eS ee Piteagenttet, 0 ae [Organic compound + Benedict's] A. brick red precipitate | roe Fain nn i l) Schiffs reage [Organic compound + Schift's] A pink colour isobtained reagent ‘Test for Ketones (CO-) a) medinitro benzene test ‘group CCOOH) a) Litmus paper p Observation 7 Inference od The carboxylic group is present ion | Briskeffervescenceiis obiained. | The carboxylic groupispresent | [Organic compound + few drops ‘A fruity smells obtained ‘The carboxylic group is present lof alcohol + 2-3 drops of conc. |H.SO, , heat, cool & pour the; mixture into Na,CO, solution VL TEST FOR PRIMARY AMINES (NH,). ) Litmus paper test. A Tat ‘Observation Inference fa compound:hred littius| Redlitmuspaperturns blue _ Primary amineispresent [paper S b) Carbylamine test £ Primary amine is present [Organic compound + CHCl, +] Offensive, / bad smell is alcoholic KOH, heat obtained (aliphatic aromatic) c) Diazotisation or Azo dye test (Test for aromatic primary ami = ae ; Drie cmpoueddsoved in [A edoroinge eis ond | pony anvmatc. amine i ‘coled NaNO, solution + ice present oled solution of B-naphthol in iaOH Ua: ine)| Cerio mmoniumniteiow 2 Lucas reagent test » Neutral FeCl, test . Phthalein dye test Red colour (ay No Layers re formed Layers separate within mint ‘Aldehydes 1. 2,4 DNP 1. Orange yellow ppt. (CHO) 2. Tollen’s reagentiest 2. Silver mirror 3. Febling’s reagent test 3. Brick red ppt, 4. Benedietis/Schiff's reagent | 4 Pink colour test. Ketones 1. ‘m-dinitrobenzene 1. Violetcolour C0.) 2. Soditmnitroprusside test |2. Redcotou, | Carboxylic acid 1° Sodiumbicarbonatetest | 1, Effervescence | (COOH) 2. Esterification test 2. Fruity smelt Amines 1. Carbylamine test 1. Foulsmell (NHL) 2. Diazotisation test 2. Yellow ppt. 43‘equimolar FeSO, & (NH))SO, golution upon eonee SSE ; heat Rita’ FeSO, (NES. +610 > ae Procedure: a L4got FeSO, are trated with 2ml of il 1,80, ina 100ml b areadded into it. é thecrystals of FAS, 3, Thecrystalsare separated by filtration & purified by Result: The yield of FAS = 10.2 Preparation of potash alum ‘Chemicals required : 6.6 g Al,(SO, ), ,2, Procedure: 1. 6.6gAl,(SO, )s and0.5 mL d crystals are added into it, 2. The mixture is heated with constant stirring until K,SO, dissolves completely. 3, The solution is cooléd to get white cryStals of potash alum, The erystals are finaly ssparted by filtration and dried between folds f filter paper. K,SO, + Al($0,), + 24H,0 —> K,S0,.Al(SO,), 24,0 Result : Yield of potash alum = ze 10.3 Preparation of potassium trioxalatoferrate (III) Chemicals required: 3gofoxalicacid, 3.8 g of KOH, 2.5 gof FeCl, Procedure: 1. 3g oxalic acid is dissolved in 15 mL of hot distilled water and 3,8 g KOH are dissolved ina beaker with constantstirring. 2. 2.5 g FeCl, are added into the above solution with constant stirring, The solution is then boiled & cooled to get white crystals of potassium trioxalatoferrate (III). The crystals are separated by filtration and dried between the Reiter heat FeCl, + 6KOH+3H,C,0, “3 K,(Fe(C,0,)]+3KC1+ 61,0 Result : Yield of potassium trioxalatoferrate (III), 4411, PREPARATION OF ORGANIC COMPOUNDS iment No. 1d nett agin acetanilide from aniline, einicals Required: Aniline (5 nL), Acetic nhye : a funnel, RD Mash (1001), benkes AS crt Mnvdtide (5 mL), Glacial ncetie acid (Smt) Ethanol, rrean be propare byheating aniline With acetic anhydride < ) aniline is issolve in Sil acetic anhydride andl 5m. placa acete we 4 dating inaround bottomed flask lt The mixture is reflused on a sand bath for about 15 minites, Anifine giving acetanilide nets he © The reaction mixture is poured into a beaker containing 100/mL of ive w precipitates from the solution as white solid. It is separated by filtration fied by reerystallization from hot water containing little alcohol. Aus Glacial acetic acid NH-CO:CH, C +(CH,CO),o0 —————___ + CHCoon Aniline Acetic anhydride ‘Acetanilide’ Acetic ses Experiment No. 11.2 se Aim:To prepare dibenzal acetone (Dibenzylidine acetone), Apparatus and Chemicals Required : Benzaldchyde (3.2 mL), Ethanol (25 mL), Acetone (23 mL), NaOH solution, Conical flask (250 mL), beaker (250 mL), funnel, Preparation :It can be prepared by the treatment of benzaldchyde with acetone in the Presence of dil NaOH/dil. KOH solution. The reaction is called Claisen- Schmidt reaction CHO dil NaOH CH=CH-CO-CH=CH + GHCOCH, \ "+ 0 + 2HO Benzaldehyde Acetone Dibenzal acetone Procedure: * 3.15 g of NaOHis dissolved in a mixture of 25 mL ethanol and 30 mL distilled water taken in a 250 mL conical flask. Cool the mixture in anice bath, ® Benzaldehyde is mixed with acetone in a beaker, The mixture is then added into a conical flask Containing above NaOH solution with constant shaking forabout 30 minutes. * Benzaldehyde and acetone react giving a yellow solid of dibenzal acetone which is separated by filtration and purified by recrystallisation from Ethyl alcohol, “Se- ee ee ExperimentNo. 113 HLA Aim: Preparation of psnitro acetanilide: Apparatus and Chemicals Required; Acetaitide (x), Clava aeatic aid (2 mL), Cone. HNO\( (100 mL), funnel, glass od, ice bath, hs Preparation sItcan be prepared by the nitration of acetanilide, NHCOCH, E NHCOCH,, Cone. H,SO, + Cone HNO, ——=—+ Acetanilide Procedure: 4+ 2g acetanilide is dissolved in 2 ml glacial acetic acid taken ina Ee added slowly with constant shaking until a clea goluti i obtai cold water bath for some time. a The reaction mixture poured into 100mL ice water taken in a beaker. A yellow solid of p-nitro acetanilide is obtained, Its separated by filtration and purified by recrystallisation from ethyl alcohol, White solidi obtained : Experiment No, 11.4 Ai :To prepare phenyl-azo-B-naphthol (azo dye) Chemicals Required : Aniline (2 mL), concentrated HCI (6.5 mL), Glacial acetic acid (12 mL), Sodium hydroxide (2g),Sodium nitrite (1,6g)and B-naphthol (3.22) Preparation :When aniline is treated with ice cold sodium nitrite ( NaNO,) solution and cone. Hydrochloric acid solution benzene diazonium chloride is formed (Diazotization reaction), which on treatment with alkaline B-naphthol solution gives an orangered dye phenyl-azo--naphthol} NEL Nano, + ConeHCl NEN-Cl 6 caphthol +Dil. NaOH i, “<(sGmmnt a (0-5'C) 5 Aniline Benzene diazonium chloride phenyl-azo-B-naphthol (orange red dye) Aefesse Clan NANO, are dissolved in water in separate beakers and the volution is cooled to O°C vice Similarly -Naphtho is dissolved in 10% dil, NNOH in a beaker. ini ‘The HCL and NaNO, solution are mixed together and aniline is added to it with constant stirring. “Anitinemakes diazotization reaction giving yellow solution of benzene diazonium chloride. fe The solution of alkaline B-naphthol is added into the above solution with constant shaking. An orange red precipitate of phenyl-az0-B-naphtho! is obtained. It is separated from the solution by filtration and purified by recrystallisation from glacial acetic acid, Experiment No. 11.5 Aim:To prepare aniline yellow (p-amino-az0-benzene), Apparatus and Chemicals Required : Aniline (7 mL), Aniline hydrochloride (1.5 g), Glacial acetic acid (7 mL), Carbontetrachloride (9 mL), Diazo aminobenzene (3 g), COnical flask (100 mL), thermometer, funnel, water bath, Preparation :It can be prepared by the reaction of diazo aminobenzene with aniline hydrochloride in presence ofaniline solvent. eB HCL C) non) — C+} rewcrsuin{ > Diazo aminobenzene Benzene diazonium chloride. Aniline oe; NE=N-Cl + Cpe —— Cp} nen{ NH, + HCI Benzene diazonium chloride. Aniline Aniline yellow (P-amino-azo-benzene) Procedure : 3g of diazo aminobenzene is dissolved in 7 mL of aniline in a conical flask. Add 1.5 g powdered aniline hydrochloride into it. The reaction mixture is warmed ona hot water bath for about 1 hour. Remove the flask from hot water bath & allow to stand atroom temperature for30.minutes. Add 9 ml of 1:1 aqueous acetic acid to the above mixture & shake thoroughly to remove excess of aniline. : fed Aniline yellow precipitate is formed which is separated by filtration and purified by Tecrystallisation from CCI, Itis finally dried between the folds of filterpaper. aa12. TESTS FOR CARBOHYDRATES, FATS AND PROTEINS Experiment —; Observation, Inference 1) Molisch test (General test for Carbohydrates) Aqueous solution of the compound + alcoholic solution of c-naphthol + Cone. H,SO, is added carefully along the sides of the test tube A deep violet ring is formed at the junetion of the two layers Carbohydrate is present General test for redueing sugars : 2) Benedict's reagent test : Solution of the compound + Benedict's reagent. The test tube is heated on a water bath. A red precipitate is formed Carbohydrate is redueing sugar 3) Fehling’s solution test : Solution |] ofthe compound + Fehling’s solution A red preci Carbohydrate i$) reducing sugar | | The test tube is heated ona waterbath. 4) Tollen’s reagent test : Solution of| | | the compound + Tollen’s reagent. The [testtubeis heated ona water bath. Ablack precipitate’of silver or a shining silver mirror is obtained Carbohydrate is reducing sugar : Distinguish test between monosaccharide and ccharide | [5) Barfoed’s test : Solution of the compound + Barfoed’s reagent. The test tube is heated on a water bath Orange red precipitate NoOrange red precipitate Carbohydrate is a monosaccharide| Carbohydrate is a disaccharide | Distinguish test between Ketose and Aldose 6) Seliwanoff’s test : Solution of the compound +. Seliwanoff"s reagent The test tube isheated on a water bath, Red colourorpretipitate Blue green colour Nocolourorprecipitate Carbohydrate is Ketohexoses Carbohydrate is ketopentose Carbohydrate is aldose | Test for polysaccharides (starch) 7) Iodine test : Starch Solution + few A blue colour is obtained Starchisconfirmed —~ | | | drops of iodine sotution |B. Test for oils and fats 8) Acrolein test : 3 drops of the oil or melted fat+ few crystals of potassium hydrogen sulphate. The’ mixture is heated gently A pungent smell is obtained acrolein. due to the formation of oil or fatis present C. Test for Proteins 9) Biuret test (For peptide bonds): Protein solution (egg albumin) + 2m of 10% NaOH + few drops of CuSO, solution, warm the mixture. Aviolet colouris obtained Proteinis present 10) Ninhydrin test : Protein solution +Ninhydrin solution, heated & cooled Ablue colour is obtained Protein is present 11) Xanthoproteic test : Protein solution + few drops of conc. HNO, warmed the mixture Yellow colour is obtained which turns to orange red on Protein is present (Test for proteins containing benzene adding NaOH solution ring) 48.YEAR PUC PRACTICAL EXAMINATION VIVA QUESTIONS FOR FUNCTIONAL GROURS IN ORGANIC COMPOUNDS FOR ALCOHOLS , funetic yal group of alcohol ? SerAiehals group) eohols Namea test foralcol Cericammonium nitrate test, Explain Cericammonium nitrate tes agitors When an alcohols shaken with Ceric ammonium nitrate ‘olution, pink or red colour appears Which type of alcohol reacts slowly with Lucas reagent? Primary alcohols. Which type of alcohol reacts instantaneously with Lucas reagent? Tertiary alcohols. name the chemical reagent used to distinguish Primaryaaleohol, segondary alcohol and tertiary alcohol ? Lucas reagent, Whatis Lucas reagent? Amixture ofanhydrous ZnCl, and Cone. HCl called Lucas reagent Whatis the meaning of 2’ alcohol? Thealeohol in which -OH group is, attached to secondary carbon atom, Reaatis the general formula ofprimary algohot? R-CH,-OH Whatis the general formula Ofsecondary alcohol? R-CHR' OH PHENOLS Whats phenolic -OH group? “Ol group whichis directly bonded to Benzene ring. Phenol does not displace CO, from NaHCO, solution (Sodium hydrogen carbonate) Why? Sincephenolislessacidic than carbonic chi Write any to tests for phenols ') Neutral Fertic Chloride test ii) Phthalein dye test Explain Neutral ferric chloride test for phenol 2 When phenol is treated with Neutral ferric chloride, a violet, colouris obtained, Explain phthalein dye test for phenol Phenol is mixed with phthalic anhydride and Cone. HS Poured into a dilute Sodium hydroxide. A. pink coloured: Why pink colouris formed in phthalein dye test? Itis due to formation ofphenolphthalein =a RS emote 49.ee 2,4-DNPhydrazine test Expand 2,4-DNPhydrazine 24-Dinito phenyl hydrazine Name the orange coloured product formed when benzaldehyde is treated with 2, hydrazine, Benzaldehyde 2,4 -DNPhydrazone) WhatisTollen’sreagent? Ammonical silvernitrate solution is called Tollen’s reagent. Explain Tollen’s reagenttest. When analdehydeis heated with Tollen’s reagent, a black ppt, (silver) is formed. Name atest forketones. m-dinitrobenzene test or Sodium: piroieside test, vis let red CARBOXYLIC ACIDS What is the functional group of Caboxylic acids? -COOH (Carboxyl group) Explain litmus test for carboxylic acids. Explain Sodium bicarbonate test for caboxylic acids, When a carboxylic acid is treated with sodium bicarbonate solution, effervescence occurs d tothe liberation of CO, gas. -50-cohol and a few drops of Cone. osodium carbonate solution, fruity, Suerte payee ‘ester formes! when acetic acd is heated with ethyl alcohol in of Cone, COtherthancarboxylicacid which acid ‘Cone. H, SO,. Pi ~ Whatistherleof Cone. H.S0, nesterficaton? ‘ \ ‘Dehydrating agent. ‘Namethe tests forcarboxylic acids, Revie pepertest 2. Sodium bicarbonate test 3. Esterification test AMINES Whatisthe general formulaof", 2" and 3* amines? T'amines:R-NH, 2'amines: R-NH-R" 3'amines: RN-R' 1 ‘Name the confirmatory test forprimary amines. R" Carbylamine test which is answered by both aliphaticand aromatic Primary amines, How do you distinguish between aliphatic and aromatic primary amines ? Byazo-dye test which is answered only by aromatic primary amines, Whichis the functional group ofprimary amines? -NH, (amino group) Which type ofaminesanswerscarbylamine test? All primary amines. What type of odour is observed in carbylamine test? Offensiveorbad odour is observed, Explain azo dye test for primary amine An aromatic primary amine is dissolved in dil HCI and mixed with ice cold sodium nitrite solution, to this -naphthol solution in NaOH is added, ared. dyeis formed. : Explain carbylamine test for primary amines. en a Primary amine is heated with chloroform and alcoholic potash (KOH), a bad emell of carbylamine is obtained. ‘Why bad smell is obtained in carbylamine test? Dueto liberation ofcarbylamine. Whatis alcoholic potash? Asolution of KOH dissolvedin alcohol. _- 's used in esterification test? a pie ae go RY Pr re a es sie‘Titration (Volumetric Analysis) Estimate the Molarity of KMnO, solution ia aiven ase Ce athe pereauzale titration shouldbe siven). ee ot [Seco erresieiriat SZ om re SCHEME OF VALUATION qi Sanais (ova 1) Preliminary tests (any two correct) ii) Detection of Acid radical (4Marks) Group detection (Correct group identification - | mark Comectradicalidentification- 1 Mark) Confirmatory test iii) Detection of Basicradical (4 Marks) Group detection (Correct group identification - I mark Correct radical identification - 1 Mark) 2marks Confirmatory test 2marks For writing systematic procedure with absence: ‘of previous groups 1 mark Qur_ | Titration (10 Marks) 1) Forperforming the experiment 3 marks Forrecording the readings in the tabularcolumn Imark ii) Foraccuracy of the Titre value 3imarks Upto +0.3 mL error 3 marks £0.4mLerror 2marks +£0.5mLerror : Imark £0.6mL& above Omark iii) Calculations of Molarity (2 Marks) a. Formula ; T mark b. Substitution and answer(1 +1) 2marksPourquestions, on functional group in organte con Submission ofthe duly poUNA (2 marks) ‘woeach on any Wo inctional groups (1, 4) Completed and certified record 6 Marks: TOTAL | 30 Marks oof experiments performed and Maximum marks to be SI'No, recorded awarded p— aided ee ell 1 >90% 6 2 81% 10.90% 5 3 71% to 80% 4 4 41% 10.70% 3 2 5 40% 0 | Note: 1)No need to enter scheme of valuation’ and viva Questions given in the Laboratory Manual in the Practical Record, 2)Viva questions are to be asked from the laboratory manual only, 9) The following salts are suggested to be given for analysis for NHL, (AL(SO,),, MgSO, /MgCo,. b) Forviva: Functional group Tests Alcohol Ceric ammonium nitrate test and Lucas ea Phenol Neutral ferric chloride, Phthalein dye test Aldehydes and Ketones ~ DNP and Tollen’s reagent test, Fehling’s reagent test Carboxylic acid Litmus test, sodium bicarbonate test and esterification test Primary amine Carbylamine test, azo dye test (Coupling reaction) lar practical class for practice. ‘o be conducted and recorded. @Smentioned in the II PUC practical manual are t8 9. 10. Potassium chromate (0.2N): Dissolve 9.7 gin 500ml of distilled water. ining oe te Add 170mLot.cone, HClt 800 mL of water wit Nitricacid (2N): Add 128mLofeone, HNO, to $00 mt of water with dilute to | Titre, Sulphuric acid (2N): ; Add 100mLofcone. H,SO, to 800 mlof water carefully and dilute to I litre, Acetic acid (2N): ; Dilute 114mLofGlacial acetic acid to 1 litre of water Sodium hydroxide 2N):_§0,0fNaOHis dissolved in ire of Ammonium Hydroxide 2N): Dilute 133 mLofNH,to1 liteOf water. Ammonium carbonate (2N) me >, 2, v 96 gof Ammonium carbonate is dissolved in liquor ammonia and diluted to 1 litre with water, Barium Chloride(0.5N): Dissolve 30.5g in 500 mL of distilled water. Lead Acetate (0.5N) : Dissolve 47.5¢ of the solid in a mixture of 250 mL water and 10 mL glacial acetic acid and dilute to 500 mL with water. ‘ Preparation of Some Special Reagents 10. Ammonium acetate (2M): Dissolve 154g of the salt in distilled water and dilute to 1 litre, Ammonium chloride (SM) : Dissolves 267.5g of the saltin distilled waterand dilute to L litte, Ammonium molybdate: Dissolve 100 g of the salt in a mixture of 100 mL. of liquor ammonia solution and add 250 g of ammonium nitrate and dilute itto 1 litre with distilled water. Ammonium oxalate (0.5M) ; - Dissolve71 gofthe saltin distilled water and dilute to 1 litre, AmmoniumSulphate (1M): Dissolve 132. ofthe salt in distilled waterand diluteto 1 lire, Bromine Water (approx.saturated) : : Add2mL of bromine in 100 ml of distilled watershake the mixture wel Keepitinadarkbettle, Chlorine water: Prepare chlorine gas by treating solid KMnO, with cone, HCl. Saturate one litre of distilled water with chlorine gas and keep solution ina dark coloured bottle, Dimethyl glyoxime (1): Dissolve 1.0 g ofthe solid in 100 mL of ethyl alcohol, Diphenylamine (0.5%) : i Dissolve 0.5g of the solid in 85 mL of cone. sulphuric acid and dilute it with care with distifled + water to 100 mL : Disodium hydrogen phosphate Na,HPO,12H,0(0.3M): Dissolve 120 g ofthe saltin distilled waterand makeup the volume to | litre, She12 1 MW 15, | 16. | nn. 18. 20. | | | | | | 19. | 21. 10min. and cool it Special Reagents Use in Organic Analysis (FeCL.6H,0) (0.4); Dissolve 90 g of the salt in distilled water containing 10, mL ofcone, HEL and make up the volume tol litre, Todine solution: Dissolve 1 g of iodine crystals in a solution Of 28 potassium iodide in minimum amount of water andailute thesolution to LOO mL, ‘Lime water (Ca(OH), ) (0.02 M) ; Shake 2-3 y of Calcium Hydroxide with | litre distilled ‘water, fill ler the solution after sometime and Keep itn a reagent bottle, Bottle Should be securely Stoppered in orderto protect the Teagent from CO, of atmosphere Nessler’s reagents : Dissolve 23 g of Mercurie iodide and 16 g of Potassium, iodide in distill Volume to 100 mL, Add 150 mL of 4 M NaOH solution, Allow itto stan Solution. Solution should be Stored in dark coloured bottle, Potassium ferrocyanide 0.15 M) : led water and make up the \d for 24 Hrs and decant the Dissolve 46 g of the saltin distilled waterand dilute to I litre. Potassium ferricyanide (0.2 M Dissolve 55 g ofthe salt in distilled water a Potassium iodide (0.5 M) ; | ind diluteto 1 litre, Potassium thiocyanate (0.5 M): Dissolve 49 g ofthe saltin distilled water and dilute to | litre, | Dissolve! g ofthe solidin 100 mL of ethyl alcohol. ve 4 ofthe solid in 100 mL of distilled water. Starch: Prepare apasteofabout 1 miL ofboiling water with constant st 8 of soluble starch ino old water and: ig. Boil it for Pourit to gradually in 100 Alcohol (1 Mixequal volume ofr. Cctified spirit with distilled water, Alcoholic Potassium Hydroxide Solut ion Dissolve 11.2 gofpotassium hydroxide in Alkaline B-naphthol : Dissolve 10 gof B-naphtholin 100:nL of 10% sodium hydroxide solution, Barfoed reagent: 8 copper acetate in 200 mLof 1 % acetic acid, 100 mL ethanol by boiling for 30 mins, Dissolve 13; Benedict’s solution : Dissolve 17.3 g of crystalline copper sulphate in 10 Sodium citrate and 100 g of anhydrous sodium Solutions and make up the volumeto | litre 0 mL of water. Separately dissolve 173 g of carbonate in 800 mL of water. Mix-both the eseaa Disolve69.28,0fCuSO, si it solution B: Dissolve 350g of Rochelle’s saltand . . + Dissolve 69.5 gofdry. be 1, Molisch’s reagent: : Dissolve 10 g of e-naphthol in 90 mL of rectified spirit 12. Ninhydrin reagent: Prepare 0.25% aqueous solution. “13. Schiff’s reagent: ~ 2 Dissolve | g of rosaniline in 50 mL water with gentle 2 aS ‘Cool saturate with sulphur di 2s. Dilute the solution upto | litre with water, Ifpink colour reappears on standing. add few¢ of saturated aqueous solution of SO, with stirring until the colour just disappears. 14. Seliwanoff’s reagent: 3 Dissolve 1 g of resorcinol in 100 mL of 20% HClacid. 15. Sodium hydrochlorite (2M) : Dissolve 100 g of NaOH in 200 mL of water in a large beaker. Cool the solution and add ab 500 g of crushed ice. Weigh the beaker on a rough balance and pass chlorine gas until the ¥ increases by 72 g. Dilute the solution to | litre with water. The solution must be kept in a cool d place. Even then it slowly decomposes. 16. Tollen’s reagent : To 1 mL of 2% solution of silver nitrate add 1 mL of 10% sodium hydroxide till the precipitate appears. Add solution of ammonium hydroxide with stirring till the solution becomes cles Ammonium hydroxide should not be added in excess. (Always use fresh Tollen’s reagent), Amor 56.