Purity determination and compounds separation Flashcards
Solubility of acids
- Dissolved well in non polar organic solvents at low pH
- Soluable in polar solvents at a high pH
Solubility of bases
- Solubility in organic solvents when the pH is high
- Soluable in water when the pH is low
When is seperation required
- If comound isnt pure after partition purification is required
Purification
When the compound is pure after partition (solid and liquid)
Recrystalisation
- Solubility of solids increase with increased temperature
- Required desired product to no be soluable in room temperature but in a hot solvent
- Imurity must be soluable (or partially) at room temperature and when solvent is hot
- Add impure and desired to hot solvent allow to cool to room temp and desired will recrystalise
Distillation
- Liquid converted to vapours by heating then condensation of vapours via cooling
- Seperate non volatile liquid from volatile as they have diffrent boiling points
Chromatography
- Seperating mixture into components identify components and measure the concentration
- Distribute components between 2 phases
- Partition coefficient = solute phase 1/solute phase 2
- Higher partition coefficent means higher ratio of concentration
- Mobile phase gas or liquid stationary is solid or liquid
Process of chromatography
- Sample containing 3 components are placed on colum containing stationary phase
- Sample is carried along the column by the mobile phase the component spreds out
- End od column the components are seperated due to diffent speed and affinity to stationary phase
Thin layer chromatography
Qualitative
- Thin layer of absorbant coating (SiO2 and Al2O3)
- Small amount of sample solution spotted on the plate
- End of TLC immersed into pool of solvent
- Placed above solvent moves up stationary phase via capillary action
Retention factor
Distance travelled by solvent/Distance of solvent front
If compounds in chromatography are colourless?
- Add fluorescence to stationary phase which will glow when exposed to UV ligtht
- Areas containing solute will not glow and appear darker (mobile phase)
Stationary phase
- Silica gel (silica oxide)
- Very polar free OH group can form hydrogen bonds vander waals forces and dipole dipole interactions
Polar compound attraction to stationary phase
More polar compounds more formation of H bonds with silica gel more firmly so stronger absorbtion
Non-polar compound attraction to stationary phase
- Forms weak vander waals forces so less attraction so carried more by mobile phase
- Low polarity compound has higher rf value than high polarity
Mobile phase
- Ability to dissolve ‘like dissolves like’ how fast they move up the TLC
- Polar compounds run faster in polar solvent and non polar in non polar solvents
Mobile phase absorbtion to stationary phase
- Ability to be asorbed by silica can displace compond and push up the TLC plate (affinity to the stationary phase)
Solvent too strongly absorbed
- Fully displace all compounds they all move up the TLC plate and no seperation occours
Solvent too weakly absorbed
- Solvating power is too weak to move the compound up the TLC to show enough seperation
Eluting strength
mobile phase
How strong it is absorbed on the silica which increases with solvdent polarity