purification Flashcards

1
Q

3 steps to purify organic liquid

A

separate organic + aqueous layer using a separating funnel

add a drying agent

redistill at narrower temp range

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
2
Q

what does each step in purifying liquid do

A

separating funnel - separates organic + aq layer

drying agents - removes excess water

redistill - removes organic impurities

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
3
Q

what to do if theres acid impurities in liquid

A

add aq sodium carbonate

releases carbon dioxide

slowly open tap to release gas

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
4
Q

how can you tell which is the organic layer + which is the aqueous layer in separating funnel

A

add distilled water and see which layer gets bigger

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
5
Q

separating funnel method

A

ensure tap of funnel is closed

pour mixture into the funnel

place a stopper + invert

allow layers to separate

add distilled water to see which layers increase in volume - aq layer

empty into a conical flask

open tap regularly - release build up of pressure

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
6
Q

examples of drying agents

A
How well did you know this?
1
Not at all
2
3
4
5
Perfectly
7
Q

drying agents method

A

add the organic liquid into a conical flask

add 1 spatula of drying agents + swirl

place a stopper to prevent product evaporating

decant the liquid from the solid

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
8
Q

how can you tell if there is still excess water

A

if the solid has stuck together in a lump - there is still water

if the solid is dispersed as a fine powder // clear liquid - no more water

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
9
Q

why may these liquids have organic impurities

A

boiling points relatively close together

the narrower the temp range - the purer the product

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
10
Q

3 steps to purify an organic solid

A

filter under reduced pressure

recrystallisation

check purity

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
11
Q

filter under reduced pressure method

A

connect one end of the pressure tubing to the vaccum / the filter pump / tap while attaching the other end to a Buchner flask

fit the Buchner funnel to the Buchner flask

switch on vaccum / tap

check for good suction

place a peice of filter paper inside buchner funnel

wet with the same solvent used in preparing the solid

pour the mixture into the funnel + rinse beaker to get all the solid

rinse the crystals in the funnel with more solvent + leave them to dry under suction for a few minutes so that the crystals start to dry

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
12
Q

how do you check for suction in buchner funnel

A

place hand across the top of the funnel

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
13
Q

recrystallisation method

A

Dissolve impure solid in minimum volume of hot
solvent

Cool solution first to room temperature and then to an ice bath

crystals form

collect crystals via filtration under reduced pressure

Scratch with glass rod

Wash with cold solvent/solvent and dry

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
14
Q

how to choose the solvent for recrystallisation

A

depends on desired product and it’s solubility

you want the impurity to fully dissolve in cold solvent

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
15
Q

how to check purity

A

determine the melting point + compare to a data base

How well did you know this?
1
Not at all
2
3
4
5
Perfectly
16
Q

how do impurities effect melting points + boiling points

A

Impurities lower the melting point (over a range) and increase the boiling point

17
Q

how to determine melting point

A

need to ensure sample is dry + free flowing

take a glass capillary tube

hold one end into a bunsen burner

rotate until end is sealed

allow to cool

fill with crystals to about a 3mm depth (push the open end into the solid)

place into the melting point apparatus with a thermometer

once you see sample starts to melt - take temperature

repeat - but this time when the melting point is approached - set to low and raise the temperature slowly to get more accurate reading

18
Q

how can some product be lost in purifying an organic solid

A

crystals lost when filtering / washing

some product may stay in solution after recrystallisation

other side reactions may occur

19
Q

when an alcohol is dehyrdated 0 why do two layers form

A

aq + organic layers have different densities and are immiscible

20
Q

why is the solution cooled in ice immediately after crystallisation

A

to decrease the solubility of the product so that it crystallises

lower temp increases size of crystals

21
Q

explain why recrystallisation separates impurities

A

impurities are more soluble in the cold solvent - remain in solution

22
Q

how to separate water soluble impurities

A

separating funnel