21. Two-step synthesis
- 01:00 What forms when the temperature is above 10oC?
- 01:10 Why the need to wash the product with ethanol?
- 01:14 Why the need to use a minimum volume of hot methanol?
- 02:09 What’s the reason for adding acid at this stage?
- 02:23 Why use only a minimum volume of HCl?
- 02:31 How do you know how pure your sample is?
- 02:37 What affects percentage yield?
cold de-ionised water
digital balance (pref. 3-d.p but minimum 2-d.p.)
access to ice
spatula
weighing-boat
2 x 100 cm3 conical flask
25 cm3 measuring cylinder
ice-bath
glass Pasteur pipette with rubber teat
glass stirring rod
250 cm3 beaker
buchner funnel + suction apparatus
filter paper
10 cm3 measuring cylinder
hot water-bath
round-bottomed flask or pear-shaped flask
reflux condenser
thermometer
sample vial
labels / fine-tipped permanent marker
anti-bumping granules
heating mantle / Bunsen burner with water-bath
clamp-stand, clamp, boss
melting-point apparatus / Thiele tube
capillary tube
Hazard | Risk | Control measure |
---|---|---|
Conc. H2SO4 solution – corrosive. |
Contact with eyes & skin |
Eye: flood with tap-water (10min). See doctor. Skin: remove excess with dry towel. Drench with water |
Methylbenzenecarboxylate (C6H5COOCH3) – irritant. |
Ignite close to flame. |
Extinguish using fire-blanket |
Conc. HNO3 solution- corrosive |
Contact with eyes & skin. |
Eye: flood with tap-water |
Methanol (CH3OH) – flammable, acute toxicity, serious health hazard. |
Ignite close to flame. Contact with skin/eyes or swallowed. |
Extinguish using fire-blanket. |
Solid sodium hydroxide – corrosive. |
Contact with skin & eyes. |
Eye: flood with tap water Skin: drench with water |
Conc. HCl solution – corrosive |
Contact with skin & eyes |
Skin: remove excess with dry towel. Drench with water. Eye: flood with tap water (10min). See doctor |
0.1 mol dm-3 HCl solution – no hazard. |
Contact with skin & eyes. |
Skin: drench with water. Eye: flood with tap water (10min). |