The tap is opened to let the denser, bottom layer run into a receiver
o The tap is closed and the receiver is changed.
o The tap is opened to let out the top, less dense layer run out.
Chromatography
There is only one method to separate immiscible liquids: Chromatography

Chromatography

- Method of separating and identifying both coloured and colourless mixtures.


- Mixtures can be solids, liquids or gases but their components must be able to dissolve in
the same solvent to different extents.
- Generally involves 2 phases : stationary phase (solid support e.g. paper) and mobile
phase (solvent or a gas).
- For example, to separate dyes in ink:
o Test mixture is applied onto the chromatography paper and a solvent is then
allowed to pass over the paper.
o As the solvent does so, the components of the mixture travel along with it.
o The solvent used depends on the substances to be separated.
o The component will travel at different rates over paper depending on: their
solubility in the solvent and their affinity for the water on the chromatography
paper.
o Generally, the more soluble the component is in the solvent, the faster it would
move with the solvent on the paper and hence the spot appears further up the
paper
o Result of chromatography is known as the chromatogram
- Two methods of developing the chromatogram:
- Ascending method: solvent running up the paper by capillary action
- Descending method: solvent running down the paper by both capillary action and gravity
- Advantage of the descending method over the ascending method:
o good for long pieces of paper thus better separation
o aided by gravity thus faster
- Precautions:
o paper must not touch the sides of container
o spot (of mixture) must be small and applied above level of solvent
o starting line must be drawn in pencil
- Unknown substances could be identified by the Rf values:

Question: If an ink is supposed to have 2 dyes but only one dye is present after a
chromatography test, what can be done to reveal the other dye?

- Make sure that both inks are soluble in the same solvent
- Spray locating agents to show the position of the spots on the paper

Created by: Ang Wee Shuen (01) 3P1

Taken from: http://vle.hci.edu.sg/chemistry/beijing/expt%20techniques/lesson1.html