By M. R. F. Ashworth
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Extra resources for Analytical Methods for Glycerol
Sodium periodate-1 % potassium permanganate in 2% aq. sodium carbonate (1+4). After leaving at room temperature and then washing under the tap they obtained brown spots on an almost white background. Rather more specific tests are based on oxidation to formaldehyde, which is then detected. An early example is due to Kolthoff (1924) who treated the sample for 10 min with 4 N phosphoric acid and 3 % potassium permanganate. After adding acetic and dilute sulphuric acids he then tested with the Schiff reagent which demonstrated through a reddish-violet colour that formaldehyde from glycerol oxidation was present.
Carbonyl Compounds Bally and Scholl (1911) showed that acrolein reacts with an throne to give benzan throne: This dimerises in cone, sulphuric acid to give violet-red dibenzanthrone or green isodibenzanthrone. Schutz (1938) based detection of as little as 2 [ig of glycerol per ml in parchment paper extract on this. The aqueous extract was heated to 170°C with 0-1 % anthrone-conc. sulphuric acid to give a reddish-yellow solution with marked orange fluorescence, intensified by adding sulphuric acid.
Acrolein was then identified through the eutectic temperature of its p-nitrophenylhydrazone, thus prepared, with acetone p-nitrophenylhydrazone, prepared from a drop of aqueous acetone and the same reagent in excess. Ganassini (1930) utilised hydrazone formation in a colour test. He heated the sample with potassium hydrogen sulphate, boron trioxide, or phosphorus pentoxide to give acrolein, reacting this with phenylhydrazine and converting the phenylhydrazone into phenylpyrazoline which yielded a violet colour with acidic oxidising agents.
Analytical Methods for Glycerol by M. R. F. Ashworth