EXPERIMENT 1: DISTILLATION

Distillation
- Used to separate a mixture of liquids, the liquid can be heated to force components,
which have different boiling points, into the gas phase.
- Process of heating a liquid mixture to form a vapor and then cooling that vapor to get a
liquid.
- Main purpose: purify drinking water

Purified Water, USP is obtained by Distillation, Ion exchange treatment and Reverse osmosis.
(Get RID of WATER)

Apparatus used in Distillation setup:

 Distilling Flask - used to separate mixture of two liquids with different boiling points.
 Condenser - is used to cool hot gases into liquids.
 Vacuum Adapter – used to reduce the pressure of the entire system in the distillation
making it easily to vaporize the subs.
 Thermometer

40% Ethanol + Water = VODKA

Alcohol at low amount = CNS Stimulant
Alcohol at high amount = CNS Depressant

Sources
Wine “WiPes” Fermented grapes
Brandy “hBW” Distilled wine
Whiskey “WhiGra” Fermented grain

Types of Distillation:
1. Simple Distillation - is a procedure by which two liquids with different boiling points can
be separated.
Example: Ethanol and Water

2. Fractional Distillation - Technique used to separate miscible liquids that have boiling
point difference of less than 25ºC.

3. Vacuum Distillation - is a method of distillation performed under reduced pressure. It is

also used when the boiling point of the compound (or the solvent) is too high

4. Steam Distillation - is an alternative method of achieving distillation at temperatures

lower than the normal boiling point.

• Boiling Point - temperature at which liquid pressure is equal to atmospheric pressure.

“LP = AP”
 EXPERIMENT 2: EXTRACTION

Extraction
- Involves the separation of medicinally active portions of animal or plant tissues from the inactive
components through the use of selective solvents.
- Example: Tea

Apparatus used in Extraction:

 Separatory funnel – used to separate immiscible liquids.

Immiscible – incapable of being mixed together or blended together.

Two layers are formed because of DENSITY; higher density being on the bottom and lower density on
top.

Separatory Funnel

Organic Phase – contains uncharged species or neutral compounds

Aqueous Phase – contains water and other uncharged species.

Stopcock

ALKALOIDS
- Bitter, Nitrogen containing and usually ends in –ine.

 Caffeine
- 1,3,7 – Trimethylxanthine
- Stimulates the CNS, causing alertness.

 Theophylline
- 1,3 – dimethylxanthine
- Tea (Camellia sinensis)
- Used to treat asthma.

 Theobromine
- 3,7 – dimethylxanthine
- Theobroma cacao
 EXPERIMENT 3. SUBLIMATION AND MELTING POINT DETERMINATION

Sublimation
- chemical process used to separate nonvolatile impurities from volatile compounds.
- involves heating an organic compound so that it goes from a solid phase to a gaseous or vapor
state without going through the liquid phase.
- Example: Mothballs

Melting point
- temperature at which the substance changes from a solid to liquid state.
 EXPERIMENT 4. RECRYSTALLIZATION

Crystallization
- Process of formation of large crystals in pure state from their solution.
- Formation of a new, insoluble product by a chemical reaction.

Soluble versus Insoluble

Solubility – property of a solid, liquid or gaseous chemical substance called solute to dissolve in a solid,
liquid or gas solvent.
Insolubility – inability to dissolve in a solid, liquid or gaseous solvent.

Recrystallization
- Process of dissolving the solid to be crystallized in a hot solvent or solvent mixture and then
cooling the solution slowly.
- Technique used to purify solid compounds.

Best Recrystallizing Solvent:

Compound should be insoluble at room temperature, very soluble while heating and very insoluble
upon cooling.
 EXPERIMENT 5. COLUMN AND THIN LAYER CHROMATOGRAPHY

Chromatography
- Separation of a mixture into various fraction by distribution between two phases, one phase
being stationary and essentially two dimensional (a surface), and the remaining phase being
mobile.

Column Chromatography
- One of the most common types of chromatography. It uses a strip of paper as the stationary
phase.
- Capillary action is used to pull the solvents up through the paper and separate the solutes.

Principle of Separation:
 Higher the adsorption to the stationary phase, the slower the molecule will move through the
column.
 Higher the solubility in the mobile phase, the faster the molecule will move through the column.

Adsorption – property of how well a component of the mixture sticks to the stationary phase.
Solubility – property of how well a component of the mixture dissolves in the mobile phase.

Term Definition
Mobile Phase or Carrier Solvent moving through the column
Stationary Phase or Adsorbent Substance that stays fixed inside the column (Ex:
Silica Gel)
Eluent Fluid entering the column
Eluate Fluid exiting the column (that is collected in flasks)
Elution Process of washing out a compound through a
column using a suitable solvent
Analyte Mixture whose individual components have to be
separated and analyzed

Thin Layer Chromatography

- This is a simple and rapid method to check the purity of an organic compound. It is used to
detect pesticide or insecticide residues in food.
- Thin-layer chromatography is also used in forensics to analyze the dye composition of fibers.

Rule of thumb:
 The component that travels the least distance on the TLC plate is the most polar, since it binds
to the silica most tightly.
 The component that travels the maximum distance is the least polar; it binds to the silica least
tightly and is most soluble in the non-polar solvent.

𝐷𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑡𝑟𝑎𝑣𝑒𝑙𝑙𝑒𝑑 𝑏𝑦 𝑡ℎ𝑒 𝑐𝑜𝑚𝑝𝑜𝑢𝑛𝑑

𝑅𝑒𝑡𝑒𝑛𝑡𝑖𝑜𝑛 𝑓𝑎𝑐𝑡𝑜𝑟 (𝑅𝑓) =
𝐷𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑡𝑟𝑎𝑣𝑒𝑙𝑙𝑒𝑑 𝑏𝑦 𝑡ℎ𝑒 𝑠𝑜𝑙𝑣𝑒𝑛𝑡

Other Types of Chromatography:

 Liquid Chromatography
- Used to test water samples to look for pollution in lakes and rivers.
- It is used to analyze metal ions and organic compounds in solutions.
 Gas Chromatography
- Used in airports to detect bombs and is used is forensics in many different ways.
- It is used to analyze fibers on a person’s body and also analyze blood found at a crime scene.
- In gas chromatography helium is used to move a gaseous mixture through a column of absorbent
material.
NOTES:
 Dichloromethane is a suspected carcinogen.
 Methanol can cause blindness.
 Methanol and hexane are flammable and volatile.
 IUPAC – International Union of Pure and Applied Chemistry

DISTILLATION SETUP