Calculations And Procedure Flashcards
Gravimetric analysis
The mass of an element or compound present in a substance is determined by changing that substance into another of known chemical composition that can be readily isolated , purified and weighed
To use gravimetric analysis we need:
The equation
The reaction to proceed to completion
The accuracy of gravimetric analysis depends on…
The dexterity of the person carrying out the procedure
The two types of gravimetric analysis
Precipitation/ filtration
Heating (volatilisation)
Precipitation/ filtration
The substance undergoes a precipitation reaction which is then separated, washed and dried to constant mass. The filtrate is tested to ensure the reaction has gone to completion
Must be carried out carefully to ensure all material is transferred and all apparatus dried and weighed with extreme care
For precipitation/ filtration the product must have
Low solubility so that all the product is precipitated
Particle size large enough for filtration
Be stable at temperatures of 100-105°C so that it can be dried in an oven
Heating (volatilisation)
Involves heating to change one substance into another
E.g dehydration of a hydrated salt to calculate the number of miles of water of crystallisation
Phase equilibriums
A solute is added to two immiscible liquids and the solute is soluble in both, then some of the solute will dissolve in both liquids. It will distribute itself in a definite ratio which we call the partition co-efficient
Partition co-efficient
A measure of the distribution of a solute between two immiscible solvents and is simply a specific case of equilibrium
The size of a partition co-efficient will vary as it depends upon
The solute
The nature of the two immiscible liquids
The temperature
The partition co-efficient is independent of…
The amount of solute
The volume of solvent
Partition co-efficient can be calculated with
[solutex]solvent B(top layer)
K= —————————————
[solutex]solvent A(bottom layer)
What are the solvent requirements for phase equilibria
The solvent used must be immiscible with the liquid mixture or soloution
The solute must be more soluble in one of the layers
The solvent must be volatile which allows the solute to be obtained by evaporation of the solvent
The solvent must be interactive with the solute
Most organic solvents are less dense in water so…
Will be on the top layer (except chloroform/ dichloromethane)
Vacuum filtration
Using a Buchner, hirsch or sintered glass funnel. These methods are carried out under reduced pressure and provide a faster means of separating the precipitate from the filtrate. The choice of filtering medium depends on the quantity and nature of the precipitate
Recrystallisation
A laboratory technique to purify solids based upon solubility.
The impure compound is dissolved gently in the minimum volume of hot solvent then filtered to remove the insoluble impurities. The filtrate is allowed to cool slowly to force crystallisation. The more soluble impurities are left behind in the solvent
For recrystallisation must be carefully selected so…
The impure compound is insoluble at lower temperatures
Refluxing
Heat energy is applied to a chemical reaction mixture over a period of time. The liquid is placed in a round bottomed flask along with anti-bumping granules with a condenser at the top. The flask is heated vigorously over the course of the chemical reaction; any vapours given off are immediately returned to the reaction vessel as liquids when they reach the condenser