1. Analysis of Zero Group Cation (NH4) Experiment and Procedure Observations Inference Take 0.1 g of the given salt and heat with | A pungent smell of ammonia is| NHj cation may be present, 1-2 mL of conc. NaOH solution. obtained. _| NHj cation is present, | Bring a glass rod dipped in HCI near the | White dense fumes are mouth of the test tube. observed. : = , Presence of NH; ion is Pass the gas through Nessler’s regent. | Brown precipitate is obtained. | oo ag.(Analysis of group-I cations Experiment & Procedure Observations Inference To the original solution prepared in A white precipitate is formed Group I, Pb* may be Water add 1-2 mL. of dil. HCI. present. For Pb* : Dissolve the white precipitate in hot water and divide the solution into three parts: (a) To the first part of the hot solution, | A white ppt. is formed which is soluble [Presence of Pb” is in ammonium acetate solution. confirmed, add few drops of alcohol and dil. H,SO, (0) Potassium chromate test : Add Potassium chromate (K,CrO,) solution ‘0 the second part of the solution. A yellow precipitate is formed which is soluble in hot NaOH solution but insoluble in ammonium acetate solution. This confirms the presence of Pb* ions. () Potassium iodide test : Add KI {polassium iodide) solution to the third Part of the hot solution, ‘A yellow precipitate is formed which is soluble in boiling water and on cooling, shiny crystals are formed. Presence of Pb™ ions is confirmed. Class 12 ®Gi) Analysis of group-II cations . : This group includes Pb** and Cu” in IIA group and As™ in IIB group. These are Precipitated as their sulphides If group 1 is absent, the test for radicals of group Il are carried out. Group reagent for this group is H,S gas, the presence of dil. HCI. Dissolve the black ppt. in hot ammonium acetate solution acidify acetic acid and divide the solution in two parts : (i) Potassium iodide test : To one part, add hot potassium iodide solution. (ii) Potassium chromate test : To another ium chi S.No. Experiment & Procedure Observations Inference 1. [If group 1 is absent, add excess of water | Appearance of black or yellow | It indicates the presence of to the same test tube, shake and warm the | precipitate is observed. group-II cations, solution, pass H,S gas for 1-2 minutes. Black ppt. indicates the presence of Cu or pb ions. Yellow ppt. indicates the presence of As* ions, 2. | Confirmatory tests for Cu* Dissolve the black ppt. in 1-2 mL of 50% HNO), Divide it into 2 parts : (i) toone part, add dil. HSO, and alcohol. | No ppt. is observed. Cu may be present. (ii) Add NH,OH in excess to the rest of Blue coloured solution is | Cu* is confirmed. solution. obtained. Confirmation : (i) Potassium ferrocyanide test : To one | Chocolate brown precipitate | Cu** is confirmed. part of the blue solution add acetic acid | is formed. and potassium ferrocyanide solution. Gi) Potassium iodide test : To another! A white ppt. is formed in| Cu is confirmed. part add acetic acid and potassium | brown coloured solution. iodide solution. 3. | Confirmatory tests for Pb? Yellow ppt. is formed. The ppt. dissolves in boiling water and recrystallises on cooling. Yellow ppt. is formed which laOH solution. Pb** is confirmed. Pb** is confirmed. Lab Manual | ChemisttY4 | For As®* | | Dissolve the precipitate in hot cone, HNO, [a lve into to parts {i) Ammonium molybdate test : To Yellow precipitate is formed | one part of solution add ammonium |. abv ston and het (i) Magnesia mixture test : To the second | White precipitate is formed, [art of the soliton, add NHOH solution and magnesia — minture | containing solution of MSO, NHC | _and NH,OH mixed in equal volumes As is confirmed. As is confirmed.Gi) Analysis of group-III cations (vhite ppt) Experiment & Procedure Observations Inference If group I cations are absent, take about 5 mL of the original solution and add 4-5 drops of cone. nitric acid. Boil the solution for sometime, Add to it about 2g of solid NH,C1 and boil again. Cool the solution under tap water. Add excess of ammonium hydroxide to it and shake. Filter the ppt. obtained and note its colour. Reddish brown precipitate is obtained. White precipitate is obtained. Fe* may be present, AI may be present, 1. Confirmatory tests for Fe* Dissolve the precipitate in dil. HCI and divide into 2 parts : (i) Potassium ferrocyanide test : Add a littleamount of potassium ferroyanide to one part. Potassium thiocyanate test : Add a little amount of potassium thiocyanate to the second part. I. Confirmatory tests for Al* Dissolve the white ppt. in dilute HCI and divide it into two parts : (Lake test : Two drops of blue litmus solu added to one part in the solution. To this add NH,OH dropwise along the sides of the test tube. (ii) Sodium hydroxide test : To the second part add NaOH solution and warm. (i Prussian blue colouration appears. Blood red colouration appears. Blue colour dissolves which floats in the colourless solution, A. gelatinous ppt. is obtained which is soluble in excess of NaOH solution. Fe* is confirmed. AP" is confirmed. AP" is confirmed.>| confirmatory tests for is of group-1V cati Experiment & Procedure F- fif group-lll cations are absent, pass HS gas to the original solution of group-IIl for a few minutes her white, black or buff coloured precipitate appears, Group IV cations Zn", Mn™, Ni?” Co™ may be present, or ne Dissolve the white precipitate in dil. HCL Boil off H,S and divide the solution into two parts (i) Sodium hydroxide test : Add NaOH solution to the first part, (ii) Potassium ferrocyanide test : To the second part, add NH,OH to neutralise it and then add potassium ferrocyanide solution. A white precipitate is obtained which is soluble in excess of NaOH solution. | A bluisl -white ppt. appears Presence of Zn" ions is confirmed. Presence of Zn™ ions is confirmed. Cass 1 Confirmatory tests for Mn () Sodium hydroxide and bromine water test : Dissolve the buff coloured precipitate in dil. HCI by boiling off H,S gas. Add NaOH solution in excess. Now, add bromine water to the white ppt obtained. Lead peroxide test : To black ppt. add conc. HNO, and lead peroxide. Boil, cool and allow to settle. Dissolve the black ppt. in aqua regia. Heat the solution to dryness and cool, Dissolve the residue in water and divide the solution in parts for confirmatory test of Ni" and Co”. Confirmatory tests for N () Dimethyl glyoxime test : Add NH,OH solution to one part of the original solution and then add a few drops of dimethyl glyoxime. Shake the test tube. Sodium hydroxide - bromine water test : To another part, add sodium hydroxide (in excess) and bromine “i ie (i ‘A white precipitate is formed. The white precipitate turns black or brown, | Pink coloured solution is formed. A bright red precipitate is obtained, A black ppt. is formed. water, Bring it to boil. The presence of Mn** ions is confirmed The presence of Mn** ions is confirmed, The red_ precipitate confirmsthe presence | of The presence of Ni?* ions is confirmed5. Confirmatory test for Co” (i) i) Potassium nitrite test : Add NH,OH|A_ yellow coloured complex or | Presence of Co ing solution to the one part and then add | precipitate is obtained. is confirmed. acetic acid and a crystal of potassium nitrite, Ammonium thiocyanate - ether test :|Blue colour in ethereal layer is| Presence of Co ions To another part, add 1 mL ether. Add | formed. is confirmed. a crystal of ammonium thiocyanate, shake it well and allow to settle.Experiment & Pros 1. Ie group-IV cations are absent, then proceed for | detection of fifth group cations. To the original solution, add 2-3 g of solid NH,Cl. Boil and | cool the contents. Now, add excess of NH,OH solution till the smell of ammonia persists, followed by the addition solid (NH,);CO,, 2 | Preserve the small amount of precipitate for flame test. Boil remaining white precipitate with “dilute acetic acid and divide the solution into _ three parts, one each for Ba”, Sr?" and Ca* ions. 3. Confirmatory tests for Ba** |G) Potassium chromate test : Add a few drops @ of potassium chromate solution to the first part (ii) Flame test : Take the preserved precipitate ona platinum wire dipped in cone. HCland heat in the non-Juminous flame of bunsen burner. Observe the colour of the flame produced Cass 12 (uiue colour) | Inference | A white precipitate is| The appearance of white observed, precipitate indicates the | presence of group-V cations. Theinsolublecarbonates of Ba, Sr and Ca dissolves in acetic acid due to the formation of White precipitate dissolves. : soluble acetate. | [ | Ayellow precipitate is | The yellow precipitate obtained. confirms the presence of Ba?” | in the salt. | A grassy green colour of the | flame confirms the presence of Ba® ions, A grassy green flame is obtained.Confirmatory tests for Sr ions Sr ions are tested, if Ba” ions are found to be absent. (i) Ammonium sulphate test : To the second part of the solution add 1 mLof ammonium sulphate solution. Heat and scratch the sides of the test tube with a glass rod and cool. lw Flame test : Perform flame test with the | __ precipitate. A white precipitate is obtained. Acrimson red flame is produced. The white precipitateconfinms the presence of Sr ions, A crimson red flame confirms the presence of Sr" ions, Confirmatory tests for Ca* | Ca®* ions are tested, if Ba** and Sr ions are absent. (i) Ammonium oxalate test : To the third part of the solution, add 1-2 mL of ammonium oxalate solution and shake well. (i) Flame test : Perform flame test with the | precipitate. A white precipitate is obtained, A brick red flame which looks greenish yellow through blue glass, The white precipitate confirms the presence of Ca* ions, Abrick red flame confirms the presence of Ca” ions.(ui) Analysis of group-VI cation = Experiment & Procedure Observations Inference If group-V cations are absent, then proceed for] A white crystalline | The white _ precipitate detection of group-VI cation. Precipitate is formed on the | formed on the inner wall Ammonium phosphate test : Take a part of the | inner walls of the test tube | of test tube indicates the original solution and, add 2-3 g of solid NH,Cl and | which can be scratched | presence of Mg” ions. excess of NH,OH solution. Warm the solution and | with a glass rod. cool it, Now; add solution of disodium hydrogen phosphate till white crust formation takes place in the inner walls of the test tube. Reactions involved For Mg” : Ammonium phosphate test : MgCl, + NH,OH + NajHPO, —> Mg(NH,)PO,! + 2NH,CI+H,O Disodium hydrogen ‘Magnesium’ phosphate ammonium phosphate (White ppt.) Conclusions (The cation present in the salt/salt mixture is (i) The anion present in the salt/salt mixture is Precautions 1. Read the labels on the reagent bottles carefully before using them. Do not use unlabelled reagent. 2. Never mix chemicals and reagent unnecessarily. Never taste any chemical. For smelling any chemical, fan the vapours gently towards your nose. Never put your nose directly above the test tubes or beakers. Wash your hands immediately after touching any salt as it may be corrosive. Do not add sodium metal to water or do not throw it in the sink or dustbin. Never point the test tube towards a person while heating or adding a reagent. Always use the reagents in minimum quantity. Always pour acid into water for dilution. Never add water to acid. Il, SYSTEMATIC ANALYSIS OF ANIONS A. Confirmatory Tests for CO?-, 2", SOF” and NO The confirmatory or wet testis performed with either water extract (original solution) or sodium carbonate extract. en sat is completely soluble in water, the aqueous solution is used for confirmatory test of acid radicals. When salt is insoluble in water, sodium carbonate extract is prepared. : Preparation of sodium carbonate extract : Take 1 g of salt and 3 g of sodium carbonate in a boiling tube. Add 15 mL of distilled water to it. Stir and boil the content for about 10 minutes. Cool, filter and collect the filtrate na test tube and label it as sodium carbonate extract.When the salts are boiled with sodium carbonate extract, the carbonates of metallic radicals are while the sodium salts of corresponding acid radicals being soluble in water pass into the solution. The un, sodium carbonate needs to be destroyed before using the extract. Hence, the extract is ac we and boiled to expel CO: Confirmatory tests for a (a) Confirmatory test for carbonate (CO;*) Precipita ified With som, radicals which react with dilute H,SO, are given below. Indicated by brisk effervescence due to evolution of CO, with dil. H,SO, S.No. | Experiment Procedure Observations Inference 1. [Magnesium | Add MgSO, solution to the| White ppt. is observed. | COF"is confiemeg sulphate test | prepared water extract of the | salt. 2 Lime water test | "Add dil, HCl or dil. H.SO, to| Brisk effervescence with | CO} is confirmed) the salt solution and pass the | evolution of CO, occurs gas evolved through lime water. | which turns lime water milky. atta 1 aigth S.No. 7 inmatory Experiment Sodium nitrepriy solution test Lead acetate test Cadmium carbonate test Silver nitrate test st for sulphides (8) Add NH,OH to Im of water extraet or sodium extract, Shake it well with dil, 1,50, and then add few drops of sodium nitroprusside solution. reedure Add dil. 1,50, to 1 mL of water extract or sodium extract and warm the solution, Add lead acetate solution to the above solution, ‘Toa portion of water extract or sodivimextract,addasuspensi of cadmium rbonate in water and shake well. To a portion of water extract or sodium extract, add 1 to 2. mL of AgNO), Observations Inference S* is confirmed, | A.gas with rotten egg, smell is evolved when H,SO, is added | to salt solution. On addition of sodium — nitroprusside, violet or purple colouration is | obtained. Gas with rotten egg smell is evolved. Black precipitate of PbS is formed which is insoluble in CH;COOH. A yellow ppt. is observe S* is confirmed, ‘A black ppt. is formed which | §® is confirmed | is soluble in HNO, | ee |e ee Lab Manual | Chemist'y(@) Confirmatory test for sulphites (60?) 1 Experiment Procedure Observations Inference | Barium chloride (BaCl,) test Take 1 mL of water extract or sodium extract of salt in a test tube and add BaCl, solution. Further, add dil. HCI to the above solution, A white ppt. is obtained which is soluble in dil. HCI with the evolution of SO, gas. This confirms the presence of SO} ions. Potassium permanganate (KMnO,) test To a portion of water extract or sodium extract add few drops of acidified KMnO, solution, Pink colour of KMnO, is discharged. This confirms the presence of SO} ions. Potassium dichromate (K,Cr,0,) test ‘Add dil. H,SO, to water extract of salt. Then, dip K,Cr,O, paper to this solution. Solution tums green due to the reduction of K,Cr,0, to Cr" ions. This confirms the presence of SO} ions.{@) Confirmatory test for nitrite (NOD Observations | Inferenay S.No. Experiment Procedure 1. Stardriodide Add I mL of KI lution to the salt solution or water Deep blue colour NOS ing fest extract followed by addition of freshly prepared appears. confirmed starch solution and acetic acid to acidity the solution. 2 To a portion of water eviract acidified with acetic Red azo-dye is NOzionw acid add sulphanilic acid and I-napthylamine. obtained. confimed 3. "Add a few drops of dil. acetic acid and few drops | Dark brown or ‘Os ions black ppt. is formed. confirmed. sulphate test__ of FeSO, to a salt solution.r confirmatory Tests for CI, Br“, I", NOg, CHyCOO- and C,07- * Gonfirmatory tests for anions which react with cone, H,50, fa confirmatory test al [g se. [ Bopesimen 7, [Silver nitrate | |(agNOy) test for chloride (Cr) ____ Procedure a 1-2 mL of water extract or sodium carbonate extract of salt and add dil. HNO,, Boil it for some then add AgNO,. me, cool and TA curdy white precipitate [This confirms are given below : Observations [Inference the | solublein NH,OHsolution | presence of co is formed. |fonsin the salt. | 7 [Chromyl chloride (CxO, Cl,) test | (i) Take 0.1 g of salt ina test tube, adda few crystals of K,Cr,O, to it and add 3-4 drops of cone. H,S0,. Heat the reaction mixture. (ii) Pass the vapour through the test tube which contains NaOH solution. (iii) To this above yellow solution, add dilute CH,COOH and lead acetate solution. Red vapours are evolved. [This confirms the | |presence of Cr) lions in the salt. | | | The solution tums yellow. | | Yellow ppt. is formed. | | ‘Manganese dioxide (Mn0,) test Take 0.1 g of salt in a test tube, add a pinch of MnO, and 3-4 drop of conc. H,$0j. Heat the reaction mixture. Bring a moist starch iodide paper near the mouth of test tube. Yellowish-green pungent | Yellowish pungent | gas is liberated which |gas confirms the | tums moist starch iodide | presence of CI paper blue. jions. |(b) Confirmatory test for bromide (Br) S.No. | __ Experiment Procedure Observations ie 1. |Silver nitrate “TFake 12 mLof sodium carbonate | Pale yellow precipitate of | Br ion is ~~ | (AgNO, test catvact or water extract: Add dil. | AgBr partially soluble in | confirmed | HNO, and AgNO; solution and | NH,OH is obtained. I | shake the test tube. / 2 Tfanganese (MnO,) [Heat a small quantity ofthe salt [Yellowish brown vapour Br mon | | dioxide test vith aolid. manganese dioxide | evolved which turns moist | confirmed, | and conc. H,SO,. starch paper yellow. 3. | Carbon disulphide | Add freshly prepared Cl,- water Orange-brown Orange-brown |(CS)or chlorine [and few drops of CS, or CCl | colouration in organic | colouration | water test or chloroform to the aqueous | layer is observed. | confirms the i solution or sodium carbonate peat ie extract neutralised with dil. HCI. ions. Shake it well and allow to stand.(©) Confirmatory test for iodide (I) S.No. | Experiment Procedure Observations Inference 1 Silver nitrate (AgNO, test Take 1 mL of sodium carbonate extract or water extract, acidify it with dil, HNO, and add AgNO; to it, Yellow precipitate is obtained which is insoluble in NH,OH. Appearance of yellow precipitate confirms the presence of iodide ions. Manganese dioxide (MnO,) test Heat a small quantity of the salt with a little manganese dioxide and cone. HS. Evolution of violet vapours which turn starch paper blue. Presence of I ions is confirmed. Chlorine water test Add 1 mL of CHCl, (or CCl) and chlorine water in excess to the aqueous solution (or sodium carbonate extract) and shake the test tube vigorously. Violet colouration in organic layer is observed, Violet colouration the presence Lab Manual | Chemistry(@) Confirmatory test for nitrate (NO3) oo (a) Confirmal | Experiment Procedure Observations | Inference | ‘Ring test | Add 2 mL of cone. H,SO, | A dark Presence of to 1 mL of water extract | brown ring is | NO; ion is and shake well. Cool the | formed at the |confirmed. | test tube under tap water. | junction of Now, add freshly prepared | two solutions. | ferrous sulphate solution | dropwise along the side of the test tube, so that it forms a layer on the top of | the liquid already present in | | FeSO, soluti Dark brown ring Water extract + cone. the test tube. | Fig: Brown ring testig. Confirmatory f ) ——___ Procedure 1g of the given salt | ina china dish, Add 1 mL ethanol and 0.2 mL cone. H,SO, and heat, (wrown ting) Observations Fruity odour is observed. Fruity odour of ethyl acetate indicates the presence of CH;COO ions. Inference Table 1 mL of water extract or sodium carbonate extract of the salt in a test tube and add neutral FeCl; solution to it, (i) To one part, add dil HCI. (ii) To second part, add water and boil. Blood red colouration is obtained. Blood red colour disappears. Reddish brown precipitate is formed. Blood red colour of Fe(CHsCOO), | confirms the presence | of acetate ion. 3. | Oxalic acid [(COOH),] test Take a small quantity of the salt on a watch glass. Mix it with solid oxalic acid. Prepare paste of it with a few drops of water. Rub the paste and smell. Smell like that of vinegar comes out, ‘CH;COO™is confirmed.| Tests for Special Group Acid Radicals : so radicals cannot be detected by cither dil, 1 hese , Uedsome § geod infirmatory tests for sulphate (S03) | Experiment (SO}> and PO;) 250, or cone, HO, F wcitic tests, ‘or detection of these acidic radicals, we Procedure [Inference | Barium Take a part of the water extract of the sal, addl| White ppt. insoluble in SOF is \ chloride a few drops of dil, HCL and then BaCl, solution. | cone, HCI is obtained. | confirmed BaCl,) test | | an equal amount | Violet or purple streaks | SO; is, a drop of water | are produced. | confirmed. alittle of this paste | d matchstick or wooden | | | in the reducing flame of the | bunsen bumer till the whole mass fuses (melts). | _ Dip the fused mass into some ammoniacal sodium | | _nitroprusside solution taken in a china dis | | White ppt. soluble in| SO} is carbonate extract, aciclify with acetic acid, bol] excess of ammonium | confirmed. | off CO, and cool at room temperature. Add lead | acetate solution is, | | acetate solution to the extract. | obtained. Match stick | Mixa small amount of salt with test of solid sodium carbonate. Add | to make a thick paste, Apply Lat the end of a carbonize plinter and heat i 3. Lead acetate [Take a portion of the water extract or sodium test |jy confirmatory test for phosphate (PO}) t eee ent Expel (White ppxy Procedure Ali Observations Inference | molybdate 1 | ‘Ammonium [test Acidify the sodium extract or water extract with conc. HNO; and add ammonium molybdate solution. Heat to boiling. | ‘A canary yellow | Presence of POY Precipitate is obtained. ions is confirmed. 3, | Magnesia mixture test Add magnesia mixture to 12 mL of aqueous salt solution and allow it to stand. (Magnesia mixture is formed by boiling the mixture of NH,Cl and MgCl; solution. Then, adding NH,OH till a strong smell of ammonia is obtained). A white precipitate is obtained. | | Presence of POY | ions is confirmed. |