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Qualitative Analysis PDF
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Test 1 Preliminary examination of substance A. Appearance + Crystalline and hydrated Many salts + Crystalline and wet (deliquescent) Nitrates and chlorides + Crystalline then becomes powdery Sodium sulphate and sodium (effluorescent) carbonate + Liquid All soluble salts and many B. Colour organic substances Possible identification are as follows. Black Oxide/sulphide of Cu’*, Co™, Fe’, Pb**, Mn* Blue Cu’, Co** (anhydrous) Green Cu, Fe**, Ni?* Oran Cr,0> of NH}, or K; Hg0 Pink Co* hydrated Purple-black _ |KMnO, Red Pb,O, Reddish brown | Fe, Hot lead (II) oxide Nite Nat, K*, NHj, Ca’, Zn?+, AP* Yellow Lead ore a RIOD chromate; Iron (III) salt solution; None (colourless) Water, hydrogen perioxide, acids, alkalis, ethanol, methanol and Solutions of Na‘, K*, Mg’, Ca, Ba®, Zn, Pb, ‘Sn’*, NH? ethanal.Chapter 18: Qualitative Analysis Cc. Smell NH, NH} compounds HS __[Sulphides SO, _ [Sulphides Test 2 Solubility characteristics of common ionic solids Add + spatula full of solid under observation to } of a test tube of cold water and shake. Compounds of Group I elements | All soluble Compounds with NH; ion All soluble Nitrates All soluble Hydrogen carbonates Most are soluble Chlorides, bromides or iodides All soluble except those of lead or silver. Those of lead are soluble in hot and not in cold water. All soluble except those of barium and lead. Sulphates Calcium and silver sulphates are slightly soluble. - All insoluble except those of Group I metals and NH,OH. Hydroxides Barium and calcium hydroxides are slightly soluble. Carbonates All insoluble except those of Group I metals and (NH,),CO, : All insoluble except those of Group I metals. CaO reacts Oxides with water to form Ca(OH), which is partly soluble : All insoluble except those of Group I metals, (NG, Sulphides and CaS : oTest 3 Action of heat on a compound Heat a small spatula full of the dry substance in a small dry test tube till no change is ob- served White solid sublimes Ammonium salts Salts with water of crystallization from hydrated salts. Water vapour (H,O) produced Hydrogen carbonate, some sulphate compounds and hydroxide compounds may contain water or produce water vapour. Change in colour: Yellow when hot, white when cold. Zinc (Il) oxide Reddish brown when hot, yellow when cold. | Lead (II) oxide All carbonates except those of Group I metals. Carbon dioxide (CO,) produced Hydrogen carbonates Nitrates, peroxides, few oxides, chlorates or Oxygen (O,) produced B permanganate Ammonia (NH,) produced Some ammonium compounds All nitrates except those of Group I metals and Nitrogen dioxide (NO,) produced NH.NO? P Sulphites except those of Group I metals and Sulphur dioxide (SO,) produced ae ear tes Pp Nitrogen (N,) produced NH,NO, Di-nitrogen oxide (NO) produced NH,NO, Sulphur trioxide (SO,) produced Some sulphates Hydrogen sulphide (H,S) produced Some sulphidesChapter 18: Qualitative Analysis Test 4 Flame test A clean piece of nichrome, or platinum wire mounted on a glass rod handle is required to con- duct this test. 1 2. Put a few drops of concentrated hydrochloric acid in a watch glass. Light a Bunsen bummer and adjust it to give a non-luminous flame. Dip the wire in the acid and then heat it in the flame; repeat this procedure until the wire does not give a colour to the flame. Put the wire into the substance under investigation, so that it is well coated with the substance. Put the coated wire in the flame and note the colour of the flame ‘Compounds of] Observation elements (Colour of flame) | associated with the flame Pale green —_| Barium Brick red Caleium Bluish-green | Copper Bluish Lead Lilac Potassium Brilliant yellow | Sodium Flame red —_| LithiumTest 5 Identification of acidic radicals (anions) Action of dilute HCI Test Observation 1 (a) Add about 3.0 cm? of dilute HCI | Immediate effervescence. to | spatula full of unknown solid in a test tube Odourless, colourless gas produced paper soaked in Pb(NO,) solu- tion into the gas (b) Pass gas into lime water Lime water turns milky ee CO} or HCO; ion! present 2(a) Add about 3. P i = f (a) : out 3.0 cm’ of dilute HCl | No reaction No CO? or HCO, ion to x Spatula full of unknown! present solid in a test tube (b) Heat 2 (a) Colourless gas with choking | Gas is SO, smell produced (© Pass gas into either acidified | Acidified yellow K,Cr,0, | 59% ion present K,Cr,O, solution or paper or | turns green or acidified pur- acidified KMnO, ple KMn0, is decolorized (d) Heat 2 (a) Smell of rotten egg HS produced (e) Put lead acetate paper or filter | Paper turns black S* present Equations for reactions in tests 1 and 2 above: 1a) (b) 2@) (b) CO® (s) + 2H*(aq) > CO, (g) +H,0 0) HCO} (s) + H* (aq) > CO, (g) +H,0 0) Ca(OH), (aq) + CO, (g) > CaCO, (s) + H,0 (1) white No reaction SO* (s) + 2H" (aq) > SO,(8) + H,0 0Chapter 18: Qualitative Analysis (©) @ () K,Cr,0, (aq) + H,SO, (aq) + 380, (g) > Cr,(SO,), + K,SO, (aq) + BLO 0) orange or green colourless 2KMnO, (aq) + 5SO, (g) + 2H,0 (1) > K,SO, (aq) + 2MnSO, (aq) + 2H,SO, (aq) purple colourless S* (s) + 2HCI (aq) — H,S (g) + 2CI (aq) S® (s) + Pb(NO,), (aq) > PbS (s) + NO; (aq) colourless S*(s)+ Pb(CH,COO), (aq) > colourless Action of Concentrated H,SO, black PbS (s) + 2CH,COO- (aq) black colourless colourless paper soaked in Pb(NO,) solu- tion into the gas 3 (a) Add 2.0 cm cold concentrated | No effervescence No reaction HSO, to } spatula full of un- known solid in a test tube (b) Heat 3 (a) gently; do not boil | Effervescence. CO, produced Odourless and colourless gas produced (c) Pass gas into lime water in a test | Lime water turns milky Co? and HCO, ions tube present 4(a) Heat 3 (a) gently; do not boil Choking smell SO, produced (b) Pass gas into either acidified | Orange acidified K,cr,0, SO2- present K,Cr,0, or acidified KMnO, turns green. Purple acidified KMnO, turns colourless (©) Heat 3 (a) gently; do not boil Colourless gas with smell of EE produced rotten egg. (d) Put lead acetate paper or filter | Paper turns black S* presentPut Jspatula of unknown solid and J spatual of copper turnings or copper powder in a test tube, ‘Add 2.0 cm? of concentrated duced Tex Observation Conclusion 5 (a) Heat 3 (a) gently; do not boil. | Colourless, fuming, irritat- | HCl fumes produced Put damp litmus papers in tube | ing gas. Blue litmus paper tums red. (b) Put + spatula full of unknown| Yellow-green gas with Chlorine (C1) solid and } spatula full of MnO, | irritating smell produced | produced into a test tube and add 2.0 cm? of concentrated H,SO, and heat or add MnO, to 5 (a) (©) Suspend damp litmus paper in | Blume litmus paper turns | Cl present 5b) pink and is then bleached (d) Repeat 3 (a) and heat gently. Do | Choking colourless fumes | HBr and Br, not boil. Suspend damp litmus | and choking reddish brown | produced paper in tube | vapour produced. Blue litmus | turns pink (e) Repeat 5 (b) Choking reddish brown va- | Br, produced pour produced | (Suspend damp litmus into 5 (e) | Blue litmus paper turns pink | Br - present and is then bleached 1 @) Repeat 3 (a) and heat gently. Do | Irritating colourless fumes | HI and 1, vapour not boil. Suspend damp litmus | and purple irritating vapour | produced. paper in tube produced. Blue litmus turns | Possibly H,S pink (h) Repeat 5 (b) Irritating purple vapour I, produced produced. | (i) Suspend damp litmus paper into Blue litmus turns pink I present 5(h) 6 (a) Repeat 3 (a) and heat gently. Colourless or pale yellow | HNO, vapour Suspend damp litmus paper in choking fumes. Blue litmus | produced (b) tube turns pink Brown irritating gas pro- | NO, produced into Blue litmus turns pinkChapter 18: Qualitative Analysis Equations for reactions in 3 to 6 in Test 5 Equations in 3 and equations in 4 are the same as equations in J and equations in 2 respectively in Test 5. 5(a) CIs) + H* (aq) > HCI (g) (b) MnO, (s) + 4HCI (aq) — Cl, (g) + MnCl, (aq) + 2H,0 @ (d) Br -(s) + H* (aq) > HBr (g) (e) MnO, (s) + 4HBr (aq) — Br, (g) + MnBr, (aq) + 2H,0 (1) (g) F-(s) + H* (aq) > Hl (g) (h) — MnO, (s) + 4H — I, (g) + Mal, (aq) + 2H,O @ 6a) NO; (s) + H,SO, (aq) —> HNO, (g) +HSO; (aq) (b) 4HINO, (g) + Cu(s) > Cu(NO,), (aq) + 2NO, (g) + 2H,O (0) . If no positive result is arrived at for one gas, test for the next gas. a If all the above anions are absent, then test for sulphate and sulphite respectively. . Prepare a solution of the unknown solid, for further tests for anions and identification of cations. The solution must be dilute because concentrated solutions produce contrary results. Procedure to prepare the solution of the unknown solid ‘Add a small spatula full of the unknown to about 10 cm? of distilled water in a boiling tube. Stir the contents of the tube, or shake the tube well and heat only to boiling point if necessary to dissolve the unknown, but do not boil. If the unknown is insoluble in water, replace the water with dilute HCl to prepare the chloride. If the unknown is insoluble in dilute HCl, replace the HCl with dilute HNO,, to prepare the nitrate1 Test 6 For sulphate from aqueous solution of unknown Alternative confirmatory tests for acidic radicals (anions). (a) Take about 1 0 cm of aqueous solution of unknown in a test tube. Acidify with dilute HC] and add a little BaCl, solution Thick white precipitate deposited. BaSO, formed. SO} present. (b) Take about 1.0 cm’ of aqueous solution of unknown in a test tube. Acidify with dilute HNO, and add a little Ba(NO,), solu: tion Thick white precipitate deposited, which is insoluble in dilute HNO, BaSO, formed. SO} present. (©) Take about 1.0 cm’ of aqueous solution of unknown in a test tube. Add a little Pb(NO,), soltuion and acidify with dilue HNO. White precipitate deposited, which is insoluble in dilute HNO, PbSO, formed. SO? present. From HCI solution of unknown @) Proceed as for (a) above From HNO, solution of unknown © Proceed as for (b) above Equations for reactions in 1(a) and in 1(¢) in Test 6 1(a) or 1(b) le) SO? (aq) + Ba** (aq) — BaSO, (s)L white SO7 (aq) + Pb* (aq) > PbSO, (sd whiteChapter 18: Qualitative Analysis 2. Tests for chloride, bromide and iodide radicals respectively Observation "Test (a) Take about 1.0 cm? of aqueous | Thick whtie precipitate is ‘AgCl formed solution of unknown in a test tube | formed, which turns violet and acidify with dilute HNO, fol- | when exposed to light. lowed by few drops of AgNO, solution. Put about 1.0 cm’ of aqueous so- | Precipitate is formed, which | Presence of Cl- lution of unknown ina test tube. |is soluble in ammonia confirmed Adda few drops of dilute AgNo,, | (NH,OH) solution then excess NH,OH solution. (b) Repeat (a) Pale cream or white precipi- | AgBr formed. tate is formed. The precipi- | Presence of Br tate is slightly solube in am- confirmed monia (NH,OH) solution | (c) Repeat (a) Yellow precipitate is formed. | Agl formed. The precipitate is insoluble | Presence of I” con- in ammonia (NH,OH) solu- | firmed tion Equations for reactions in 2 in Test 6 2(a) Agt (aq) + Cl" (aq) > AgCl (sv white ‘AgCl (s) + 2NH, (aq) > Ag(NH,)2 (aq) + Cl (aq) (b) Ag* (aq) + Br (aq) > AgBr (sv cream AgBr (s) + 2NH, (aq) > Ag(NH,)2 (aq) + Br (aq) () Ag* (aq) + I- (aq) > Agl (sd yellow3. Tests for nitrate radical @) Take about 1.0 cm? of aqueous solution of unknown in a test tube. Add the same volume of freshly made FeSO, solution and carefully pour about 1.0 cm? of concentrated H,SO, down the inside wall of the tilted test tube, without shaking the tube. A brown ring appears where the acid meets the mixture of the solution of the unknown and the FeSO. ),, solution. NO; confirmed (b) Take about 1.0 cm? of aqueous solution of unknown in a test tube. Add 1.0 cm? of NaOH solution and } spatula full of aluminium powder and heat. Suspend damp litmus paper in tube. Pungent smell Pink litmus paper turns blue NH, produced NO; confirmed © Add water to unknown solid ina test tube and shake. Insoluble NO; absent Equations for reactions in 3 in Test 6 3 (a) (b) H,SO, (aq) + NO; (aq) > HSO, (aq) + HNO; (aq) 2HNO, (aq) + 3H,SO, (aq) + 6FeSO, (aq) > 3Fe,(SO,), (aq) + ato () + 2NO (g) FeSO, (aq) + NO (g) > FeSO,.NO (aq) 2Al + 2H,O + 2NaOH > 2NaAlO, + 2H, 2NO; + 8H, — 5H,O + 2NH, +O%Chapter 18: Qualitative Analysis 4. Test for sulphite radical (a) Take about 1.0 cm’ of aqueous | The coloured solution turns Sulphite reduces io- solution of unknown ina test tube | colourless idmie cx bromupeand and add a few drops of iodine or is itself oxidizied by bromine solution them. SO} present (b) OR Take about 1.0 cm? of aqueous|A white precipitate is SO} present solution of unknown ina test tube | formed which dissolves in and add a few drops of BaCl, fol- | dilute HCl lowed by excess dilute HCI (©) OR Take about 1.0 cm? of aqueous|A white precipitate is|SO} present solution of unknown ina test tube | formed which is soluble in and add a little Ba(NO,), followed | dilute HNO, by excess dilute HNO, (@ OR Take about 1.0 em? of aqueous | Purple KMnO, decolour-| SO} present solution of unknown in atest tube | ised. | and addjabout 1.0 cm? of acidified | Orange K,CrO, turns green | SO} present KMn0) or acidified K,Cr,0, (©) @ Takelabout small spatula | Effervescence SO, produced fall of the unknown solid, | Choking smell ‘Add 2.0 cm? of acidified KMn0, or acidified K,Cr,0, and heat. (ii) Suspend a piece of acidified | Orange K,Cr,O, turns green | SO} present K,Cr,0, paper in test tube. Equations for reactions in 4 in Test 6 @) $0?" (aq) + Br, (aq) + H,0 (1) > SOF (aq) + 2HBr (aq) SO? (aq) +1, (aq) + H,0 () > SOF (aq) + 2HI (aq)(b) (©). (@ SO} (aq) + BaCl, (aq) > BaSO, (s) + 2CI- (aq) white SO: (aq) + Ba (NO,), (aq) > BaSO, (s)l +2NO3 (aq) white’ KMn0O, (aq) + SSO, (g) + 2H,0 (1) + K,SO, (aq) + 2MnSO, (aq) + 2H,SO, (aq) K,Cr,0, (aq) + 3SO, (g) +H SO, (aq) — K,SO, (aq) + Cr, (SO,), (aq) + H,O () soy (aq) + 2HCI (aq) + SO. }, (g) + 2Cl (aq) + H,O (1) K,Cr,O, (aq) + 380, (g) +H 2SO, (aq) > K,SO, (aq) + Cr, (SO,), (aq) + H,O (1)Test 7 i Identification of metallic radicals (cations) Action of NaOH solution Test Observation Conclusion 1(@) To about 1.0 cm? of aque- | The solutions are soluble in each | No precipitate formed ous solution of the unknown | other substance in a test tube, gradually add NaOH solu- tion until the contents of the test tube are just alkaline. © (c Heat 1 (a) gently A colourless characteristic smell | Possible smell of NH, Suspend a piece of damp | Pink litmus turns blue. Alkaline | NH, gas produced litmus paper in the test tube | gas. from ammonium salt if in 1 (b) present 2 To about 1.0 cm’ of aque- | (a) A white gelatinous precipi- | Ca* present ous solution of the unknown tate is deposited which is | Ca(OH), formed substance in a test tube, insoluble in excess NaOH é gradually add NaOH soltu- ion until the contents of the |(b) A white gelatinous precipi-| Al*+, Zn?* or Pb? test tube are just alkaline, tate is deposited which is | present then add excess NaOH. soluble in excess NaOH Al(OH), Zn(OH), and Pb(OH), are soluble in excess NaOH (©) Ablue gelatinous precipitate | Cu* present is deposited which is insolu- Cu(OH), formed ble in excess NaOH (d) A dirty green gelatinous pre- | Fe* present cipitate is deposited which is Fe(OH), formed insoluble in excess NaOH (©) A reddish brown gelatinous | Fe* present precipitate is deposited Fe(OH), formed which is insoluble in excess NaOHEquations for reactions 1 and 2 in Test 7 1(6) NaOH (aq) +H; (aq) — Na* (aq) + NH, (g) +H,0 () | 2(a) 2NaOH (aq) + Ca** (aq) Ca(OH), (s)l + 2Nat (aq) (b) i. 3NaOH (aq) + AP* (aq) — AIO), (5) + 3Na*(aq) ii, 2NaOH (aq) + Zn** (aq) + Zn(OH), (s)) + 2Nat (aa) ili, 2NaOH (aq) + Po* (aq) + POH), (sh + 2Na* (aq) (c) 2NaOH (aq) + Cu’* (aq) —> Cu(OH), (s)d + 2Na* (aq) (d) 2NaOH (aq) + Fe* (aq) —> Fe(OH), (s)) + 2Na* (aq) (e) 3NaOH (aq) + Fe** (aq) > Fe(OH), (8) + 3Nat (aq) The hydroxides of Al’*, Zn? and Pb?* are respectively amphoteric because: . They are soluble in and react with excess alkali to form only salt and water and + They are soluble in and react with excess acids to form only salt and water. Equations of reactions of hydroxides and dilute acids on amphoteric substances AI(OH), + NaOH (aq) — NaAloO, (aq) + 2H,0 sodium aluminate AI(OH), (s) + 3HCl(aq) > AICL, (aq) + 3H,0 0) Zn(OH), (s) + 2NaOH (aq) > Na,ZnO, (aq) + 2H,O z sodium zincate Zn(OH), (8) + 2HCl(ag) > ZnCl, (aa) + 2H,0 Pb(OH), (s) + 2NaOH (aq) > Na,PbO, (aq) + 2,0 sodium plumbate Pb(OH), (s) + 2HCI(aq) > PBCh (aq) + 2,0 0lZ al ajeydioaid ou ajeydoaid ay Lvognyos jo ajdues ysay 2 o3(be) {HN ssaaxa ppe wd Aigissod ajeydioaid moyan| isis 0 sal 10 od ‘a7 410 .2N ‘anjossip oju seop Auqssod ‘anjq suiny snuuyy peu hae i ajeydioaid aya sanjossip ayeydoaid "AUOLULE o jauls IUOWUE Jo ows OU doup Aq (be) HORN ssa2xe ppe $$ ray UaY) (be) HORN $s92xe ppe 4 fe 4 j fi 4 unojoo ui Burierpep | att OeN' PHN aje\dioesd umoug-pas ajeydoaid uaei6 ajeyetoand ang Axissod ayeydoaid ou fegeo ajeydoaid ayn AGIXOUGAH WNIGOS SNOANOYV ONISN SNOLLVS ONILOALAGTest 8 Alternative tests for metallic radicals (cations) Action of NH,OH solution ———————— (d) (©) soluble in excess NH,OH to form a deep blue soltuion A dirty green gelatinous precipitate is deposited which is insoluble in excess NH,OH Areddish brown gelatinous precipitate is deposited which is insoluble in excess NH,OH Hest, Observation ‘Put about 1.0cm* of aqueous | (a) A white gelatinous precipi- | Ca’* present and Ca(OH), solution of the unknown tate is deposited which is in- | formed. | substance into a test tube and soluble in excess NH,OH | Al+ may be present and jadd NH,OH dropwise until Al(OH), formed. the contents of the test tube Pb?* may be present and are just alkaline, then add Pb(OH), formed. excess NH,OH (b) A white gelatinous precipi- | Zn?* may be present and tate is deposited which is Zn(OH), formed. soluble in excess NH,OH (c) A blue gelatinous precipi- | Cu* present. tate is deposited which is Cu(OH), formed. Fe** present. Fe(OH), formed. Fe** present. Fe(OH), formed.Chapter 18: Qualitative Analysis Equations for reactions in Test 8 (a) (b) (c) (d) (e) Ca* (aq) + 2NH,OH (aq) —> Ca(OH), (8) + 2NH; (aq) AI* (aq) + 3NH,OH (aq) > Al(OH), (sv + 3NH: (aq) Pb** (aq) + 2NH,OH (aq) > Pb(OH), (s)) + 2NH (aq) Zn** (aq) + 2NH,OH (aq) > Zn(OH), (s\) + 2NH; (aq) But NH,OH (aq) = NH, (g) + H,0 (1) “. Zn(OH), (s)_ + 4NH, (aq) > Zn(NH,)?* (aq) + 20H (aq) white zinc ammonium complex colourless solution Cu* (aq) + 2NH,OH (aq) > Cu(OH), (s+ 2NH; (aq) i Cu(OH), (s) + 4NH, (aq) > Cu(NH,);* (aq) + 20H (aq) white copper ammonium complex deep blue solution Fe** (aq) + 2NH,OH (aq) > Fe(OH), (sb + 2NH; (aq) Fe** (aq) + 3NH,OH (aq) — Fe(OH), (s)l + 3NH} (aq)oid : arendioaid moja uoanjos ajduies ysaye 03 (be) DH PPE Od +O adV0 2d «2 (be) ‘HN ste 0} aunsodxa uo vd uognjos aniq deep ayossip jou se0p [| sseove u agnios sunpep mm anossp Yu anosspp jou nenp ayeydoasd ayy || ajeyctoaid ayy | saop eypydoaid Soop ejeydioeid 0) sanjossip ajeyidioaud ans pue (be) HN, ‘ss20x9 ppe ans pue (be) HN s520x9 ppe ssa2x0 ppe ‘ siniaiialAny San F E 1el¥I0 2d ‘elZ wd Aaissod | aNd SW 2N' THN'280 Aigissod ayejidioasd ayy Aigissod ayeydioaid ueai6| ayendoaid unox-par | Ayqyssod ayeyidioaud nig ajendoaud ou doup Aq dosp (be) ‘HN ppe uowinjog snoanby ut | VINOWAY SNOANOV ONISN SNOILVO ONILOALAGTest 9 S Confirmatory tests for some metallic radicals (cations) To identify Al, Pb, or Zn cations AFTER completion of Test 7 or Test 8 1. Action of H,S Pass HS into about 1.0 cm? of aque- |(a) No precipitate if| Alt absent ous solution of the unknown substance acidified with HCI in a test tube. (b) White precipitate | ZnS formed Zn** present (c) Black precipitate PbS formed Pb** present 2. Other tests to identify Pb cations (a) Add a few drops of dilute H,SO, | White precipitate Pb* present. to about 1.0 cm’ of aqueous solu- PbSO, formed tion of the unknownn substance ina test tube (b) i. Add 1.0 cm? of concen- | White precipitate Pb* probably present trated HCl to about 1.0 cm} of aqueous solution of the unknown substance in a test tube Heat (b) i. Precipitate dissolves _ PbCL, formed Add a few drops of KI solution | Yellow precipi to about 1.0 cm’ of aqueous solu- | _ : _tion of the unknown substance inEquations for reactions 1 and 2 in Test 9 1@) 4H,S(g)+ Al* (aq) > ALS, (aq) + 2H" (aq) no precipitate in acid solution (b) HS (g)+Zn?* (aq) > ZnS (sb + 2H" (aq) white precipitate (c) HS (g)+Pb* (aq) > PbS (sl + 2H* (aq) black precipitate 2(a) H,SO,(aq) + Pb** (aq) — PbSO, (s)) + 2H¢ (aq) white precipitate (b) 2HCI (aq) + Pb** (aq) — PbCl, (sw + 2H* (aq) white precipitate in cold, precipitate soluble on heating (©. 2K (aq) + Pb (aq) Pl, (sb + 2K* (aq) yellow precipitate (@) — K,CrO, (aq) + Pb™ (aq) > PbCrO,(S) = + 2K" (ag) yellow precipitateTest 10 Confirmatory tests for iron salts 1 Action of potassium hexacyanoferrate (III) K,Fe(CN), solution (a) Add a few drops of K,Fe(CN), | Dark blue precipitate Confirms presence of solution to about 1.0 cm’ of aque- | deposited Fe (II) ions, or Fe* ous solution of the unknown sub- stance in a test tube (b) Add a few drops of K,Fe(CN), | Brown solution formed Confirms presence of solution to about 1.0 cm’ of aque- Fe (IID) ions, or Fe** ous solution of the unknown sub- stance in a test tube 2 Action of potassium hexacyanoferrate (II) K Fe(CN), solution (a) Add a few drops of K,Fe(CN),| Very pale (almost white) Confirms presence of solution to about 1.0 cm’ of aque- | precipitate deposited Fe (II) ions, or Fe ous solution of the unknown sub- stance in a test tube (b) Add a few drops of K,Fe(CN), | Dark blue precipitate Confirms presence of solution to about 1.0 cm’ of aque- | deposited Fe (IID) ions, or Fe* ous solution of the unknown sub- stance in a test tube 3 Action of potassium thiocyanate KSCN solution (a) Add a few drops of KSCN solu- | No reaction tion to about 1.0 cm? of aqueous solution of the unknown sub- stance in a test tubeEquations for reactions 1, 2 and 3 in Test 10 1 (a) (b) 2 (a) (b) 3 (a) (b) Fe” (aq) + K,Fe™ (CN), (aq) > KFe® [Fe (CN),] (s) + 2K* (aq) dark blue precipitate Fe** (aq) + K,Fe**(CN), (aq) + Fe* [Fe (CN),] (aq) + 3K* (aq) brown solution Fe’ (aq) + K,Fe**(CN), (aq) > K,Fe* [Fe*(CN),J (s) + 2K*(aq) very pale blue precipitate Fe* (aq) + K,Fe** (CN), (aq) > KFe* [Fe**(CN),] (s)) + 3K* (aq) dark blue precipitate Fe (aq) + KSCN (aq) — No reaction Fe** (aq) + 3KSCN (aq) > Fe(SCN), (aq) + 3K* (aq) blood red solutionTests to identify specific gases or vapours Gas/Vapour | Colour Smell Ligtaacd er Osi Uta Conclusive testis) NH, Colourless |Choking | Extinguishes | Red to blue | Gives thick white c (ammonia) the flame fumes of NH,C! with | concentrated HCL Br, |Reddish | Choking | Extinguishes | Blue tored | White HBr fumes and (bromine) | brown the flame | then brown Br, fumes produced vapour bleached when heated with concentrated H,SO, co Colourless |Odourless |Burns with | None Apply lighted taper to (carbon pale blue burn gas, then add lime- monoxide) flame water, which turns milky | because CO, is produced. CO, Colourless |None | Extinguishes | Blue to pink | Forms white precipitate | (carbon the flame of CaCO, that appears dioxide) | milky with Ca(OH). | Excess of the gas forms | | | soluble Ca(HCO,), Cl, |Greenish |Irritating | Extinguishes | Blue to red | Turns damp starch- (Chlorine) | yellow the flame _| thenbleached | iodide paper blue, because it displaces | iodine A, Colourless | Odourless | Burns with | None Produces water when (hydrogen) a blue flame burnt with lighted taper. that is extin- The water turns guished with anhydrous copper a pop if air is sulphate blue present HCI Colourless | Irritating | Extinguishes | Blue to red | Gives thick white (hydrogen the flame fumes of NH,Cl with chloride) concentrated NH, solution HS Colourless |Of rotten | Burns with | Blue to pale | Turns lead acetate (Hydrogen eggs blue flame, | pink [Pb(CH,COO), Jor sulphide depositing lead nitrate [Pb(NO,),] sulphur paper blackColour Smell 0) eee Sebati __| Lighted taper | Damp! i Purple Irritating | Extinguishes| Blue to red |Turns damp starch pa- (iodine) the flame per or starch solution vapour blue black NO, Brown —_| Irritating | Extinguishes|Blue to red |H,S gas burns in it to |(nitrogen the flame produce NO, H,O and dioxide) | | deposit of sulphur NO Colourless_| Unknown, | Extinguishes | None Becomes reddish brown (nitric oxide because it| the flame NO, on exposure to air or nitrogen is readily or freshly prepared (I) oxide) | oxidized FeSO, solution acidified | to NO, | with dilute H,SO,; turns | dark brown, when gas is | passed through it. |N,O Colourless | Sickly Rekindlesa | None Extinguishes a wooden | di-nitrogen | brightly glow- taper with little glow. | oxide or nitro- ing taper to It is decomposed when | gen(1) oxide, | | produce N, burning magnesium is or laughing | gas, but put into it, to yield ni- gas) extinguishes trogen and MgO a taper with little glow \N, Colourless |Odourless | Extinguishes | None Combines with red-hot (nitrogen) the flame Mg to form nitride, which will react with water when, heated to produce ammonia. So, Colourless [Choking | Extinguishes | Blue to red | Changes colour of acidi- (sulphur smell of | the flame fied K,Cr,0, from dioxide) burning orange to green sulphur (Conclusive test). Removes purple colour of acidified KMnO, White Irritating | Extinguishes | Blue tored | Readily dissolves in fumes the flame concentrated H,SO, to form H,$,0, Crystallizes on cooling to room temperatureH,O (water vapour) Changes the colour of anhydrous CuSO, from white to blue. Changes the colour of anhydrous CoCl, from blue to pink. HNO, (nitric acid) vapour Pale yellow | Choking as it decom- poses. Colourless when pure Taper continues to burn Blue to red Pass vapour into water, add FeSO, solution and concentrated H,SO, dropwise. A brown ring confirms a nitrate from the vapourTests to identify oxidizing agents The following substances can be used to identify oxidizing agents: * hydrogen sulphide (H,S), * concentrated hydrochloric acid (HCl) and * acidified solution of potassium iodide (KI). fe (a) Bubble H,S gas into 1.0 em’ of _| Yellow precipitate of sulphur | H,S is oxidized, an aqueous solution of the deposited The substance is an unknown substance oxidizing agent. (©) i Add 1 cm of concentrated | Choking pale greenish Chlorine gas possibly HCl to 1.0cm? of an yellow fumes produced evolved. aqueous solution of the Hydrochloric acid is unknown substance and oxidized. warm, ii. Suspend damp blueand _| The blue litmus paper turned | Confirm that chlorine pink litmus paper into (b) (i) | pink initially and then gas is produced. bleached. The initial pink —_| The unknown substance litmus is bleached is an oxidizing agent (©) Add 1 cm’ of potassium iodide | Orange brown Aqueous iodine solution to 1.0 cm? of an solution produced produced. aqueous solution of the unknown Potassium iodide is substance and acidify with a few oxidized. drops of dilute sulphuric acid. The unknown substance is an oxidizing agent If any observation is negative, the unknown substance is not an oxidiz- ing agent Equations of some of the above reactions: (a) 2KMn0, (aq) + 3H,S0, (aq) + SH,S (g) > K,SO, (aq) + 2MnSO, (aq) + 8H,0 (1) +55 (6) Purple acid colourless ©) Cr, (aq) + 14HCI (aq) > 2KCI (aq) + 2CrCI, (aq) + 3C1, (g) + 7H,0 () orange concentrated green (©) 2X1 (ag) + H,$0, (aq) + H,0, (ag) > I, (ag) +K,S0, +241,0 + $0,Tests to identify reducing agents The following substances can be used to identify reducing agents: * acidified potassium permanganate (KMn0O,). * acidified potassium dichromate (K,Cr,0,) * chlorine gas (Cl,). (a) Add 1.0 cm’ of an aqueous solu- | The purple solution is de- | Potassium permanga- a tion of the unknown substance | colourized nate is reduced. to 1.0 cm’ of acidified potassium The substance is a re- | permanganate solution ducing agent ©) Add about 1cm® of the unknown | The solution turns green | Potassium dichromate ** substance to 1.0 cm? of acidified solution is reduced. potassium dichromate solution The substance is a re- | ducing agent (c) i. Pass chlorine gas into 1.0/ A colourless and odourless | The gas supports com- cm? solution of unknown | gas is produced. bustion and is oxygen. substance. ii. Put a glowing taper into | Glowing taper bursts into a|The unknown sub- the gas. flame stance is a reducing agent. ** Aways successful If any observation is negative, the unknown substance is not an oxidizing agent Equations of some of the above reactions (a) 2KMnO, +3H,SO, +'5Na,SO, > 2MnSO, + 5Na,SO, + K,SO, + 3H,0 (aq) (aq) (aq): (aq) (aq) (aq) qd) purple colourless (b) K,Cr,0, + 6FeSO, + 7H,S0, > Cr,S0, + K,S0, + 3Fe(S0,), + 7H,O (aq) (aq) (aq) (aq) (aq) (aq) a orange green (c) Cl, (g) + H,O, (aq) — 2HCI (aq) + O,
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