BUCHI Melting Point M-565 - Manual (Page 27)

6 Operation
27 Melting Point M-565 Operation Manual, Version D
Preparation of the samples:
• The samples being investigated must be fully dry, homogenous, and in powdered form. Moist
samples must be dried first (the pharmacopoeias prescribe that the substance needs to be dried
in a vacuum for 24 hours over silica gel R). Coarse crystalline samples and non-homogeneous
samples are finely ground in a mortar.
• To fill the capillary tubes with the sample, the open ends of the tubes are pressed into the
substance. The substance is moved to the bottom of the tubes by repeatedly pounding the tubes
against a hard base.
• Enough substance must be filled into the glass capillary to form a compact column 4 to 6 mm
in height. (A height of 4–5 mm is recommended for precision measurements.) To ensure compa-
rable results, it is important to fill all three capillary tubes to the same height and to compact the
substance well in the tubes using the Sample Loader M-569.
6 .2 .2 Determination without pre-registered melting point method
• Choose the menu for melting point determination.
• Make sure that all samples are removed.
• Press START to start the determination process immediately with the last parameters used.
NOTE
If the current parameters do not meet your needs, press Edit and set start temperature, stop temper-
ature, and temperature gradient.
a b c
d
a Start temperature
b Stop temperature
c Temperature gradient
d Edit
• To adjust the desired melting parameters,
press Edit.
• Chose start temperature
with the rotary knob, and
press
Next.
• Chose stop temperature
with the rotary knob, and
press
Next.
• Chose temperature
gradient with the rotary
knob, and press
Save.