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Sr., No., , Test, , Observation, , Inference, , Distinguish between Acid & Phenol:, a. Effervescence of CO 2, Acid is Prsent., b. No effervescence of CO2, Phenol is Present., , Sub + 4 drops 10 %, Sodium bicarbonate, solution (NahCO3), III., If acidic, add a sub to Soluble with effervescence of, 10 % sodium, CO2 & reprecipitated by Conc, bicarbonate solution. HCl, IV., If not soluble in water Completely soluble &, then try 2 N NaOH, reprecipitated by conc HCl, If not soluble in 2N, Completely soluble &, V, NaOH , then try in, reprecipitaed with 2N NaOH, dil. HCl, (exess ), If all the tests I, II, III, are negative, 4., Action of reagent:, I., , II., , III., , IV., , Action of cold NaOH, :, About 0.2 gm / 3, drops of compound +, 2 ml of water + 2ml, of 10% NaOH &, mixture is shaken, well., Action of hot conc, H2SO4 :, 0.1 g solid or 2, drops of liquid +, 1ml conc. H2SO4, warm., , Action of Na2CO3:, 10 ml of 10 %, Na2CO3 solution +, 0.2g of solid or 4, drops of liquid., Action of KMnO4, solution:, 0.2 g of solid or 4, drops of liquid + 10, ml Na2CO3 solution, + drop by drop, KMnO4, , Acid is present & confirmed., , Phenol is present & confirmed., Base is present & confirmed ., , Neutral sub. is present., , Yellow color changes to Orange, red., No orange red colour, , a. Nitrophenol is present., , Completely soluble, , c. Acid / Phenol is present., , b., , Nitrophenol is absent., , Blackening with effervescence, of CO2 or SO2, , Carbohydrates like cane sugar or, higher hydroxyl acid., , Blackening without, effervescence, , Poly-phenols, phenolic acids., , Effervescence but no blacking, , Formic , Oxalic or citric acids., , Pungent vapours, , Acetic acid, benzoic, succinic ,, phenol & its derivatives esters., , Yellow color changing to, brown but no changing, , Glucose., , Effervescence of CO2, No effervescence of CO2, , Acid is present., Acid is absent., , Pink color of KMnO4, disappears, , Unsaturated or easily oxidisable sub, is present., , No decolourisation, , Saturated sub is present., , 2
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Sr., No., V., , Test, Action of Bromin, water:, , Observation, , Inference, , Decolorisation without, precipitate, , Unsaturated compound., , Decolorisation with formation, of precipitate, Action of bromine, in CHCl3 :, , VI., , Action of FeCl3, Solution :, Sub + Water + 2-3, drops of FeCl3, solution., , Decolourisation without, evolution of HBr., Decolorisation with HBr, , Unsaturated compound., , Green coloration changing, through blue 7 violet to red by, Na2CO3, , O- Dihydroxybenzene i.e. catechol., , VIII., , Heating on Oxidized, Copper gauze :, (Beilstain test), Take 10 mg sub on, clean copper gauze, (spatula) & heat on a, blue flame., Heating with Soda, lime:, Take in hard glass, test tube , o.5 g of sub, + 2g of finely, powdered soda lime., Close the tube by a, cork with a bent, delivery tube , heat, from top of test tube, downwards gently at, first & then strongly, & collect the product., , Saturated compound or compound, which is easily brominated e.g., aldehyde or Ketone, , Red color, , Phenol, phinolic acid (e.g. Salicylic, acid ), Phinolic ester (e.g. methyl, salicylate), p-Hydroxybenzolic acid., , Sooty Flame, , Aromatic sub is present., , Non- sooty Flame, , Aliphatic sub is present., , Green Flame, , Halogen is present., , Formation of aniline, , Sulphanillic or anthranilic acid., , Smell of burnt sugar, , Carbohydrates, citric or tartaric acid., , Smell of nitrobenzene, , Nitrobenzoic acid., , Blue or violet colouration, , VII., , Compound which is easily, brominated e.g. phenol aromatic, amine etc., , Conclusion:, On the basis of test performed above & with reference to handbook the given organic drug, compound is :, - Aromatic / Aliphatic Saturated / Unsaturated, - Acidic / basic/ Neutral / Phenol halide., 3
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II., , DETERMINATION OF PHYSICAL CONSTANT:, , 1. Melting point: It is defined as the temp. at which a solid sub in condition of equilibrium, passes into liquid state ., 2. Boling Point: It is defined as temp. at which vapour pressure of liquid becomes equal to b, atmospheric pressure., Conclusion: The melting point / boiling point of the given organic compound was found to, be…….. °C, III., , DETERMINATION OF ELEMENT (Lassigne’s Test):, Take a sodium fusion tube (small tube ) & place very small dry pieces of sodium metal, in it. Then heat the tube till sodium gets fused. Cool the tube & place little sub. (Solid or, Liquid) in it.. Then heat the tube gently, If vigours reaction occurs , remove the flame ,, allow the reaction to stop. Add further little quantity of sub & continue heating to, redness for 3-4 min. Then break the hot tube in 5-10 ml distilled water taken in, evaporating dish. In this way break at least two tubes. Concentrate the solution by, boiling & filter it. This filtrate is called as sodium fusion extract. Test filtrate for, presence of nitrogen, sulphur & halogen as follows., Sr., No, a., , b., , Test, Test for Nitrogen :, 1 ml sodium extract + few crystals of, FeSO4 + 1 drop of NaOH boil well ., cool in ice water & acidify with conc., HCl or dil. H2SO4, Test for Sulphur:, 1. 2ml filtrtate + 1 drops of dil. Sodium, hydroxide solution+ 4 drops of, freshly prepared & very dil. Solution, of sodium nitruprusside., , Observation, Green or Blue colour, , Nitrogen is, present., , Instant purple colour, , A black ppt of lead, 2. 2 ml filtrate + acetic acid to acidify + sulphate., few drops of lead acetate solution, , 3. 2ml filtrate +HCl to neutralize the, solution + few drops of FeCl3, solution., , Inference, , Deep red color, discharged by HgCl2, , Sulphur present, , Sulphur present, , Sulphur & nitrogen, present, , 4
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Sr., No, C., , Test, , Observation, , Inference, , Test for Halogen:, Acidify 5 ml the filtrate with dil. H2SO4, boil well to reduce the volume to one, third to expel H2S if N , already found, to be present. Then add few drops of dil., HNO3 (to acidify & AgNO3 ) solution., Chloroform layer test:, Filtrate , acidify with conc. HCl &, mineral acid + 1 ml of chloroform + few, drops of of fresh chlorine water, shake, well & observe the color of chloroform, layer., , Heavy , curdy , white, or yellow ppt. of, silver halides., , A halogen present, , Color of lower layer., 1. Colorless, , Chlorine present., , 2. Yellowish, brown, , Bromine present, , 3. Violet, , Iodine present., , NOTE:, From sodium fusion test all Organic substances are classified as follows:, 1. Substances containing C, H, (O) elements.: Salicylic acid, Benzoic acid,, Resorcinol, Dextrose, Acetone, ethyl, acetate, Ethyl alcohol, 2. Substance containing C,H, (O) & N elements : ( Nitrobenzene , Urea), 3. Substance containing C,H , (O) N & S elements: (Thiourea), 4. Substance containing C, H, (O) & halogen elements: (Chloroform), , Conclusion: The given organic drug/ compound found to contain ....... ………… elements., , 5
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IV., , DETERMINATION OF FUNCTIONAL GROUP/GROUPS, (FOR…………..ELEMENTS.), A. Compound containing C,H, (O) Elements:, Sr., No, 1, a), b), , Test, , Observation, , ACIDS- (R-COOH or Ar-COOH), Functional Group Test:, Effervescence of CO2, 10mg sub. +10% NaHCO3, Sepration of acids:, a)Violet colour, i)Neutral solution of acid sub. + discharged by dil. HCl, 2 drops of FeCl3, b)Buffer or brown ppt,, solution in dil HCl., , Infernce, Carboxylic group, Acid is present, a)Salicylic acid., a)Aspirin., b)Benzoic acid, b)Clinamic acid., b)Phthalic acid., c)Acetic acid., , *Neutral Solution of Acid: 0.1 g of given acid sub + 1ml NH4OH boil well till ammonia gets, evolved (i.e. moist turmeric paper should not turn brown). Use this solution for sepration of above, acids., , 2, a), , b), , PHENOLS-(Ar-OH), Functional Group Test:, 10mg sub. + 10 drops ethyl, alcohol +2-3 drops of neutral, FeCl3., Separation of Phenols:, 1mg sub. + Phthalic anhydride, +2 drops of conc. H2SO4 ., Warm then cool in ice + Excess, of NaOH., , 3)NEUTRAL, A)Carbohydrates(Water soluble solid), 10 mg sub. +3-4 drops of αnaphthol in alcohol. Shake, well., Then add 1ml conc. H2SO4, From the wall of test tube., B)Ketones-(R-CO-R,), 1)10mg/2-3 drops of sub +4, drops of sodium nitroprosside +, NaOH shake it., C)Esters- (R-COO-R’), (Liquids-water immiscible), , a)Blue/ Green/Violet, colour., , Ar-OH (Phenolic), group present., , a)Very faint green, colour with, slightflurosence., b)Dark green, colouration., c) Yellowish red, solution with green, florescence., , a) β-naphthol., , Violet red colouration, at the junction of the, two layers., , Carbohydrates present., (Dextrose), , Red colour, , Ketone is present., (Acetate), , Pink colour disappears, after heating., , b) α-naphthol., c)Resorcinol., , Ester group is present., 6
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2-3 drops of sub+1ml water+1, drop of phenolphthalein +very, dil. Naoh till a pink colour, appears & persists. Then heat, the tube., D) Alcohol—(R-OH), Liquids, 5-6 drops of sub. In a dry test, tube + a piece of dry sodium, metal & close the mouth of, tube with thumb & heat in a, water bath., , (Phenolphthalein gives,, pink colour in alkaline, media. Ester on, hydrolysis gives an, acid hence pink colour, disappears), , (Ethyl acetate), , Evolution of H2 gas, , Alcohol is present., (Ethyl alcohol), , B. Compound containing C,H, O, N Elements:, Sr. No, Test, Neutral substances, Nitro-hydrocarbons:, (yellow solid/liquid), (Ar-NO2), 10 MG SUB + 1 ml 50%, alcohol + 6 drops of CaCl2 +, pinch of Zn dust. Heat to boil &, filter into 1 ml of Tollens, reagent, (5 drops AgNO3 + 1 drop of, NaOH+ NH4OH till ppt., dissolves.), Amides- (R-CO-NH2), ( water soluble solid), 10mg sub. + 1ml NaOH & boil, it., , Observation, , Inference, , Black or Gray ppt., , Nitro-hydrocarbon, present., (Nitrobenzene)., , Evolution of NH3 gas, which turns turmeric, paper red., , Amide group is present., (Urea), , C. Substance containing C, H, (O) N & S Elements:, Sr.No., , Test, , Observation, , Inference, , 10 mg sub. Fuse in a test tube, cool, + 1 ml water + 2 drops FeCl3, Solution., , Blood red Solouration, , Thiourea, present., , 7
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D. Substance containing C, H, (O) & Halogen Elements:, Sr.No., , Test, 5 drops sub. + 1 ml Noah, boil well, & cool, acidify with conc. HNO3., Then add 2 drops AgNO3 & shake, well., , Observation, a] white ppt settles at the, bottom., , b] No white ppt at the, bottom., , Inference, a] Aliphatic, halide present, (R-X), (chloroform), b] Aromatic, halide present, (Ar-X), (Chlorobenzene), , Conclusion: The given organic drug/ compound was found to contain……… Functional group / groups., Results: The given organic drug/ compound was having…………………………C M.P./ B.P., …………………………With reference to literature the organic drug/ compound may be………, , 8
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V., , Characteristic tests (C.T.) for substances:, , Compound containing, C, H (O) elements, 1. Acids: R-COOH, Structure, Salicylic Acid (M.P., 158°C), , Test, , Observation, , 5 mg sub + 10 drops methyl alcohol +, 3-4 drops of conc., H2SO4, warm it., , Smell of Methyl salicylate, , COOH, 10 mg sub. + Soda lime (1:3) mix well., Heat the mixture in a test tube., , Smell of phenol., , Sub. + Phthalic unhydride in dry test, tube moisten with few drops of H2SO4, Cool, Excess of NaOH solution, , Red coloration., , 10mg sub. + 1ml ethyl alcohol + 4-5, drops of conc. H2SO4 warn it., , Smell of ethyl benzoate (ester)., , Sub. + Ferric chloride solution., , Pale buff color, , Take 5 drops acetic acid in a test tube,, add 1 ml ethyl alcohol &3-4 drops, of conc. H2SO4 .warm on water bath., , Fruity smell of ethyl acetate, (ester)., , 10 mg sub. + 10% Noah + 5 drops of, chloroform (CHCl3)., , Brilliant red color, , 0.2 gm of sub. + 0.2 ml of conc. H2SO4., Cool Sol. & pour it in water, , Green color fluorescence, , OH, , Benzoic acid (, M.P.122.C), , COOH, , 3] Acetic acid: (B.P., 101.C):, , O, H3C, , OH, , 2] Phenols: (Ar-OH), Resorcinol, (M.P.108.C):, OH, , OH ., , 9
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Structure, , Test, , Observation, , Neutral Substances, Carbohydrates:, Glucose (Dextrose):, (M.P. 146 °C), , Dissolve 10mg of glucose in water &, Red ppt of Cu2O is formed, add few drops of fehlings solution (A+B, equal amount) & warm, , Iodoform test: Take about 4 drops, acetone in test tube. To this add 10%, Acetone : (B.P. 56®C) Na2CO3 or NaOH solution. Then add, I2 solution with constant shaking till, ., colour persists Warm on water bath, Ketones: (R-CO-R’), , O, H 3C, , CH3, , C)Ester (R-COOR’), Ethyl acetate : (B.P., 77 °C), O, H 3C, , O, , Red colour obtained, , Barfoed’s test :, 1ml of sol. + 1ml Barfoed’s reagent., Heat on water bath., , C6H12O6, , Pale yellow coloured crystals of, iodoform settle at the bottom., , 10 mg sub + 10mg m-dinitrobenzene Violet Color, +NaOH in excess & shake, ., 10 mg sub. +1ml dil.NaoH & boil., , Smell of ethyl alcohol, , C 2H 5, , Ethyl alcohol: (B.P., 77 °C), , 1. Miscible with water, 2. 5 drops of ethyl alcohol +1 ml Pale yellow coloured crystals of, , CH3-CH2-OH, , a, , NaOH + I2 solution & warm on iodoform., water bath, , ., , Neutral Substances Containing C, H, (O) & N elements., Structure, Urea : (M.P. 132®C, ., , Test, Biuret test: Heat a little quantity of urea in, , Observation, Violet to deep blue, , a dry test tube. Add 1 ml NaOH. Shake &, add drop wise very wise dil. CuSO4 solution., , 10
