REAZIONI DI IDENTIFICAZIONE DI ANIONI DI INTERESSE FARMACEUTICO E TOSSICOLOGICO • • • • • Cloruri Bromuri Ioduri Solfati Borati • • • • • Nitrati Fosfati Ossalati Carbonati e bicarbonati Acetati 1 CLORURI CHLORIDES (Eu Ph) a) Dissolve in 2 ml of water R a quantity of the substance to be examined equivalent to about 2 mg of chloride (Cl–) or use 2 ml of the prescribed solution. Acidify with dilute nitric acid R and add 0.4 ml of silver nitrate solution R1. Shake and allow to stand. A curdled, white precipitate is formed. Centrifuge and wash the precipitate with three quantities, each of 1 ml, of water R. Carry out this operation rapidly in subdued light, disregarding the fact that the supernatant solution may not become perfectly clear. Suspend the precipitate in 2 ml of water R and add 1.5 ml of ammonia R. The precipitate dissolves easily with the possible exception of a few large particles which dissolve slowly. Cl- + Ag+ AgCl AgCl + 2NH3 [Ag(NH3)2]+ + Cl[Ag(NH3)2]+ + Cl- + 2H+ AgCl + 2NH4+ Composti di interesse farmaceutico HCl, NaCl, KCl, CaCl2, MgCl2, NH4Cl Attività farmacologica e tossicologica Elemento essenziale. 2 BROMURI BROMIDES (Eu Ph) a) Dissolve in 2 ml of water R a quantity of the substance to be examined equivalent to about 3 mg of bromide (Br–) or use 2 ml of the prescribed solution. Acidify with dilute nitric acid R and add 0.4 ml of silver nitrate solution R1. Shake and allow to stand. A curdled, pale yellow precipitate is formed. Centrifuge and wash the precipitate with three quantities, each of 1 ml, of water R. Carry out this operation rapidly in subdued light disregarding the fact that the supernatant solution may not become perfectly clear. Suspend the precipitate obtained in 2 ml of water R and add 1.5 ml of ammonia R. The precipitate dissolves with difficulty. Br - + Ag+ AgBr AgBr + 2NH3 [Ag(NH3)2]+ + Br Acqua di cloro 2Br - + Cl2 Br2 + 2Cl - (colora di giallo CHCl3) Acido solforico conc. 2Br - + SO42- + 4H+ Br2 + SO2 + 2H2O Composti di interesse farmaceutico KBr, NaBr, NH4Br Attività farmacologica e tossicologica Elemento microessenziale. 3 IODURI IODIDES (Eu Ph) a) Dissolve a quantity of the substance to be examined equivalent to about 4 mg of iodide (I–) in 2 ml of water R or use 2 ml of the prescribed solution. Acidify with dilute nitric acid R and add 0.4 ml of silver nitrate solution R1. Shake and allow to stand. A curdled, pale-yellow precipitate is formed. Centrifuge and wash with three quantities, each of 1 ml, of water R. Carry out this operation rapidly in subdued light disregarding the fact that the supernatant solution may not become perfectly clear. Suspend the precipitate in 2 ml of water R and add 1.5 ml of ammonia R. The precipitate does not dissolve. I- + Ag+ AgI b) To 0.2 ml of a solution of the substance to be examined containing about 5 mg of iodide (I–) per millilitre, or to 0.2 ml of the prescribed solution, add 0.5 ml of dilute sulphuric acid R, 0.1 ml of potassium dichromate solution R, 2 ml of water R and 2 ml of chloroform R. Shake for a few seconds and allow to stand. The chloroform layer is coloured violet or violet-red. 6I + Cr2O72 + 14H+ 2Cr3+ + 3I2 + 7H2O Acqua di cloro 2I - + Cl2 2Cl - + I2 (colora di viola CHCl3) 4 2I - + Cl2 2Cl - + I2 I2 + 5 Cl2 + 6 H2O 2 IO3- + 10 Cl- + 12 H+ Acido solforico conc. 2 I- + SO42- + 4H+ I2 + SO2 + 2H2O Composti di interesse farmaceutico KI, NaI, I2 Attività farmacologica e tossicologica Elemento oligoessenziale. 5 IO3- / I2 = 1,19 BrO3- / Br2 = 1,52 6 SOLFATI SULPHATES (Eu Ph) a) Dissolve about 45 mg of the substance to be examined in 5 ml of water R or use 5 ml of the prescribed solution. Add 1 ml of dilute hydrochloric acid R and 1 ml of barium chloride solution R1. A white precipitate is formed. Ba 2+ + SO4 2- BaSO4 Composti di interesse farmaceutico Na2SO4.10H2O, MgSO4.7 H2O, CuSO4, BaSO4, ZnSO4 7 BORATI Borax Borax Na2B4O7,10H2O Mr 381.4[1303-96-4] DEFINITION Disodium tetraborate decahydrate. Content: 99.0 per cent to 103.0 per cent of Na2B4O7,10H2O. CHARACTERS Appearance: white ►or almost white◄, crystalline powder, colourless crystals or crystalline masses, efflorescent. Solubility: soluble in water, very soluble in boiling water, freely soluble in glycerol. IDENTIFICATION A. To 1 ml of solution S (see Tests) add 0.1 ml of sulphuric acid R and 5 ml of methanol R and ignite. The flame has a green border. 3CH3OH + H3BO3 3 H2O + B(OCH3)3 8 HO Curcumina O R R= O O R CH=CH R OH B OH O R O H3BO3 R R + H2O OH OCH3 Composti di interesse farmaceutico H3BO3, Na2B4O7.10H2O, NaBO3 Attività farmacologica e tossicologica Elemento traccia-essenziale. 9 NITRATI a) Via umida Solfato ferroso soluzione satura NO3- + 3Fe2+ + 4H+ 3Fe 3+ + NO + 2H2O Fe 2+ + NO + SO42- [Fe(NO)]SO4 b) Via secca Lega di Devarda (45% Al, 5% Zn, 50% Cu) NO3- + 4Zn + 7OH - + 6H2O NH3 + 4[Zn(OH)4]2- 3NO3- + 8Al + 5OH - + 18H2O 3NH3 + 8[Al(OH)4]Composti di interesse farmaceutico KNO3 10 FOSFATI PHOSPHATES (ORTHOPHOSPHATES) (Eu Ph) a) To 5 ml of the prescribed solution, neutralised if necessary, add 5 ml of silver nitrate solution R1. A yellow precipitate is formed whose colour is not changed by boiling and which dissolves on addition of ammonia R. 3 Ag+ + PO43- Ag3PO4 b) Mix 1 ml of the prescribed solution with 2 ml of molybdovanadic reagent R. A yellow colour develops. Reattivo molibdico 3NH4+ + 12MoO42- + PO43- + 24H+ (NH4)3PO4.12MoO3 + 12H2O Composti di interesse farmaceutico NaH2PO4.2H2O, CaHPO4, KH2PO4 Attività farmacologica e tossicologica Elemento essenziale. 11 OSSALATI Argento nitrato 2 Ag+ + C2O4 2- Ag2C2O4 Calcio cloruro C2O4 2- + Ca2+ CaC2O4 2 MnO4- + 5 H2C2O4 + 6 H+ 2 Mn 2+ + 10 CO2 + 8 H2O Attività farmacologica e tossicologica Sequestra ioni calcio. 12 CARBONATI e BICARBONATI CARBONATES AND BICARBONATES (Eu Ph) Introduce into a test-tube 0.1 g of the substance to be examined and suspend in 2 ml of water R or use 2 ml of the prescribed solution. Add 3 ml of dilute acetic acid R. Close the tube immediately using a stopper fitted with a glass tube bent twice at right angles. The solution or the suspension becomes effervescent and gives off a colourless and odourless gas. Heat gently and collect the gas in 5 ml of barium hydroxide solution R. A white precipitate is formed that dissolves on addition of an excess of hydrochloric acid R1. CO32- + 2H+ CO2 + H2O CO2 + Ba2+ + 2OH- BaCO3 + H2O Composti di interesse farmaceutico CO2, Na2CO3, NaHCO3, CaCO3, MgCO3, K2CO3, KHCO3 Attività farmacologica e tossicologica Antiacido gastrico HCO3- /H2CO3: sistema tampone dell’organismo 13 ACETATI ACETATES (Eu Ph) a) Heat the substance to be examined with an equal quantity of oxalic acid R. Acid vapours with the characteristic odour of acetic acid are liberated, showing an acid reaction (2.2.4). 2CH3COOK + H2C2O4 2CH3COOH + K2C2O4 Composti di interesse farmaceutico Acido acetico, Mg-acetato, Na-acetato, K-acetato, Ca-acetato 14