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ERROR2 an experiment has been performed below. what can be the sources of error in this experiment and how can you devel

Posted: Sun May 22, 2022 5:01 pm
by answerhappygod
ERROR2
an experiment has been performed below. what can be the sources
of error in this experiment and how can you develop the
experiment to get a better yield, for example. The
yield is written below.
alcohol oxidation= 20 mmol
flowchart alcohol oxidation
transfer to a 50 ml erlenmeyer flask of 2,1 ml of
cyclohexanol, 10ml ethyl acetate and 1,6 ml of pyridine by
pipette.

add a stir bar and stir the mixture until
homogeneous.

mix 5ml ethyl acetate and 1,2g TCCA and transfer into a
100 mL beaker, then stir with a glass stirring until it dissolved
(takes a few minutes)

transfer the mixture of the beaker to a separatory
funnel and set up as a dropping funnel for the erlenmeyer
flask

drip the contents of the separatory funnel into the
erlenmeyer flask over a period of 5-10 min (the erlenmeyer flask
will be hot make sure it does not get hotter than 40
degrees)

stir the solution an additional 20 minutes

run a TLC of the solution by using as a eluent 30% ethyl
acetate and 70% hexane (If the alcohol is not detected by TLC glass
wool filter the solution and rinse the product that is stuck in the
filter funnel with 3-5 ml of ethyl acetate.)

test the solution for excess TCCA by placing a drop of
the reaction mixture on a wet starch-iodine test drip. If you get a
color its positive means that you will add 3-5 ml saturated sodium
bisulfite and shake vigorously. If you don't get any color or light
yellow it means negative so continue with next
step

Wash three times the organic layer with 10mL 1 M HCl, 10
mL 5% sodium bicarbonate (NaHCO₃) and 5 mL saturated NaCl.
Separate the two different layers and discord the lower aqueous
layer after every wash.

transfer the organic layer to a 50 mL Erlenmeyer flask
and dry it with MgSO₄

glass wool filter the solution

evaporate with rotary evaporator

record the yield and run IR-spectra
Theoretical yield: 0,02x100,168g/mol= 2,00g
maximum
Weight of the rounded bottom flask= 78,65g
weight of the rounded bottom flask + products solution=
80,51g
weight of the products solution=
80,51g-78,65g=1,86g
Yield= 1,86g/2gx100= 93%.