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Experiment 13
Name : __________________________ (
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Date : ____________
Mark : ______
Quickfit set
balance
titration apparatus
1.0 cm3 graduated pipette
measuring cylinder
ice bath
Procedures
[Hazard Warning : Glacial ethanoic acid and concentrated sulphuric(VI) acid are corrosive,
propan-1-ol is flammable, and 0.5M sodium hydroxide is irritant.]
1. Put 0.25 mole of glacial ethanoic acid (density = 1.05 g cm-3) and 0.25 mole of propan-1-ol
(density = 0.8 g cm-3) into a clean, dry pear-shaped flask. Mix thoroughly.
2.
Titration 1 : Transfer 1.0 cm3 of the mixture by pipette to a 250 cm3 conical flask
containing about 25 cm3 deionized water and 2 drops of phenolphthalein indicator. Titrate
to end point (twice) with 0.50M sodium hydroxide solution. Record the mean titre (V1
cm3).
3.
4.
Titration 3 : Add a few anti-bumping granules to the flask, and attach it to a water-cooled
reflux condenser. Reflux for 45 minutes. Cool the flask and its contents first under
running tap water, then in an ice-bath. Remove 1.0 cm3 sample from the flask for titration
with the 0.50M sodium hydroxide as before. Record the titre needed and correct it for the
sulphuric(VI) acid.
5. Titration 4 : Continue refluxing for an additional half hour, cool, and titrate another 1.0 cm3
sample. The two titres should agree to within 0.2 cm3. Otherwise, repeat this step.
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Results Tables :
Titration 1
1
Final burette reading / cm
Mean titre / cm
V1 =
V2 =
Titration 3
1
Final burette reading / cm
Mean titre / cm
Titration 4*
2
Titration 2
2
If the mean titre in titrations 3 and 4 do not agree, reflux for another half hour and carry
out titration 5.
Questions
1.
What is the purpose of adding a small amount of concentrated sulphuric(VI) acid to the
reaction mixture at the beginning of the experiment ?
2.
Why should anti-bumping granules be added to the reaction mixture before refluxing ?
3.
Why should the refluxing be continued in step (5) until the titre of sodium hydroxide used
approaches constant ?
4.
Write the equation for the esterification reaction between ethanoic acid and propan-1-ol.
5.
Calculate the concentration of ethanoic acid remaining at the end of the reflux.
6.
7.
8.
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