Simple Separation Methods

Crystallization

Used to

obtain pure material in the crystalline state.

oncentrating a solution containing the component of interest by

heating it

allowing it to stand

Optimal solvent composition

s designed to minimize contamination of the crystals with other materials.

Membrane Separation

Definition

It a separation process that utilize semipermeable membranes to allow passage of certain chemical species completely, while stopping or strongly restrict the permeation of others.

Some Applications

Convert salt water to drinkable water

Removal of urea from blood

Separate azeotropic mixtures

Examples

Ultrafiltration

Dialysis

Reverse Osmosis

Methods

Structure and properties

General important properties of membranes

Good mechanical stability

Good chemical stability.

Various semipermeable membranes

Microporous Membranes

Used to

Separate particles that differ significantly in size.

The principle

If the size of particles (or molecules):
>>pores sizes -> rejected to pass

<< pore size -> allowed to pass

intermediate pore size -> partially rejected

Homogeneous Membranes

Composition

a homogeneous film or interphase through which a mixture of chemical species can be carried by molecular diffusion

The principle

Particles of exactly the same size can be separated with homogeneous diffusive-type membranes when their solubilities in the film or their concentrations differ significantly

Thin Membranes

The thinner the membrane; the faster the transport rates through membranes.

Charged Membranes

The principle

The separation is accomplished by:

pore size as well as

exclusion of coions (ions of the same charge as
The fixed ions) from the membrane

Membrane-Based Separation Methods

Ultra filtration

The process

Application of hydrostatic pressure between 1 & 10 atm to separate solutes with diameters > 20 Aْ

Reverse Osmosis

Dialysis

Electrodialysis

Evaporation

Usage

As a first preparation step for further separation.

As final step for obtaining an isolated material as a residue

Methods

Using an open container for a period of time

Application of heat

example

evaporation of seawater to get sea salt salt (NaCl)

Definition

t is the process of removing the solvent from a sample by heating or by utilizing air currents which lead to concentrate the sample or transfer it into a solid state.

Precipitation

formation of precipitate (PPT)

By Increase the concentration of a solute in a solution to a higher level than its solubility

formation of pure crystals

By carried out in (a proper solvent & a controlled manner)

Methods

Solvent Precipitation

Addition of another miscible solvent to the solution which lower the solubility of the component of interest

Precipitation via Chemical Reaction

Addition of a species that form a lower solubility salt with the target species.

Common ion effect

Precipitation by Adjustment of pH

Mainly organic & inorganic weak acids & bases

Filtration

The principle

Porous material with a certain particle sizes (such as filter paper or membranes) allow the solvent to pass through while retaining the solids with particle sizes higher than the pore sizes.

used to

separate solids from liquids.

Types of filtration

Filtration under vacuum

Using Buchner funnel

Using Membrane Filters

Simple filtration

Using simple filter papers (made from cellulose) and exhibit particle retention levels down to 2.5 μm.

Using gravitational force to separate solids from the liquid.

Extraxtion

Definition

Distribution of solute between two immiscible solvents

Distribution Coefficient Kc

Distribution of a solute concentration (C) between two solvents ( 1 and 2) during extraction can be represented by the following equation: Kc = C1/C2

Distribution Coefficient of a Species

Distribution Coefficient is used for one species.

Distribution ratio D

Excluding all complications according the interactions between the extracted species and the used solvents; these interactions should be ignored to simplify the calculations. D = total concentration of solvent in organic phase/total concentration of solvent in aqueous phase

Successive Extractions

If Kc >1000 -> 1 signal extraction stage is enough to extract all of the target species.

If Kc < 1000 -> divide some of the extraction solvent into smaller portions and for each portion use successive extractions.

Extraction of Mixtures

Multiple Extractions

Craig Apparatus

method of multiple liquid-liquid extractions is countercurrent extraction, which permits the separation of substances with different distribution coefficients (ratios)

Countercurrent Extraction Versus Differential Column System

Distillation

related to

evaporation but all the components of interest are volatile. while volatile components are separated from non-volatile ones in evaporation.

solids

sublimation (highly specialized distillation method), is used to volatilize their component if possible .

Phases in Distillation

used

for separation of the components of liquid mixtures.

The principle

It depends on the distribution of constituents between
the liquid mixture and vapor in equilibrium with the mixture.

more volatile components concentrated in the vapor

less volatile ones are in greater concentration in the liquid.

Forms and Modes of distillation

Fractional distillation

It is based on the condensation of the hot vapor at verious levels in the column and the resulting liquid refluxes to a lower level where it is vaporized, which corresponds roughly to a re- distillation.

Flash distillation

It is instantaneous and continuous vaporization of a definite fraction of the liquid mixture in such a way that the total vapor produced is in equilibrium with the residual liquid.

vacuum distillation

It is distillation under decreased pressure to reduces the boiling temperatures.

Applications

To separate

high-boiling mixtures.

materials that decompose below their normal boiling points.

steam distillation

The mixture boiling point tempreture is reduced by vaporixing it into a stream of carrier vapor

Azeotropic/Extractive distillation

Any technique used to break an azeotrope (mixtures that are difficult to separate) in distillation.

The process

Adding another component to alter the relative volatility of the mixture substances and form lower-boiling azeotrope that is heterogeneous.

Applications

To separate mixtures whose components boil too close together for economic fractional distillation.

Example

Formation of two immiscible liquid phases by addition of benzene to water and ethanol.

Distillation as the Precursor to Gas Chromatographic Methods

volatile components

separated on a packed or capillary column

non- volatile components

HPLC