Required Practical 10

• what is reflux and why is it used?

  continuous boiling and condensing of a reaction mixture. Used because: this allows an organic reaction mixture to be heated without losing any reactants or products.
• why use anti-bumping granules?

  to prevent vigorous or uneven boiling, by making small bubbles form instead of large bubbles.
• what is the purpose of a separating funnel?

  to separate into two layers: higher density liquid (typically aqueous) is the bottom layer, and organic product layer above.
• how do you purifying an organic liquid?

  ● Put the distillate of impure product into a separating funnel ● Wash product by either:

  o Sodium hydrogencarbonate solution, shaking and releasing pressure from CO2 produced - Sodium hydrogen carbonate removes acidic impurities by neutralisation (converts to H2 O, CO2 and Na2 SO4 )

  o Saturated sodium chloride solution - helps separate the organic layer from the aqueous layer

  ● Allow layers to separate in funnel, and then run and discard the aqueous layer ● Run the organic liquid into a clean, dry conical flask and add 3 spatula loads of drying agent (anhydrous sodium sulphate - drying agent should be insoluble in the organic liquid and not react with the organic liquid) to dry the organic liquid

  ● Carefully decant the liquid into the distillation flask

  ● Distil to collect pure product
• how do you use the melting point to determine purity?

  ● If the sample is very pure then the melting point will be sharp (same value as quoted in data books).

  ● If impurities are present (and this can include solvent from the recrystallisation process) the melting point will be lowered and the sample will melt over a range of several degrees.

  ● Can be measured in an electronic melting point machine or by using a practical set up where the capillary tube is strapped to a thermometer immersed in some heating oil. ● In both cases a small amount of the salt is put into a capillary tube.

  ● The tube is heated up and is heated slowly when near the melting point.

  ● Compare experimentally determined melting point value with one quoted in a data source to determine purity. ● Error may occur if the temperature on the thermometer is not the same as the temperature in the actual sample tube.
• how do you measure the boiling point?

  ● This can be done in a distillation set up or by simply boiling a tube of the sample in an heating oil bath.

  ● Pressure should be noted- changing pressure can change the boiling point of a liquid.

  ● Not the most accurate method of identifying a substance as several substances may have the same boiling point.

  ● To get a correct measure of boiling point the thermometer should be above the level of the surface of the boiling liquid and be measuring the temperature of the saturated vapour.
• Describe recrystallisation

  1. Dissolve the impure compound in a minimum volume of hot (near boiling) solvent. 2. Hot filter solution through (fluted) filter paper quickly. So the desired compound is pure in crystals formed.

  3. Cool the filtered solution by inserting beaker in ice.

  4. Suction filtrate with a Buchner flask to separate out crystals.

  5. Wash the crystals with distilled water.

  6. Dry the crystals between absorbent paper.
• why dissolve the impure compound in a minimum volume of hot solvent?

  So the compound is pure in crystals formed.
• why use a hot filter solution?

  removes any insoluble impurities and heat will prevent crystals reforming during filtration
• Why cool the filtered solution in ice?

  Crystals will reform but soluble impurities will remain in solution form because they are present in small quantities so solution is not saturated. Cooling/Ice will increase the yield of crystals.
• why use a Buchner funnel?

  water pump connected to the Buchner flask reduces the pressure and speeds up the filtration.
• why wash the crystals with distilled water?

  remove any soluble impurities
• why dry the crystals?

  water would affect % yield
• what could be a possible reason for loss of yield?

  ● Crystals lost when filtering or washing

  ● Some product stays in solution after recrystallization

  ● Other side reactions occurring