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rp10c - melting point
solid organic compound in capillary tube, slowly heat with solvent surrounding tube (solvent higher b.p. than compound)
note temperature melting begins and ends - repeat calc. mean
capillary tubes thin glass - fairly confident temp. inside tube matches temp. on thermometer
pure - sharp melting point
impure - lower mp, over range of temps. if an organic liquid - higher bp over a range
impurities - solvent used (press between filter paper to remove)
pure crystals are larger and white
rp 10d - organic liquid
layers form because organic liquid is immiscible (doesn’t mix with water, hydrophobic/insoluble - no H bonds, long carbon chain)
layer at top lower density (organic), layer at high density (aqueous)
run off aqueous layer into conical flask, collect organic in a diff. conical flask
wash organic layer with Na2CO3 to neutralise acid catalyst - produces CO2
invert funnel and open tap, repeat - CO2 rises and leaves, prevents buildup of pressure
if organic layer still contains water - drying agent, anhydrous CaCl2/MgSO4
if water present CaCl2 clumps together and sinks. dry - floats gently, slowly to bottom
both MgSO4 and CaCl2 are suitable because they absorb water well and are insoluble and inert in organic liquids
remove drying agent with vacuum filtration - organic liquid at bottom
rp 10a: preparation of an organic solid
weigh by difference method
ethanoic anhydride reaction less vigorous
acid catalyst (making an ester) phosphoric acid corrosive
heat on hot plate for 20 mins
add to ice bath to encourage crystallisation, higher yield + faster
filter under reduced pressure to remove aspirin solid
leave crystals warm to dry
weight and calculate yield - further purification
rp10 b: recrystallisation
dissolve crude product in minimum vol of hot solvent - saturated solution, ensures high yield - crystals will form on cooling
suitable solvent - highly soluble at high temp. low soluble at low temp. - impurities still soluble at low temp.
filter whilst hot to remove insoluble impurities before crystals form (gravity filter)
leave to cool - increases yield - soluble impurities stay dissolved
filter under reduced pressure - wash with cold solvent to remove soluble impurities stuck to crystals
test purity with mp and calculate yield
yield not 100% - product left in glassware <100%, sample wet when weighing >100%
vacuum filtration
faster than gravity filtration, improved separation of fine particles
more efficient, continuous filtration
air drawn through filter funnel and pulls liquid down
wash solid with cold solvent
compress crystals - ensures air passes through crystals rather than around - better drying
rp7: initial monitoring
assume conc. of iodine is proportional to iodine
add H2O2 to iodide ions in acidic conditions with starch and limited thiosulfate ions
H2O2 produces iodine, which reacts with thiosulfate to reform iodide until thiosulfate is used up - when it is blue black colour forms
time taken for mixture to turn blue is recorded
repeat with diff concentrations of iodide
plot graph 1/t against conc. - shape of curve
rp7: continuous monitoring
Measure 50 cm3 of the 1.0 mol dm–3hydrochloric acid and add to conical flask.
Set up the gas syringe in the stand
Weigh 0.20 g of magnesium
Add the magnesium ribbon to the conical flask, place the bung firmly into the top of the flask and start the timer
Record the volume of hydrogen gas collected every 15 seconds for 3 minutes
gas syringes usually only measure up to 100cm3
measuring initial rate is preferrable because we know conc. at start
other ways to monitor reaction:
electrical conductivity (if there is a change in ions)
optical activity (followed with a polarimeter)
measure change in mass
take samples and titrate
propanone + iodine - take at 5 min
quench with sodium hydrogencarbonate - titrate against thiosulfate
iodine colour fades to straw yellow - add starch, goes blue black
add more thiosulfate until colourless
repeat every 5 mins for 30 mins