NAME: Filippos Chatzittofi F16190 SAMPLE: Ascorbic Acid BEHAVIOUR OF COMPOUND DURING HEATING AND BURNING (describe what you should see during the heating of your sample in burner and choose one of possibility): turning black, carbonization- EVERY TIME! · increasing of volume · melting · releasing vapours that are flammable · sublimation An organic compound will be burnt without a rest (it can leave a black coating on inner sides of a fusion tube, because of insufficient access of the air). -------ORGANIC----/INORGANIC/ORGANIC-INORGANIC COMPOUND ELEMENTARY ANALYSIS (write down the reactions of tests you should do and mark which of them should be positive): HALOGENS (HALIDES) Acidify a portion (5 mL) of the filtrate with dilute nitric acid, and if nitrogen and/or sulphur are present, boil for 1 - 2 minutes. Cool and add aqueous silver nitrate. Formation of a heavy, white, yellowish or yellow precipitate of silver halide indicates halogen. Should be negative 1. NITROGEN (CYANIDES) To a portion (5 mL) of the filtrate add a few drops of ferrous sulphate solution and a few drops of ferric chloride solution. Boil the mixture for half a minute, cool and acidify by adding dilute hydrochloric acid drop wise. Formation of a bluish-green precipitate (Prussian blue) or a blue solution indicates that the original substance contains nitrogen. If no precipitate appears, allow to stand for 15 minutes, filter and inspect filter paper. Corg. + Norg. CN- 6 CN- + Fe2+ [Fe(CN)6]4- [Fe(CN)6]4- + Fe3+ {FeIII[FeII(CN)6]}- Should be negative 2. SULPHUR (SULPHIDE) To the cold filtrate (5 mL) add a few drops of lead acetate solution. Production of a black solution or a black precipitate indicates that the original substance contains sulphur. Sorg. S2- S2- + Pb2+ PbS Should be negative No Sulphur no halides and no halogens present. SOLUBILITY (decide according to the information in Ph. Eur.): · Freely soluble in water, sparingly soluble in ethanol pH of solution/suspension (decide according to nature of your sample): · 2.1-2.6 solution REACTIONS FROM THE FLOWCHARTS (write down your “flowcharts pathway”; describe results of your hypothetical analysis – reactions from the flowcharts you can find in material called “Identification of an unknown drug”): Identification of an organic compound containing C, H, O It is soluble in water and Is acidic . Ascorbic acid or Citric acid or Tartaric acid IDENTIFICATION REACTIONS (from your monography choose the tests necessary for identification of your substance and describe them): First identification: B, C Second identification: A, C, D A. Ultraviolet and visible absorption spectrophotometry Test solution: Dissolve 0,10g in water R and dilute immediately to 100.0ml with the same solvent. Add 1.0ml of the solution to 10ml of a 10.3g/L solution of HCL R and dilute to 100.0ml with water R. B. Infrared absorption spectrophotometry C. pH (2.2.3): 2.1 to 2.6 for solution S Solution S : dissolve 1,0g in carbon dioxide free water R and dilute to 20 ml with the same solvent. D. To 1ml of solution S add 0.2ml of dilute nitric acid R and 0.2ml of silver nitrate solution R2. A grey precipitate is formed.