Ignition Test
Observation White/Yellow/Brown etc. Solid/Liquid Fruity Pungent Carbolic/Phenolic Bitter Almond Kerosene Aromatic Odour Luminous, Sooty Flame Non-Luminous, Non-Sooty Darkens, Chars with smell of burnt sugar Melts, Vapourises, smells like NH3 Green flame [on a copper wire]
Tests for Unsaturation 1) Bromine Test 0.2g/0.2ml of compound in 2 cm Ccl4 + 2 % Br in Ccl4 (DropWise) (Blow across the mouth of the test tube) Decolourisation, No evolution of HBr Decolourisation, Evolution of HBr No Decolourisation 2) Baeyers Test: 0.2g/0.2ml of compound in H2O/acetone + Cold KMnO4 soln. (Drop Wise)
Decolourisation No Decolourisation
Inference
Esters Volatile Acids Phenolic Compounds Nitrobenzene/Benzaldehyde Aromatic Hydrocarbons Aromatic Compounds Aromatic (highly unsaturated) Saturated Aliphatic Sugars Amides/Urea Halogenated Compound
Experiment Nitrogen: 2 cm SFE + 2 cm Fresh FeSO4 soln. Boil. + sufficient dil. H2SO4 to dissolve Fe Hydroxides. + drops of FeCl3
Black ppt.
Halogens 1) If N or S Absent: 2 cm SFE + dil. HNO3 + 1-2ml AgNO3 2) If N or S Present: 2 cm SFE + conc. HNO3 (Boil till 1/2 Volume) + 1-2ml AgNO3
Distinguish Halogens: 2 cm SFE + dil. Hcl + few drops CCl4 + Cl2 Water, Shake
Inference
Nitrogen Present
Sulphur Present
Experiment CARBOHYDRATES: 1) Ignition Test 2) Dehydration: 0.2g (dry)+ conc. H2SO4, warm 3) Molisch's Test: 0.1g in 2ml water + 2 drops -naphthol in Alcohol +2ml conc. H2SO4 (Slowly on sides of tube)
Observation
Inference
Non Luminous, Smell of Burnt Sugar, Black Residue Carbohydrate Charred, turns black Carbohydrate
Carbohydrate
4) Seliwanoff's Test: 0.1g + 2-3ml 0.1% Resorcinol in water + conc. H2SO4 Carefully without mixing
Carbohydrate
5) Fehling's Test: 4ml Fehling's soln (2ml A + 2ml B) + 0.1g in 2ml water. Boil 2 mins. Red ppt. Reducing Sugar
Observation Smell of NH3, dense white fumes with conc. HCl, gas-> red litmus to blue
Divide above soln. into 2 parts a)Cool 1 part, acidify with conc.HCl White ppt b) Other part, evaporate to dryness on china dish + 2-3ml Alcohol + conc. H2SO4 & Warm. Cool and pour into water. Fruity Odour 2) 3ml HgCl2 soln. + NaOH drop wise til yellow ppt. of HgO is formed. + 0.2g compound. Warm On Heating, yellow ppt. HgO dissolves. 2RCONH2 + HgO (RCONH)2Hg + H2O Pass H2S through soln. 3) Nitrous Acid test: 0.2g in 1ml dil. HCl + 1ml of cold fresh NaNO2 soln. 4) Hydroxamic acid Test: 0.1g + 1ml hydroxylamine hydrochloride in propylene glycol + 4-5 drops 10% NaOH soln. Boil, cool, acidify with HCl + 1-2 drops of FeCl3 Black ppt. Brisk Effervescence of Nitrogen Amide of aromatic acid Amide Amide Amide Primary Amide
Burgundy/Magenta Colour
Amide
Experiment Urea 1) 0.2g + 5ml 20% NaOH 2) Nitrous Acid Test: 0.2g+ 2-3ml dil. HCl + 3ml 5% NaNO2 3) Biuret Test: 0.5g in dry t.t + heat above M.P. 1-2min .. dissolve above residue + few ml 10% NaOH soln. Cool+ 1 drop of CuSO4
2 CO(NH2)2H2N-CO-NH-CO-NH2 + NH3
Observation Pungent gas with smell of NH3. Gas-> Blue litmus to red Brisk effervescene of N2 and CO2
Inference
Urea Urea
Purple Colour
Urea
White Crystals
Urea
Experiment AMINES: 1) Carbyl amine test: compound in alcohol + 2ml of 10% alc. KOH + CHCl3 destroy the isocyanide adding dil. HCl or dil. NaOH
Observation
Inference
Offensive Odour
Primary Amine
2)Benzoylation 0.2g+ 2ml benzoyl chloride+ 2ml 10% NaOH, warm on water bath, pour into water or 0.2g+ 2ml benzoyl chloride + 5% NaOH in a conical flask & Cork shake until solid separates Schotten-Baumann Reaction:
Solid Derivative
Primary/Secondary Amine
3) Acetylation 0.2g+ Acetyl Chloride/ water+acetic anhydride. Drop Wise. Warm on water bath & pour into water, Stir RNH2 + ClOCCH3 ----> RNHOCCH3 -HCl R2 NH + ClOCCH3 ----> R2 NOCCH3 - HCl
White solid
Primary/Secondary Amine
4) Action of Nitrous Acid sub. + 5ml of (1:1 HCl), warm, if insoluble. Cool to 0degC in ice, add cooled soln. of NaNO2 slowly. Brisk evolution of N2 gas Little/no evolution of gas, clear soln. no evolution of gas but yellow oil separates slowly colored soln.
Alkyl primary amine Aromatic Primary Amine Secondary Amine Tert. Amine
Red Dye
b) Libermann's Rxn: 2nd part (oil) + wash with water to remove NaNO2+ few drops of conc. H2SO4+ Heat, cool pour into water. Add xs NaOH
Greenish-Blue colour, changes to pale red adding water, Deep blue adding alkali secondary amine
c) 3rd part + NaOH, after 5 mins + few ml of ether, shake 5) Substance + acetone + Sodium nitroprusside soln. 6) [In 1 testube Substance+water or dil.HCl]+ [In another testube: NiCl2--CS2 reagent 1ml + liq. NH3]
Green ppt., ether layer turns green Violet/ red White/Tan ppt.
Red/Purple
Tert. Amine
Experiment Carboxylic Acids: 1) Reaction with NaHCO3 substance+sat.aq soln. of NaHCO3. If no rxn takes place. Warm
CH3COOH + NaHCO3CH3COONa+ + CO2 + H2O
2) Litmus Test Compound in water. Dip Litmus 3) Ester Formation 0.5g+ 2ml Ethanol + 3-4 drops conc. H2SO4, heat for 2min., cool and pour into beaker containing Na2CO3 soln. RCO2H + R'OH ---> RCO2R' + H2O 4)Amide Formation compound+ Pcl5 on watch glass/mortar, mix well and add liquor ammonia
RCOOH SOCl R
2
C O
Cl + SO 2 + HCl
3 RCOOH
PCl 3
3R
C O
Cl + H 3 PO 3
RCOOH
PCl 5
C O
Cl + POCl
+ HCl
Observation
Inference
Effervescence of CO2
Carboxylic acid
Blue to red
Acidic substance
Carboxylic Acid
white solid
HCl
Carboxylic Acid
O3
+ HCl
Experiment Phenols: 1) FeCl3 test: 0.05g in 5ml water. Add 2 drops in neutral, alc FeCl3 soln. 3ArOH + FeCl3 > Fe(OAr)3 + 3HCl 2) Libermann's Rxn: 0.5g compound+ pinch of NaNO2 in testube, warm, cool+ few drops of conc. H2SO4+ Heat, cool pour into water. Add xs dil. NaOH 3) Phthalein Fusion Test 0.2g + 0.2g phthalic anhyride+ 2-3drops of con. H2so4 in tt. Heat, cool add few drops of NaOH soln.
C6H5-OH + C6H4(CO)2O in H2SO4---> (p-HO-C6H5)2-C-O-C=O
4) Aniline + conc. HCl+ water, cool to 0degC + NaNO2 + 10% NaOH 5) Bromine Water test 0.1g/2drops in H2O+ xs Bromine water drop wise
Observation
Inference
Violet/blue/red/orange/green
Phenol
pink/red/blue/purple/green
Phenol
Bright color Brown colour of bromine is discharged and white solid separates
Phenol
Phenol
Experiment Aldehydes and Ketones 1) Substance + 2,4 DNPH {di-nitro-phenyl hydrazine) reagent, shake
Inference Ald/ket
White solid
Ald/ket
Aldehyde Ketone
4) Tollen's Test: 1ml tollen's reagent+ 0.2g/2-3 drops compound in alcohol. Warm over waterbath. Prepare Tollen's Reagent- AgNO3 + few drops of NaOH. Dissolve brown ppt. by adding NH4OH dropwise
[Ag(NH3)2]+ (aq) + e-Ag(s)+2NH3 (aq) RCHO (aq) + 3 OH-RCOO- + 2 H2O + 2 e
Aldehyde ketone
aldehyde ketone
6)Nitroprusside test: substance in water + alcohol + 1% Sodium Nitroprusside soln. + 10% NaOH (34drops). Acidify with acetic acid 7)Iodoform Test: 0.1g+ 1ml 5% NaOH+ Iodine soln. til colour persists. Shake soln., warm +5% NaOH til colourless
ketone
Alcohols: 1) Sodium Test few drops of compound in dry fusion tube + small piece of Na Metal 2)Esterification: compound+glacial acetic acid+ few drop conc. H2SO4. Heat, pour into water 3)Xanthate Test one pellet KOH+Substance, heat,cool add CS2
ROH + CS2+KOHROCS2K + H2O
Evolution of bubbles/effervescence
Alcohol
fruity odour
Alcohol
Alcohol
4)Substance in water+ Ammonium Vanadate (NH4VO4) 2 drops + 8Green ppt. turn red on shaking. Red color in hydroxyquinoline benzene layer Esters: 1) Hydroxamic Acid Test: 0.1g + 1ml hydroxylamine hydrochloride in alcohol+ 20% NaOH soln. til alkaline. Boil, cool, acidify with HCl + 2-3 drops of FeCl3
Alcohol
Ester
2) Phenolphthalein test: 0.5ml compound + 2ml alcohol+ 2drops of 10% NaOH+ 1-2 drops Phenolphthalein. Boil on water bath. 3) Saponification: 0.5g+ 5ml 20% NaOH in china dish. Boil till ester disappears(15-30min) Cool, acidify with conc. HCl RCOOR' + NaOH ----> R COONa+ + R'OH 4)1ml+0.5g 3,5 dinitrobenzoic acid+ 3-4drops conc. H2SO4. Heat gently for 5 min. Add carefully to 10ml water. Add NaOH till alkaline
Ester
Experiment Halogenated Hydrocarbons 1) Beilstein test: Heat the Cu wire til no green color is imparted to flame. Dip wire in compound and heat in non-luminous flame 2) Alcoholic AgNO3 test 0.2g+ 3ml alcoholic silver nitrate and boil
Observation
Inference
halogenated compound
Pink color discharged No decolorisation Decolorisation of bromine No decolourisation of bromine Pink/red/bluish red Amber/brown/yellow
Halogen attached to side chain Halogen attached to aromatic ring Unsaturated Halogenated Saturated/aromatic halogenated aryl halide alkyl halide
Experiment Anilides: 1)Isocyanide rxn: 0.2g + 3ml alcoholic NaOH soln. + 1ml chloroform. Heat 1 min.
Observation
Inference
2)Hydrolysis 0.5g+ 10ml 20% NaOH, boil 10min. Cool, acidify with conc. HCl Add more conc. HCl, cool to OdegC, add solid NaNO2, betanaphthol in alkali maintaining temp. at 0degC 3)0.1g + 2ml conc. H2SO4. Shake, add K2Cr2O7 powder Nitrocompounds: 1)Reduction 1g compound+0.5g Tin or Zn dust+ 5ml conc. HCl in china dish. Boil, filter, Divide the filtrate to 2 parts a) Filtrate+ CHCl3+ alc.KOH. Heat b)Filtrate at 0degC+cold soln. of NaNO2 and Betanaphthol in alkali No smell of ammonia Bright red dye Bluish pink color Amide absent Anilide Anilide
reduced soln. contains primary amine original compound contains nitro group
2) compound + 3-4ml alcohol+ 5-6drops 10% CaCl2 soln.+Zn dust. Boil, filter. Filtrate + Ammonical AgNO3 (Tollen's reagent) Black ppt. or silver mirror 3)0.1g compound+ FAS (3-4ml of 5% Soln.)+ KOH in methanol til Green Fe(OH)2 is oxidized to brown appt. is obtained. Cork and shake Fe(OH)3 by nitro group 4) Janowsky Reaction: Substance + acetone+ xs 10% NaOH