6 MES = 3 Authors ~ Subhas Cherigty Systematic Semi micro Qualitative analysis of an inorganic salt, In chemistry, the analysis involves the identification and estimation of the constituents of the given substance. The identification of the constituents of a substance is called qualitative analysis and the estimation of the amount of each constituent is termed as quantitative analysis, A simple inorganic salt consists of an acid radical (anion) and a basic radical] (cation). ‘The analysis involves the following steps: I. Preliminary Tests: (@ State 3 Crystalline solid or Amorphous solid (ii) Colour : White or if it is coloured, mention the colour of the salt. (iii) Solubility test: Solubility of given salt is tested using the following solvents. 1. Water (Cold/Hot) 2. Dilute HCI. II. Analysis of Acid Radials: ° Classification: Group Group Reagent Radicals r Dil. HCI cO- Il Conc.HyS04 Cr, Br NOs UL No reagent 50,2, BO; Analysis of I group acid radical Experiment Observation Inference Salt + Dil. HCL a) Reaction takes place with a brisk effervescence, A colourless and odour-| CO,2~ or HCO” may be less gas is evolved. present. & scanned with OKEN ScannerA Laboratory Manual in Chemistry ~ 11 PUC 2. Test for NOz- radical Salt + Conc.H,SO4 + Cu turnings. Heat until mixture boils b) No effervescence CO, or HCO; are absent. Confirmatory test for CO, and HCO,- radical. Experiment Observation Inference Salt + Dil.HCI Lime water turns milky. | CO,2- or HCO; is Pass the gas through present. Lime water Distinguishing Test between CO, and HCO; radical. Experiment Observation Inference Salt + water. a) Lime water does not CO,?- is confirmed. Boil and pass the gas turn milky. through lime water b) Lime water turns milky. HCO, is confirmed. Analysis of II group acid radical Experiment Observation Inference 1. Salt + Conc.HSO, in | A vigorous reaction takes place a dry test tube. with an effervescence. a) Colourless gas with white] Cl" is present. fumes which produce dense white fumes when a glass rod dipped in NH,OH and held to the mouth of the test tube. b) Reddish brown fumes are evolved. c) No vigorous reaction. a) Brown fumes are evolved b) No brown fumes Br’ is present. Ch & Br-are absent] NO, may be present, NOs. is present. NOs" is absent. & scanned with OKEN ScannerMES - 3 Authors ~ Subhas Chemis, emistry Confirmatory test for Cl-: Experiment Observation Inference 1. Chromyl chloride Test Salt + K,Cr,0; crystals Orange red vapours of in a dry test tube. Add chromyl chloride are conc.H,SO4. (Warm if | liberated. necessary) Pass the orange red —_| Yellow solution is | vapours into NaQH — | obtained. | solution taken in | another test tube. To the yellow solution | A yellow precipitate is | Cl“ is conformed. add dil. acetic acid formed. + lead acetate. | 2. Silver nitrate test | Salt solution + AgNO, | Curdy white precipitate is | CI- is conformed. solution. formed. The precipitate is soluble in excess of | NH,OH solution. Confirmatory test for Br: Experiment Observation Inference 1. Globule test: Salt solution +Excess | Orange (or yellow) globule] Br~ is confirmed. of chlorine water + 2-3) is formed in CCl, layer. drops of CCl, and shake well. 2. Silver nitrate test: Salt solution + AgNO, aa A pale yellow precipitate is] Br is confirmed. formed which is sparingly soluble in excess of NH,OH solution, & scanned with OKEN ScannerA Laboratory Manual in Chemistry - 11 PUC Confirmatory test for NOS: Experiment Observation Inference Brown ring (est: Salt solution + Equal volume of freshly prepared FeSO, solution. Add 223 drops of Cone.HSOq slowly along the inner sides of test tube. A brown ring is formed at the junction of two layers. NO, is confirmed. [Note: Ferrous ammonium sulphate solution may be used instead of sulphate in the above test.] Analysis of III group acid radical Test for SO,* radical: | | | | us Experiment Observation Inference Salt solution + BaCl, solution. To the above white precipitate add excess of dil. HCI. A thick milky white precipitate is obtained. White precipitate is insolu- ble in excess of dil.HCl. 0,27 is present. $0.2" is confirmed. Test for Borate (BO3>) radical Experiment Observation Inference 1. Ethyl Borate test: Salt + Conc.HSO, + Ethyl alcohol. Heat carefully and ignite the vapours. Boron triflouride test: Salt solution + CaF + Cone.HS04. Mix it into paste. Take the paste on a glass rod and keep it in the flame ofa Bunsen burner. The vapours burn with a green edged flame. Green flame is observed. BO,?- is present and | confirmed. BO,*is present and confirmed. & scanned with OKEN Scanner10 MES ~ 3 Authors ~ Subhas Chemiyy ty II. Analysis of basic radicals: Classification: Group Group Reagent Radicals I Dil. HCL Pb 0 Dil. HCL+ HS Cu Mm NH,Clig) + NH,OH Apt Vv NH,Clyg +NH,OH + HS | Zn, Mn+ Vv NH,Clig) + NHyOH + (NH,)5CO} Ba, C2 VI No common group reagent NHyt, Mg, K+, nae [Note: (i) Following basic radicals are given for analysis NH,*, AB*, Zn?*, Mn?*, Ba* cs, ‘Mg?*, K* and Na* (ii) Use strong salt solution (original solution) for basic radical analysis except for NBj* radical. (iti) The test for NH,* radical is done in the beginning and may be shown immediately afer the detection of acid radical. (iv) Use only a few (2-4) drops of original solution or any other reagent for better result in analysis.] Preparation of original solution (OS): If the salt is soluble in water, the original solution is prepated by dissolving the given salt in minimum quantity of water (half test tube). If the salt is insoluble in water, but soluble in dil.HCl, then the original solution is prepared by adding the dil. HCI dropwise until the salt completely dissolved. Then make the volume up to half a test tube by adding distilled water, ENote: Avoid excess of HCI which may otherwise trouble in the analysis of Ht and subsequent group basic radicals, & scanned with OKEN ScannerA Laboratory Manual in Chemistry — 11 PUC Detection of ammonium (NH A *) radical Experiment inference Salt + NaOH solution. Heat and smell the vapours. Expose the glass rod dipped in Dil. HC! to the vapours evolved. Expose a moist red litmus paper to the vapours evolved. (a) A pungent odour of ammonia is sensed. Dense white fumes of ammonium chloride are formed. Red litmus turns to blue. (b) No pungent smell of ammonia. NH," is present. NH,* is present. NH,F is present. NH," is absent. Confirmatory test for NH,* radical Experinient Observation inference Nessler’s reagent test: Salt solution + Nessler’s reagent A brown coloured precipitate is formed. NH,* is confirmed. Analysis of I Group basic radical Experiment Observation inference Original solution + Dil. HCI (a) A white precipitate is formed. (b) No white precipitate I Group basic radicals present (i.e. Pb?* or Ag*) I Group basic radicals are absent. Analysis of II Group basic radical Original solution + Dil. HCl. pass HS gas. (a) A black precipitate is formed. (b) No black precipitate present TI Group basic radicals are absent. [Note: Since, basic radicals belonging to I and II groups are not prescribed in the syllabus, students can directly go to perform the III Group analysis, But absence of I and Il Groups basic radical should be written in the analysis report.) & scanned with OKEN Scanner2 MES - 3 Authors ~ Subhas Choy, ste Analysis of II group basic radical Experiment Observation Inference Original solution + Solid (a) A gelatinous white TI group basic NH,Cl. Dissolve NH,CI precipitate is formed. radicals present completely and add. NH,OH (ie. AB*) solution in excess. (b) No white precipitate. TI group basic radicals are absent, Confirmatory Test for A+ Original solution + NaOH A gelatinous white solution drop wise. precipitate is formed. Add excess of NaOH solution | The white precipitate to dissolve the white dissolves to give a clear precipitate. » | solution. To the clear solution add solid | The white precipitate Al* is confirmed, ammonium chloride and worm.| reappears. Analysis of IV ‘group basic radical Original solution + solid (a) A white coloured Zn?* is present, NH,CI. Dissolve NH,Cl precipitate is formed. completely and add NH,OH | (b) A buff (or pale pink | Mn?* is present. solution in excess. or flesh) coloured Pass HS gas. precipitate is formed, (©) No white or buff IV group basic coloured precipitate is | radicals are absent formed. (Zn or Mn is absent) Confirmatory test for Zn?* 1, Original solution + NaOH | A white precipitate is solution. Drop wise formed. Add excess of NaOH The precipitate dissolves solution to dissolve the to give a clear solution. precipitate. & scanned with OKEN ScannerLeesan ‘A Laboratory Manual in Chemistry - 11 PUC 13 Experiment Observation Inference To the clear solution add acetic acid and pass HS gas. Original solution + K,{Fe(CN)g] solution, Confirmatory Test for Mn?* The white precipitate teappears, Greenish white precipitate which is insoluble in dilHCl. Zn? is, confirmed. Zn is confirmed 1) Original solution + NaOH solution and shake for few minutes. 2 Permanganic test Salt solution (dilute) + Small amount of lead dioxide + Conc.HNO3. Boil the mixture for 3-4 minutes. Cool and dilute with water. A white precipitate is formed which is insoluble in excess of NaOH. The precipitate turns brown slowly when exposed to air. Supernatent layer is pink (or purple) in colour. Mn?* is cor Mn is confirmed. Analysis for V group basic radical Original solution + Solid NH,Cl. Dissolve NH,CL completely. Add NH,OH inl excess + (NH,),CO3 solution. (a) A white precipitate is formed. (b) No white precipitate is formed. V group basic radicals present(Ba>* or Ca?* are present). V group basic radicals are absent. Dissolve the precipitate(a) i Test for Ba?* Divide the clear solution into 2 parts and use each part as in acetic acid to obtain a clear solution, suggested. Part 1 + Potassium chromate solution. A yellow precipitate is formed. Ba?* is present. & scanned with OKEN Scanner| LAboPr 4 " Observation Experiment nit Test for Ca an Part 2 + Ammoniunt oxalate White precipitate is formed} 42+ + MES ~ 8 Authors _ Subp, . hag re vy hy re »* Bae "gt Confirmatory Test for Ba?* and Ca a Preseny Flame Test Prepare a paste of the salt with Cone.HC! in a watch glass. Take the paste on a Platinum wire and bring it in contact with the non luminous bunsen flame. (a) An apple green colour is imparted to the flam (b) A brick red colour is imparted to the flame. Bat 1S presen le. Ca** ig Contin Since no precipitate is obtained in the above V groups, for the VI group basic radical. Analysis of VI group basic radical the analysis is Cattieg ‘Test for Mg?* 1. Original solution + Solid | (a) A white Precipitate is | Mg?* is present ané NH,Cl. Dissolve NH,CI formed. confirmed. completely. Add excess of , : ammonium hydroxide (b) No white precipitate is | Mg2* is absent 7 and ammonium phosphate formed. solution. , | 2. Original solution + N; i : | woken iaOH White Precipitate is formed | Mg?* is confirmed. which is insoluble in >—————___| Xcess of NaOH solution. Test for Kt 1. Original solution + pioys ; ictic | acid, Shake and eg (@) A yellow crystalline | K* i present al atch the us inner sides of the test tube Precipitate is formed. with a glass rod, b) No yellow precipitate is formed. | | confirmed. K* is absent. & scanned with OKEN ScannerA Laboratory Manual in Chemistry — 11 PUC 15 Experiment Observation Inference 2 Flame test Prepare a paste of the salt with Conc.HCl in a watch glass. Take the paste on a Platinum wire and bring it in contact with the bunsen flame, A lilac or violet colour is imparted to the flame. Kt is confirmed. Test for Na* 1 Original solution A white crystalline + Potassium pyroantimonate_precipitateis formed. solution. Shake and scratch the inner sides of the test tube with a glass rod. Flame test Prepare a paste of the salt with Con.HCl in a watch glass. Take the paste on a Platinum wire and bring it in contact with the bunsen flame. A golden yellow colour is imparted to the flame. Nat is present and | confirmed. Nat is confirmed. Report: (a) The given inorganic salt contains Acid radical: ..... (b) Basic radical; Hence, the given salt is .... & scanned with OKEN ScannerL Preliminary tests: (i) State (i) Colour fe + Solid of liquia colour, i) Odour (only: gmmett of vinegar for liquids) Pleasant odour Unpleasant smell, Phenolic or carbolic smell Systematic Qualitative Analysis of Organic Compounds Colourless or if the compound is coloured, mention the Oil of bitter almonds, for solids Odourless, (iv) Ignition test : Take a drop of the liquid (a) It bums with anon or a pinch of the solid smoky flame. On a spatula and ignite it in the flame of a bunsen (b) It burns with a smoky burner, flame. Aliphatic compound, Aromatic compound. Il. Solubility test: 3 to 5 drops of the liquid sample or 100 mg (0.1g) of the with the following solvents and solubility of its compound detect solid sample is shaken ted, Soluble in Soluble in| Soluble in water diLHCl | 5% NaOH Soluble in Insoluble in Conc.HySO, Conc.H,S0, Ethanoicacid | Aniline Phenol Or Or Propanone Benzoic acid Or Salicylic acid Benzaldehyde Trichloromethane / Or Acetophenone Note: Write +? for soluble, “~’ for insoluble and ‘9° Tetrachloromethane for not tested. & scanned with OKEN ScannerIES ~ 3 A; mors ~ Suny oO M Ubhas ¢ oh Conclusion: (i) The compound is soluble in ...... ms (ii) The compound may be (iii) The functional group are. IIL. Test for functional groups: Use 5 crops of liquid or 100 mg of solid sample and 2-3 crm? of reageny te Cth 1] Water soluble compounds — iL Ethanoicacid and propanone Experiment Observation Inference 1. Litmus paper test Organic compound+ Water | (a) Blue litmus tums red. | Ethanoicacié py Add a small piece of blue 7 4 litmus, (b) Blue litmus does Propanone md not turn red. ral 2. Sodium bicarbonate test Organic compound (a) Bffervescence is Ethanoicacid presen, + NaHCO, observed. (b) No effervescence Propanone present. Confirmatory test for Ethanoicacid (acetic acid) Esterification test: Organic compound + Ethyl A fruity smell is sensed. Ethanoicacid alcohol + Cone.H,S0,. Heat confirmed. the mixture carefully. Cool to room temperature and pour the contents into a test tube containing Na,CO, solution, Confirmatory test for Propanon c e (Acetone) 1. Sodium nitroprusside test: Organic compound + NaOH solution + Sodium nitroprusside solution, A red colour is observed. Propanone is confirmed. Lt — & scanned with OKEN Scanner‘A Laboratory Manual in Chemistry =I Puc Experiment 2, 24-DNPH reagent (Borsche’s reagent) test: Organic compound + 2,4 = Dinitro phenyl hydrazine reagent. Shake well, Sodium bisulphite test: Organic compound + Sodium bisulphite solution. Mix well. Todform test: Organic compound + Iodine solution until a pale yellow colour remains. Add NaQH solution. Warm and cool. Observation Yellow crystalline Precipitate is observed. White precipitate is observed. Yellow precipitate is formed with a characteristic smell. Inference | Propanone is confirmed. Propanone is confirmed. Propanone conformed. 2] Dil. Hydrochloric acid soluble compound-Aniline Acetylation: Organic compound + Acetic anhydride. Heat in a water bath for 5 minutes. Pour the contents into a test tube containing cold water. Diazotisation: Dissolve the organic compound in dil./Cl. The mixture is cooled in ice. Add ice cold sodium nitrite (NaNO,) solution. To the above mixture, add cold solution of B-napthol in NaOH A white crystalline precipitate is formed. A red dye is formed. Aniline may be present. Aniline is contirmed. & scanned with OKEN Scanner>. MES - 3 Authors - Subhas Chemistry [Observation inference Experiment 3. Carbylamine test: Organic compound + Chloroform + Alcoholic KOH solution. Warm and pour in to a beaker containing water. Bad or offensive smell Aniline is confirmed, of isocyanide is sensed. luble compounds — [3] 5%-sodium hydroxide sol Salicylic acid) (Phenol, Benzoic acid and 1. Sodium bicarbonate test: Organic compound (a) Effervescence is Benzoic acid or observed. Salicylic acid may + NaHCO, solution be present. (b) No effervescence Phenol present. 2. Neutral ferric chloride test: Organic compound (a) A violet colour in Salicylic acid or + Neutral FeCl, solution. observed. phenol may be present. (b) No violet colour. Benzoic acid present. Confirmatory test for Benzoic acid Esterification test: : Organic compound + Ethyl A fruity smell is sensed. Benzoic acid alcohol + Cone.H)SO,. Heat confirmed. the mixture carefully. Cool to room temperature and pour the contents into a test tube containing NayCO, solution. & scanned with OKEN ScannerAL confirmatory test for Salicylic aboratory Manual in Chemistry — 11 puc [~ Experiment Oil of winter green test: Organic compound + Methyl alcohol + Cone.H,SO,. Heat the mixture carefully. Cool to room temperature and pour the contents into a test tube containing Na,CO, solution. Obser A characteristic smell of oil of winter green is sensed, Salicylic acid confirmed Confirmatory test for Phenol j. Bromination Organic compound + Bromine water 2. Phthalein fusion test: Organic compound + A + Conc.H,SO,. Heat the mixture carefully. Cool to room temperature. Then add excess of NaOH solution. 3, Libermann’s Nitroso test solution + Cone.HySO, ; heat and pour into test tube containing water. pinch of phthalic anhydride Organic compound + NaNO, Orange colour of bromine water is discharged and a white precipitate is obtained. A pink coloured solution is formed. Red coloured solution; turns blue on adding NaOH. ] Phenol is present. | | | Phenol is confirmed. | | | | Phenol is confirmed. & scanned with OKEN Scanner42 4] Cone. Sulphuric acid solul (Benzaldehyde and Acetop: MES - 3 Authors - Subhas Chemistry ble compounds yhenone) ] Observation Inference Experiment 2, 4-DNPH test: Organic compound + 2, 4-DNPH reagent. The mixture is shaken well. With Schiff’s reagent Organic compound + Schiff’s reagent. The mixture is shaken well. Orange yellow crystalline precipitate is formed. (a) A pink colour is formed. (b) No pink colour. Benzaldehyde or Acetophenone is present. Benzaldehyde is present. . Acetophenone may be present. Confirmatory test for Benzaldehy yde: Tollen’s reagent test or silver mirror test Organic compound + Tollen’s reagent. Heat the mixture on a water bath. A black precipitate of silver or a shining silver mirror is formed. Benzaldehyde is confirmed. Confirmatory test for Acetophenone 1. Nitroprusside test: Organic compound + Few drops of sodium nitroprusside| solution + Little NaOH solution. To the above mixture, add acetic acid. Todoform test: Organic compound + Iodine solution until pale yellow colour remains. Add NaOH solution warm and cool. Blue colour is observed. Yellow precipitate of iodoform is formed with a characteristic smell. Acetophenone confirmed. Acetophenone is confirmed. & scanned with OKEN ScannerA Laboratory Manual in Chemistry -l Puc [5] Cone. Sulphuric acid insoluble ¢ Trichlorometh eae hane(chloroform) / Tetrachloromethane(Carbontetrachloride) 1. 43 Experiment Beilstein’s test: A copper wire is heated at the tip of a non-luminous flame until it cease to give any colour. Copper wire is dipped into the organic compound and held at the edge of the bunsen flame. Organic compound + Alcoholic AgNO; solution| warm. Fehling’s test: Organic compound + Fehling’s reagent. Heat in is formed. be chloroform. a water bath for 5 minutes. | (b) No red precipitate. The compound may be carbon tetrachloride. Observation Green or bluish green colour| imparted to the flame. White precipitate is formed. (a) A red precipitate Inference Halogenated compound chloroform or carbon tetrachloride may be present. Aliphatic or side chain halogen compound is present. May be chloroform or carbon tetrachloride. The compound may Confirmatory test for chloroform 1 Carbylamine test: Organic compound + Aniline + Alcoholic KOH solution. warm and pour in toa beaker containing water. Organic compound + Resorcinol is NaOH solution. warm. Bad or offensive smell is sensed. Aqueous layer turns red to green. Chloroform is confirmed. Chloroform is confirmed. & scanned with OKEN Scanner44 Confirmatory test for carbon tetrachloride MES - 3 Authors - Subhas Chemistry Experiment ‘Observation Inference 1. Organic compound ‘Ablue colour is formed. —_ | Carbon tetra chloride + Copper turning is confirmed. + B-napthol + NaOH solution. Heat. 2. Organic compound No colour change. Carbon tetrachloride + Resorcinol solution in is confirmed. NaOH. Heat. Report: 1) 2) 3) ‘The given organic compound is... ‘The molecular formula of the compound is ‘The structural formula of the compound is & scanned with OKEN Scanner