unit 3: organic practical techniques Flashcards
synthesis of compound techniques
heating under reflux, vacuum filtration
purification of compound techniques
distillation, solvent extraction, recrystallisation
determination of purity techniques
melting point analysis, mixed melting point analysis, thin layer chromatography (TLC)
heating under reflux
heats a reaction over an extended period of time without any vapours escaping
heating under reflux equipment
condenser, round bottom flask, heating mantle
anti bumping granules
used to ensure smooth boiling
vacuum filtration
separates solids and liquids and is much faster than gravity filtration
vacuum filtration equipment
buchner funnel connected to a vacuum flask with an arm at the side connected to a water pump
purifying
removes any impurities and side products formed during the synthesis
recrystallisation
involves adding product to hot solvent to dissolve it and letting the product recrystallise as it cools down, any soluble impurities will stay dissolved in the solvent
things to consider when choosing a solvent
product must be soluble in solvent at high temperature and minimally soluble at room temperature, it must not react with the products, the solubility of the impurities
recrystallisation technique
add minimal volume of hot solvent to your synthesised product, filter the hot mixture to get rid of any insoluble impurities, let the solvent slowly cool down which will crystallise the desired product, filter off the product which will remove any soluble impurities left in the solvent
melting point analysis
works out the purity of the sample by finding it’s melting point and comparing it to a known melting point value, impurities in the sample lower and broaden the melting point since they disrupt the intermolecular bonding in the crystal lattice
melting point range
the temperature range over which it starts to melt to when it finishes melting
mixed melting point analysis
mix the sample with a pure sample of what we meant to synthesis, if the melting point is at the correct value and the range is narrow, it is pure. if a different product was made the pure sample will act as an impurity and lower the melting point
thin layer chromatography
separates compounds by their polarity using a film of silica or aluminium oxide as the stationary phase, sample is spotted on the base line and a solvent carries the compound up, a developing agent of UV light visualises the spots and the Rf value is calculated
Rf
distance travelled by the sample / distance travelled by the solvent
if there is only 1 spot in TLC
there are no impurities
distillation
separates compounds by boiling point, more volatile substances with lower boiling points will pass through first. can identify compounds by comparing boiling points or purify substances by only collecting within the target boiling point, any collected outside will be impurities
distillation equipment
burner, distilling flask, thermometer, condenser, receiving flask