EXPERIMENT - 17 ‘Aim : To identify the functional group in the given organic compound. Apparatus Required : Test tube, test tube stand, test tube holder, dropper, litmus (blue), NaHCOs, cone. H:SO, NHOH. FeCh. Physical Properties: (CHEMISTRY PRACTICALS) Page No 20 State: Solid Colour: White Odour: Vinegar Like Flammability: Burn with non sooty flame (Aliphatic) Preliminary test : S.no._| Experiment [Observation Inference ] 1 Litmus test : Litmus solution tums from | -COOH or- OH maybe Organic compound +2 drops of litmus solution. | blue to red. __present | 2 | Organic compound + NaHICO; sluion | Colouress ores eas | COOH group may be oF - | ith brisk effervescence. phenol group present. | ‘Confirmatory test .no. | Experiment [Observation | Inference 1 | Ester test: | Fruity smell of | ——o Organic compound + | ester i ep C:H,OH + conc. H,SO, + Heat ea oe Mate | confirmed. 2 | FeCl, Test: Organie | Red colour oO appear i solution . - Cc - oH Chemical Reaction: NaHCO, Test : RCOOH + NaHCO, —>RCOONa*CO: 7 +H:0 Easter Test : RCOOH + R— OH —=*—+RCOOR +H,0 RCOONH, + FeCl, —> 4350, (Fruity smell ester) FeCl, Test : RCOOH + NHOH —+ RCOONa RCOONa + H,O — > Ammoniac salt (Soluble) (RCOO), Fe + 3NH.CL (RCOO;)Fe + H;0 —> Fe(OH) (R COO); + RCOOH Basic ferric acetate. ‘The functional group present in the given organic compound is carboxylic acid o 1 “‘\- © - onEXPERIMENT — 18 ‘Aim : To identify the functional group in the given organic compound. Apparatus Required : Test tube, test tube stand, test tube holder, dropper litmus (blue) solution, dil HCl, NaOH, Na metal, dil H2SO,, CHsCOOH. Physical Properties: State: Liquid Colour: Colourless Odour: Spirit Like Water Solubility: Soluble in Water Flammability: Burn with non-sooty flame (Aliphatic) Preliminary test : S.no. | Experiment ‘Observation [Inference 1 Organic compound + blue litmus solution. ‘No change [-COOH or- OH(Phenol) (CHEMISTRY PRACTICALS) Page No 21. ra CERRIC AMMONIUM NITRATE TEST : —OH—+>2RONa+H,% 2ROH + (NH, );CeNO,), —ROH),Ce(NO,), + 2NH NO, (Red Colour) 3 Easter Test: ROH + R COOH —*~+R'COOR + H,0 130, Alcohol acid ester Result : The functional group present in organic compound is alcohol group (-OH) group absent | 2 ‘Organic compound + dil HCl + NaOH ‘No ppt. or oily layer ~ NH; grp. Absent 3 Organic comp +Na metal Hi; gas evolved - OH (alcohol) Group may be Confirmatory test : [S.mo, | Experiment [Observation | Inference 1 Cerric ammonium nitrate | Red colour - OH group. Test | confirmed Organic compound + cerric ‘ammonium nitrate | 2 Ester Test : | Fruity smell of | -OH grp. ‘Organic compound + | ester. confirmed CH,COOH + Cone. H,S0, | |EXPERIMENT - 19 ‘Aim : To identify the functional group in the given organic compound. Apparatus Required : Test tube, test tube stand, test tube holder. dropper litmus (blue) NaHCO, FeCl, Solution, Phthalic anhydride, Con, HSO,, NaOH. Physical Properties: State: Solid Colour: Whit Odour. Phenolic Smell Water Solubility; Water insoluble Flammability: Burn with non-sooty flame (Aromatic) Preliminary test : . . Experiment Observation | Inference ] 1) Organic compound * blue | Blue litmus turn ] litmus solution. Red ‘Organic compound + Phenolic group | NalICO, solution. may be Confirmatory test : Sano. | Experiment 1 FeCh Test Organic compound + FeCl, violet | colouration 2 Phthalic test : [intense green | Phenol (- OH) grp. (CHEMISTRY PRACTICALS) Page No 22 RY 2 NaHCO, test : No effervescence | - COOH absent | | pthalic acid + 2-3 drops H,SO, + A .then cool and iaOH ‘Chemical Reaction : Confirmative test : FeCl, test 3C, HOH + FeCl, —>FAOCH,), + 3HC1 (Ferric peroxide ) CO-Os Coe S e DO Mae Result : The given organic comp. contains phenolic (-OH) grp.EXPERIMENT - 20 Alm : To identify the functional group in present in the given organic compound. Apparatus Required : Test tube, test tube stand, test tube holder, dropper, litmus solution, 2,4 DNP, dil HCl, NaOH, reagent, Fehling solution, Schiff reagent. Physical Properties: State: Liquid Colour Colourless Odour: Pungent ‘Water Solubility: Soluble in Water Flammability: Bum with non-sooty flame (Aliphatic) xper Ob: Infe ‘Organic compound + blue | No change -COOH or | litmus solution, phenolic group absent 2 ‘Organic compound + No pptoroily | - NH; gup. | | NaOH+ dil HCL layer ‘Absent 3 Organic comp +2 ml of 2, | Orange — 4DNP shake & allow itto st Confirmatory test: [Experiment | Observation Inference ‘Schiff's solution test : Pink colour -CHO group present |_Onganie compound + 2 ml of Schiff’ reagent. _| Obtained 2 | Febling’s solution test : Organic compound + | Red ppt. - CHO gyp present. | Fehling's solution (A + B) + boil ina water bath (Chemical reaction : (CHEMISTRY PRACTICALS) Page No 23 1 Preliminary test: ()2.4DNP test: nH, WH-N SCHR No, No, R-CHO+ —_— ©) sa No; No, (2,4 NP) (aldchyde - 2, 4 dil nitro phenyl hydrazone) (Orange ~ red ppt) b) — Confirmatory Test (i) Fehling’s test: Cu(OH), "4 CuO + HO R- CHO+ 2Cu0—>+Cu,0 + R-COOH (Red ppt) + SOH"! —+ RCOO™' + Cu,0 + 3,0 R-CHO + 2Cu* Result : Given organic compound contains aldehydic grp. (- CHO)EXPERIMENT - 21 Aim : To identify the functional group in present in the given organic compound. Apparatus Required : Test tube, test tube stand, test tube holder, dropper, litmus solution, 2,4 DNP, dil HCl, NaOH, sodium, nitro pruside, meta dinitro benzene Physical Properties: State: Liquid Colour: Colourless Odour: Nail paint remover like Water Solubility: Water soluble Flammability: Burn with non-sooty flame (Aliphatic) Preliminary test : _ _ _ S.no. ——Experiment___|__ Observation | _ Inference 1 Organic compound + blue litmus | No change -COOH or solution. phenolic group bsent = NH: gup. Absent 2 | Organic compound + NaOH* dil | No ppt or oily HCI layer 3° | Organic comp +2 ml of 2,4 DNP | Orange ~ red ppt. | - CHO or ketonic shake & allow itto stand. | + group present _ Experiment _____|__ Observation Inference Organic compound + sodium nitro prusside + 2 | Red colour or wine | -CHO group present |= 3 drops of NaOH and shake. red colour 2 | Organic compound +Metadinitrobenzene + | Violet colour which | Ketonie grp confirmed. __ NaOH fades on standing. (i) 2, 4 DNP test A NH,-NH, NH,-N = R R NO, NO, c=0+ ——> H,0+ t R No(Ketone 2, 4 dinitropheny hygyezone) (CHEMISTRY PRACTICALS) Page No 24 b- Confirmatory test : (i) Sodium Nitroprousside Test : oO I CH,- C -CH,+OH''!—+CH,COCH!' +H,0 o o i Il i] [Fe(cn),NOF+cH, C - CH:->| FeCN),NOCH,- C - CH, Result : Given organic compound contains Ketonic group (>C = 0)EXPERIMENT — 22 Aim : To study carbohydrates in pure form of detect its presence in food. Appeartus required : Test tube, test tube stand, test tube holder, burner etc. Theory : Carbohydrates are Polyhydroxy aldehydes or polyhydroxy ketones, their derivatives and the substance which yield them on hydrolysis carbohydrates are classified as sugars and non sugars. Sugars like glucose, fructose and cane sugar are crystalline. Among sugars, glucose, fructose and lactose are reducing while sucrose is non reducing sugar. Test : | Experiment Observation Inference 1 | Cone. H,SO, test: Charring with Carbohydrates present. Sample + burnt sugar Conc. H,SO, + Heat smell. 2 | Molisch test : Reddish purple | Carbohydrates present. Aq. Solution of sample + 2 | ring in formed drops of at the junction + cone. Hy of 2 layers 3 | Fehling solution test : Red ppt Reading Sample solution + | m/ of Sugar persent fehling A + | m/ of Fehling B +A 4 | Tollens reagent : Silver mirror is | Reducing sugar present. Ag, Solution of sample +2 | formed along m/ of Tollens eagent + A the surface of L test tube. fo 5 Red ppt Reducing sugar present Aq solution of sample + reagent + H Sample Solution + few drops of iodine solution Result : Carbohydrates is present.EXPERIMENT — 24 Aim : To study proteins from sample and detect their presence in food sample. Apparatus required : Test tube stand, test tube holder, glass rod, bumer etc. Theory : Proteins are high molecular mass, long chain polymers composed of a amino acid. Amino acids are molecule that have both -NH; and -COOH group. _ Test: S.no. Experiment Observation Inference 1 Biuret test: Sample + NaOH + | Bluish violet colour —_ Protein is present | Dil CuSO, solution appears | 2 Xanthoprotein test : ‘Yellow ppt. Protein is present Sample + few drops of | | conc.HNO; +A | | 3. Million’s test : White ppt Protein is present | Sample + 2 drops of millions which changes to reagent + A brick red on boiling | 4. Ninhydrin test : Blue colour appear —_| Protein is present Protein sample + Few drops of | ninhydrin solution + Boil the | contents for | minute Result : Protein is present.EXPERIMENT 1.1 AIM: To prepare colloidal solution (sol) of starch. APPARATUS Beakers (250 ml and 50 ml), glass rod, funnel, filter-paper, pestle and mortar, tripod stand, wire-gauze and burner. MATERIALS REQUIRED Soluble starch (500 mg) and distilled water. PROCEDURE 1. Take 500 mg of starch in a mortar and add few ml of distilled water. 2. Grind the starch to make a thin paste and transfer this paste to a 50 ml beaker. 3. Take about 100 ml of distilled water in a 250 ml beaker and heat the beaker so that water starts ame boiling. Y Tivos 4. Pour the paste slowly with stirring into boiling —~“stand water in the beaker (Fig. 1.1). 5. Continue boiling for about 10 minutes and then allow the beaker to cool. 6. Filter the contents of the beaker through a filter- paper, fixed in a funnel. Label the filtrate as ‘Starch Sol’. Fig. 1.1. Preparation of starch so PRECAUTIONS 1. The apparatus used for preparing sol should be properly cleaned. . Distilled water should be used for preparing sol in water. . Starch should be converted into a fine paste before adding to boiling water. Starch paste should be added in a thin stream to boiling water. . Constant stirring of the content is necessary during the preparation of the sol. AEDEXPERIMENT AIM: To prepare ferric hydroxide, [Fe(OH). );] sol. APPARATUS Conical flask (250 ml), beaker (250 ml), a boiling-tube, glass- rod, funnel, round-bottom flask, iron stand with a clamp, wire-gauze, tripod-stand, burner and a burette or a dropper.MATERIALS REQUIRED 2% solution of ferric chloride (prepared by dissolving 2 g of pure FeCl, in 100 ml distilled water) and distilled water. PROCEDURE 1, Take a 250 ml conical flask and clean it by steaming-out process as shown in Fig. 1.2. 2. Tothis cleaned flask, add 100 ml of distilled water and heat it to boil by placing the flask on a wire-gauze. 8, Add ferric chloride solution dropwise (by the use of a burette or a dropper) to the boiling water. 4, Continue heating until deep red or brown solution of ferric hydroxide is obtained. Replace the water lost by evaporation during boiling at regular intervals. 5. Keep the contents of conical flask undisturbed for sometime at room temperature, Label the solution as “ferric hydroxide sol”. Steam Vessel to be cleaned Glass tube Distilled water Wire gauze Fig. 1.2. Steaming-out process for cleaning conical flask. PRECAUTIONS 1. Sinee ferric hydroxide sol is affected by impurities, the apparatus required for the preparation of sol should be thoroughly cleaned by steaming-out process. 2. Add ferric chloride solution dropwise. 8. Heating is continued till the desired sol is obtained. 4. Hydrochloric acid formed as a result of hydrolysis of ferric cl wise it would destablise the sol. shloride is removed by dialysis process other-[exeenmemeer AIM: To separate the coloured components present in the mixture of red and blue inks by ascending paper chromatography and find their R, values. APPARATUS, Gas jar, glass rod, filter paper strip (Whatman No. 1 filter paper), jar cover and a fine capillary tube. REQUIREMENT ‘A mixture of red and blue inks, alcohol and distilled water. PROCEDURE 1. Take a Whatman No. 1 filter paper strip (20 x 2 cm) and draw a line with pencil above 4 cm from one end Draw another line lengthwise from the centre of the paper as shown in Fig. 5.1. Chromatographic Solvent front Separated I spots of _Cromatagraphi different paper constituents paper Glass rod to hang paper Original tine about 4.0m above the edge Jar Original spot ofthe i F Pure mare — solvent Point to put the Spot of the mixture, Fig. S.1. Spotting of the mixture.4, Cover the jar and keep it undisturbed. Notice the rising sol inks. After the solvent has risen about 15 cm you will notice the filter paper. 5. Take the filter paper out of the jar and mark the pencil. This is called the solvent front. vent along with the mixture of red and blue two different spots of blue and red colours on distance that the solvent has risen on the paper with a 6. Dry the paper. Put pencil marks in the centre of the blue and red spots. 7, Measure the distance of the two spots from the original line and the di original line. 8, Caleulate the R, values of the blue and red inks by using the formula : yz, < Distance travelled by the blue or red ink from the point of application Soe ee eer eee ee ee man tera aoe Distance travelled by the solvent from the original line istance of the solvent from the Chromatographic paper Solvent front > Spots of different constituents _- Original spot of the mixture Fig. 5.3. Calculation of Rvalues. OBSERVATIONS AND CALCU! LATIONS: ‘Substance Distance travelled Distance travelled R, Value by different components by solvent Red ink + Blue ink ‘Acm (Red ink) Xem AK Bem Blue ink) Xem BK PRECAUTIONS i vent in 1. Use good quality pencil for drawing the reference line so that the mark does not dissolve in the solvent 1 which the chromatography is carried out. ‘Always make use of a fine capillary tube. ‘A spot should be small and rich in mixture: Keep the strip erect. Do not let it to be curled. ’ Do not allow the spot to dip in the solvent. noap er Keep the jar undisturbed and covered during the experiment. ‘Allow the spot to dry before putting the strip in the jar.EXPERIMENT 6: AIM: To prepare a pure sample of potash alum (Fitkari), [K,SO,,Al,(SO,).24H,O]. THEORY Potash alum is prepared by dissolving an equimolar mixture of hydrated aluminium sulphate and potassium sulphate a little of sulphuric acid and then subjecting the resulting solution to in minimum amount of water containing f potash alum separate out. crystallisation, when octahedral crystals o! K,80, + Al,(SO,),.18H,0 + 6H,0— K,S0,.Al,(SO,),.24H,0. Potassium Aluminium Potash alum sulphate sulphate 174 666 Molecular masses : REQUIREMENTS Two beakers (250 ml), china dish, funnel, funnel stand, glass rod, wash-bottle, tripod stand and wire-gauze. Potassium sulphate, aluminium sulphate and dil. sulphuric acid.a. i crystals to it. Add 1. Take a 250 ml beaker. Wash it with water and then transfer 2.58 potassium sulphate crys " ghout 20'ml of water. Sra dissolve the crystals. Warm ifrequired, a tata ag 2, Take the other 250 ml beaker, wash it with water and then transfer 10 g aluminium sti Ti SS " Gt. Add about 20 ml of water and 1 ml of dilute sulphuric acid to prevent hy phate. Heat for about 5 minutes. If milkiness still persists, filter the sainkion. eo 8, Mix the two solutions in a china-dish and place the china-dish on a wire-gauze placed over © Burtier Soir the solution with a glass-rod. Concentrate the solution till the crystallisation poini dish over a beaker containing cold water. : 4. Soon the crystals of potash alum separate out. Decant off the mother liquor and wash the crystals with a small quantity of ice-cold water. , ous plate 5. Dry the crystals by placing them between filter paper pads or by spreading them over porous plate. OBSERVATIONS Weight of crystals obtained Colour of the crystals Shape of the crystals Note. The crystals of potash alum are octahedral in shape. Table 6.1. Shapes of crystals of some common substances ‘Substance Geometry or shape of crystal 1. Blue vitriol, CuSO,.5H,0 Triclinic 2. Green vitriol, FeSO,.7H,O Monoclinic 3. Potassium nitrate, KNO, Rhombic (Needle-like) 4. Potash alum, K,SO,, Al,(SO,),.24H,0 Octahedral 5. Sodium chloride, NaCl Cubic 6. Washing soda, Na,CO,.10H,0 Monoclinic PRECAUTIONS 1. Cool the solution slowly to get good crystals. 2. Do not disturb the solution while it is being cooled.The complex potassium trioxalatoferrate (IID) can be prepared by dissolving freshly prepared ferric hydroxide in 4 solution of potassium oxalate and oxalic acid. FeCl, +3KOH —, Fe(OH), + 3KCI 162.7 107 goon 2Fe(OH), +3 - 2H,0-—., Fe, 0), +1 O on 2 (C,0,), + 128, 2x 107 S126 376COOK Fe 0, 3 'e,(C,0,) + gpg. B#O > KatFeC,0 al -H,0 316 3x 184 2491 REQUIREMENTS ‘Three beakers (250 ml), china dish, funnel, funnel stand, glass rod, wash-bottle, tripod stand and wire-gauze. Ferric chloride, oxalic acid hydrated, potassium oxalate and potassium hydroxide. PROCEDURE 1 2, 8. 9. Dissolve 3.5 g of anhydrous ferric chloride 50 ml of distilled water in a 250 ml beaker. . In another beaker dissolve 4 g of potassium hydroxide in 50 ml of water. 3. Add KOH solution to FeCl, solution in small portions with constant stirring. Filter the precipitates of ferric hydroxide so formed through a buchner funnel. Wash the ppt. with distilled water. In another beaker (250 ml) take 4 g of hydrated oxalic acid and 5.5 g of hydrated potassium oxalate. Add about 100 ml of water and stir thoroughly to get a clear solution. ‘Add the freshly prepared Fe(OH), ppt. in small amounts to the above solution with constant stirring. The ppt. get dissolved. If ppt. does not dissolve then warm it and leave the contents for sometime. Filter and transfer the filtrate to china dish and heat on a wire-gauze to the crystallisation point. |. Now place the china dish on a beaker full of cold water and keep it aside for crystallisation. China dish should be covered with a black paper as the complex is sensitive to light. Decant off the mother liquor, wash the crystals with a small amount of ethyl alcohol and dry them between the folds of filter paper. Find out the weight of the crystals. OBSERVATIONS Weight of the crystals obtained = Colour of the crystals is PRECAUTIONS 1. Do not concentrate the solution too much. 2. Let the concentrated solution cool slowly and undisturbed to get large crystals.