In CHM 246 you will be given at least two unknowns to completely identify:
1. On the computers, any unknown could be solid or liquid
2. The solid, analyzed in lab, will be a carboxylic acid, or a phenol.
ACIDS / PHENOLS
Solubility tests: Early in the analysis you will perform solubility tests:
Water insoluble acids are soluble in weak base (bicarbonate). Water insoluble phenols are soluble in strong base (hydroxide), sometimes with a color change.
In either case, we are talking about an enhanced solubility. Acids are more soluble in bicarb than in water; phenols are more soluble in (or react with) NaOH more than water or bicarb. Phenols can be confirmed with the ferric chloride test (see below).
Sodium Fusion Tests: This test detects presence of nitrogen.
Your unknown solid may, or may not, contain N. The nitrogen, if present,
could be an amine, a nitro group, a nitrile, etc. In the wet labs, the
sodium fusion test will not be done.
(NB - On the computers, your unknown may have Cl, Br, N or any combination
of these for any unknown. Be sure to run Na fusion.)
Melting Points: An important part of the characterization of
the unknown is a precise and accurate melting point. Precision: Be sure
that melting points are performed on small, well-packed samples. Be sure
that the rate of heating near the melting point is 1deg per minute. Accuracy:
The most sophisticated MP apparatus is worthless unless it is calibrated.
Reagent grade benzoic acid is available for this purpose. (Computer mp's
are usually correct.)