Microscale reflux
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Transcript Microscale reflux
Melting point
determination
Why take melting point?
To help identify sample
To check purity of sample
Filling sample holder
dip the open end
of the capillary
into dry, powdered
sample
several times,
shoving more in
each time
Packing the sample
drop the capillary
(closed end down)
through a long glass
tube
several times
until sample is
compacted at the
bottom
Turn machine on, and
set resistor for temp range
ON button
indicated
by white arrow.
Set dial
to expected melting
range
How to determine the right setting
This chart shows
heating curves
at various settings.
For accurate m.p.
determination
the expected m.p.
is on the flat
part of the curve
Taking m.p.
Turn on
the digital
thermometer
Taking m.p.
insert
up to 3
samples
Wait for
and watch
samples melt.
Record
melting range