Microscale reflux

Download Report

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