Semimicro Qualitative Analysis: fe} V) Analysi , 7 7 inant a Groups: The precipitate formed should be washed with water first and then it is oI Saar taeeactiae solvent. A group may contain many radicals. Depending upon the nature of the eee riGkohon an be identified, Centrifugate or solution is boiled in a 10 ‘or beaker to boil off excess of NH, H,S etc. In the process, solution gets concentrated due to boiling and fused for detection of radicals, process, solution gets concent B VI) Wet Tes i ; 7 sD i ete Actually, wet test for anions should be done before the original solution frst prepared, because sme ofthe anions inrferin the separation of groups and analysis. But wie eporting should be reported atthe end ‘or wet tests of anions, either water extract or neutral solution is used depending upon solubility of anions, When anions from the same group are pres then special tests called the complexities tests are followed as in presence of each other. Simple test does not give any idea. ‘Thus, when all the above steps are followed carefully with understanding, analysis of mixture becomes easy and one can analyse the given mixture correctly. SEMI-MICRO QUALITATIVE ANALYSIS (1) Preliminary Tests Preliminary tests of a mixture include the examination of the mixture under following headings: (A) Nature (B) Colour. (A) Nature The given mixture should be carefully examined to see, whether itis crystalline or amorphous. On if the mixture is found to be gritty, itis generally crystalline but 1ous, This test cannot always be reliable as finely Iso helps us to find out the rubbing the mixture between two fingers, if itis found to be soft and fluffy, it is mostly amorph powdered crystalline substance can be made soft to the touch. Solubility test al: nature of the substance. (B) Colour This is an outstanding feature in the preliminary tests of salts. colour in solid and in soluble state, hence can easily be spotted out. Some of the ions have characteristic Tests Observations Inferences (A) Nature (Crystalline 02°, NOx, Cl, Br, F of soluble sats oF CO} of alkali salts presents. (i) Amorphous _, C0}, PO},S** of heavy metal salts present. (B) Colour (i) Pink Co**, Mn** salts present, (i) Green CuP+, Fe’, Cr+, Ni? salts present, (iii) Blue Hydrated Cu?* salt present (iv) Black ‘CuO, CuS, PbS, MnO, salts present. () Yellow PbO, Pbl; salts present. (vi) White Coloured salts are absent Scanned with CamScannera College Practical Chemistry (EY. B.Sc.) (2) Dry Tests for Cations : (D Heating of the mixture in a dry test tube Tests Observations Inferences Heat about 0.1 ¢ of the mixture in a dry test tube held almost horizontal on the Dumer flame. (® Substance fuses Salts of Na’, K*, NH or some salts of Cas, Bas, Si , Mg?* of hydrated salts etc (0 Decrepitation (crackling sound is produced due to the breaking of the crystals and particles flying off) Salts like NaCl, KC, KNO,, KI, Pb(NO)), te. (iii) Defagration (powder catches fire and bums with sparks) Some NO} salts etc. (is) Evolution of gases (@) Coloureless gas, smells of NHs, tus moist red litmus blue NH} salts. (®) Colourless gas turns freshly prepared lime water milky (©) Dark brown or reddish fumes, acidic in reaction CO} salts etc. Nitrates or nitrites of heavy metals e.g. PB(NO,)», Cu(NO,), ete. @ Violet vapours tum starch paper blue odides salts etc. (©) Red brown vapours turn starch paper yellow Bromides salts etc. Greenish yellow gas, smell of chloride, bleaches moist litmus Paper Chlorides salts ete. (g)_ Burning sulphur smell S03" present. () Sublimation (substance gives out vapour which condenses on cooler part of the test tube) (@) Greyish or Black F-salts ete, ® wi + NH salts etc. © Yellow S® salts Scanned with CamScannerSemimic cro Qualitative Analysis 2 Tests Observations Inferences (i) Change in colour of residue colour when salt | col cect] ie een heating (@ Yellow White Zn? salts ete () Orange or on Yellow Bi, Ph? salts ete. (© Black Rusty red or Fe,0, (ferric salt) brown @_ Black Black Oxides of coloured radicals e.g. MnO,, CuO, C00, NiO etc. © Violet Blue Co salts. () Yellow Yellow PbO or Pb salts. (g) White White Ca, Ba®*, Sr2*, Mg?*, AP*, K* salts etc. (hi) Blackening not accompanied by buming | Cus Mn, Ni salts ete. or odour Heating of the mixture in a charcoal cavity Tests Observations Inferences the anhydrous quantity reducing flame. Mix 0.01 g of the mixture with double (solid) Na,CO, and fill in a cavity of charcoal. Add 2 drops of water in it. Heat the cavity with a blow pipe in a (@ Fusion and sinking in the cavity Nat, K*, NH} salts or erystallines salts etc. “or | (ii). Decrepitation ie, crackling sound and NaCl, KNO,, KCl, Pb(NO,), ete flying about of particles (iii) Deflagration with the sparks and Some Cr+, NOj salts ete. residue turns green Gop Fumes and incrustation (the fumes evolved get deposited on the cooler NH and Ir salts ete. sides round about the cavity) (v) Metal beads formed (a) Rusty red Fe,0, } Yellow incrustation with brite | i, Pb? sls et. bead (© Malleable bead that marks the Pb? salts etc. paper black Scanned with CamScannerCollege Practical Chemistry (FY. B.S¢.) Tests Observations Inferences (©) Yellow matteable bead that does | Sn? salts ete _ ‘not mark paper black | (©) Red flakes Cut salts ete. | (O Grey metallic particles without Fe)*, Co®, Nid* salts ete. inenustation —~ (8) White infusible mass ADs, Zn, Mg, Ba?*, Cal*, Sr etc, 2 SReFCu09, test 5 This test is per- | (i) Blue mass AB+, PO,*salts etc. formed only when the residue in charcoal | cavity test remains | (ii) Green mass Zn** salts etc. | white. Add one drop of 5% Co(NO,), | (ii) Pale pink or indistinct mass Mg, Ba, Sr2*, Ca* salts etc. | solution and heat the | residue in an | oxidising flame. | = (IV) Flame test Tests Observations Inferences Moisten 0.01 g ofthe | Without cobalt | Through cobal mixture with 2-3 | glass glass drops of conc. HClon a clean watch glass | (i) Lilliacor violet | Crimson Kr and prepare a paste of it. Take it on a clean | (ii) Apple green Bluish green Ba** platinum wire and heat in an oxidising | (iii) Brick red Light green Cc: flame. (iv) Crimson Purple srt Observe the colour of (carmine red) the flame with naked eye and through } (») Bluish green | Blue cu cobalt glass. (vi) Bluish white |, White Bi**, Pb, Sn? etc. [Platinum wire is cleaned by dipping it in conc. HCI and heating on strong flame, till blue colour of flame remains L unchanged]. Scanned with CamScannerSemimicro Qualitative Anal lysis 65 fporax bead tes wo itis performed when Oxidising Name i Ss Fixture contains Reducing flame coloured salts. [A Hot Cold Tat savedngug [sooo ut agnor ovdpaaa | OVP Safa pa OOTY HOPN ND J0 HD "97 HO EE DPE -UONTOS 3, " . -quasaad oq Kew [PUA Thoth dno op ROUPEH ssoqinoyoo | vornjos 31 (Z) ww2sex! aq Kewl ye JOPPUE 4200 ‘42ND WOM “ald ¢ 0} aunjos 249 29np21 01 KYSER I Hog ZIEAMINAD *SO pyendpaad Taguany posood warp sag) eyedpoud ou J af syozmdas puw ayeyBaxd ov OBNYLALID acapexre &tpounsyp s9s0009 2! [3 "BONN}OS HO'HN 1N9 UAH pure LOHIN|OS [O" HN WTJ® eld2 1 PPE “worraos 210K 943 OL, SouopmUT wow s¢ Fog “wom ‘tHs0) owCypoxd OF JT -g9 “ox @fod wo wants ev amoyps aveydoya sontog “Fuafionm st Ya vou ‘eusoy spmtdtooud Om IT "HN J0 7 119 + uornyos op Jo sdoup eZ “31 e3 wornyos HO'HN TT PPY Y! 96]055Ip 0) ANS — ‘yuosoud oa worn ‘su peoand ma AreH> I “4. womans “oop CHEN) 259 J0 gO T PPV “109 FONE 2409 Jo «1D T + HoRNIOS atp Jo soup o~ Od 203 9L, uasqe 4224 Uaty ‘arendtoaxd 10 sno]0D an] OU HL SHE «24 & 4324 28PIX0 04 104 PLE ING 2FOWN 241.01 SONH "2409 J0 42 | PPY roaud 3 snoj0o anyg & vorinjos %(ND) 24°H JO 956 J0 Sdoup Z + ‘BL ON 288d “ariS Pure #280“ J0L-D 304 SS 30} SL °S0N aed 01 29504 ania ~*OS'S aunt = 70st aMuAa\ ~ "Osta. rupsaid dnos8 areyding sey sanedaganeag 20°50 os" 0S"H N30 ainnp ppe uayt ‘sis suzosd omy 509 01984 put "STH Nb 201TH JO sp zppe Lot or am jo rao nulad pare OG "¥ING B}OUN OUT Scanned with CamScanner “apd 30 LMS, 305 9L BELSON ABEd OnD}>y -wuasand 420d Spy 30S yendnoad ‘Smoyoy Se soUpny pasooad uo ‘suo ayetdiaxd OU 5 paresedas Jo doa snoraaid ap ut paurexqo a4 auengnuag amp 957) (S"H Baysn ynoynaa) sdnory oyu suopes Jo uoHeaedag TON o1q8, Sytaua> “qwasaxd st | dnosp uorp ‘suI09 averdisaud & HH IH N #50 eD JO- (1) :2I0N"Semimicro Qualitative Analysis a Phosphate Scheme Acidify the whole solution with 1-2 cm} of 4N HNO, and boil. Add 0.5 g of NH,CI and 10% Zx0(NO3)x, Zirconium nitrate solution, dropwise to precipitate PO,*. Add sightly excess of ZrO(NO3)> solution and centrifuge. Reject the precipitate of ZrO(HPO,). Centrifugate is used for further separation, IIL. Separation and Detection of Cations from the Groups Analysis of Group I (Silver Group): The precipitate is washed with 0.5 cm? of 2N HCl, centrifuged and the washing is rejected. Washed precipitate is boiled with 2-3 cn of H,O. Cool the solution thoroughly > white shining crystals of PbCI, separate out, Solution is boiled and tested as —» 2 drops of solution + 3 Grops of 5% KI solution -> yellow precipitate of PbI,, Pi2* present. cr. Analysis of Group II This group is divided into two sub groups: Group II A -» Copper Group > Cu**, Pb2+, Bi3+, Cd?* Group II B —> Tin Group Sb**, Sn?* Precipitate is washed with 1-2 cm} of H,O, centrifuged and the washing is rejected. Washed precipitate isheated with 1 cm} of yellow (NH), $ solution and 1-2 cm? of 0.5N KOH solution, stirred and centrifuged. Precipitate - Gr. ILA Centrifugate - Gr. 1B Analysis of Group II A (Copper Group) Dissolve the precipitate in 1 cm} of 4N HNO, and boil it. Add ImL of 2N H,SO, to 2-3 drops of this solution. If white precipitate forms, then add 2N H,SO, to the whole solution dropwise, till the precipitation is complete. Separate the precipitate by centrifuging, Ppt: White ppt of PbSO,] Centrifugate: It is made alkaline with 4N NH,OH solution, boiled and centrifuged. Treat it with 0.1 g of solid = CH,COONH,, 1 cm? of | Ppt: White ppt of Cenirifugate: It is boiled with 0.5 — I cm? of Na,S,0, CH,COOH & 1 em? of| Bi (OH), It is dissolved in| (Sodium dithionate) solution and centrifuged. H,O. Boil strongly and then | 4N HCI. 2 drops of soln are| Ppt: Metallic Cu. Dissolve it in 1 Centrifugate: centrifuge. Acidify the] poured in 10cm? of H,O —| cm? of conc. HNO, by boiling and | acigify it with 4N HCL. centrifugate with 4N| white ppt or turbidity of| neutralise it with 4N NH,OH. 2] add 4-5 cm} of H,O to HNO,, 2 drops of this soln] BiOCI, drops of soln are acidified with] gityte je, 2 drops of soln +2.3 drops of 5% K,C1O,| piss present CH,COOH + 3 drops of 5%] heat and pass HS > yellow ppt of PbCrO, K,Fe(CN), soln - reddish brown) yellow ppt of CdS. Pb present oe ppt of CugFe (CN), Ca** present cr Cu* present cr cr Analysis of Group II B (Tin Group) Solution (free from Group II A) is acidified thoroughly with cone, HCL It is diluted with double the volume of 140, heated and HS is passed. If precipitate forms, itis centrifuged. Centrifugate: Boil off H,S. 2 drops of soln + Iron wire, boil + 4-5 drops of 5% HgCl, soln — white ppt of Ppt: Orange ppt of Sb,S,. Dissolve it in 4N HCI. Boil off HS. 2 drops of soln are poured in 10 cm? of Hx > White ppt or turbidity of SbOCI. Heg,Cly. Sb present Sn** present cr cr Scanned with CamScanner4 Analysis of Group IIT A (Iron Group) College Practical Chemistry (FY. B.Sc.) _____Precipitate is washed with 2.cm} of H,0, centrifuged and the washing is rejected. Washed precipita, is boiled with 1 cm? of 4N NaOH solution, | cm’ of H,O and 3-4 drops of 20 volume H,O, and centrifuges, Ppt: Brown ppt of Fe (OH)s, Mn (OH),. Dissolve it in 4N HCL and dilute with 1 cm? of HO. Divide the soln into two parts First Part (for Fe™*) 3 drops of soln + 3 drops of $% KSCN soln —> blood red soln or ppt of Fe(SCN),. Fe* present cr Second Part (for Mn?*) 2 drops of soln + 3 drops of 4N HNO, + 0.002 ¢ (pinch) of NaBiO, (sodium bismuthate) > pink or violet colour of HMnH, ‘Mn** present cr ‘Centrifugate: Divide it into two parts. First Part (for AU*) 2 drops of soln + 4N HCI till acidic. Make it alkaline with 4N NH,OH — white gelatinous ppt of Al (OH), AI present cr Second Part (For Cr+) 3 drops of soln + 5 drops of 4N CH,COOH + 4 drops of 10% Pb (CH,COO), soln — yellow ppt of PbCrO,. Cr* present cr | Analysis of Group III B (Zinc Group) Precipitate is washed with 2.cm3 of H,O, centrifuged and washing is rejected. Washed precipitate is dissolved in 1 cm? of conc. HCI, boiled and centrifuged. Ppt: Black ppt of NiS and CoS. Dissolve it in cone HCI, Boil off H,S and divide the soln into two parts. First Part (for Ne*) 2 drops of soln + 3 drops of 1% Dimethylglyoxime reagent + 4N NH,OH till soln becomes alkaline —» carmine red ppt of id meg. Ni®* present cr Second Part (for Co?*) 2 drops of soln + 3-4 drops of 4N CH,COOH +3 drops of 2% ocnitroso B naphthol reagent — red precipitate. Co* present cr Centrifugate: Boil off H,S. Make the soln alkaline with excess of 4N NaOH soln, boil and centrifuge. Centrifugate: Neutralise it with conc. HCI. Make it alkaline with 4N NH,OH and pass HS Ppt: Brown ppt of Mn(OH),. Dissolve it in 4N HNO, and dilute it with 2 cm? of HO. 2 drops of soln + 0.002 ¢ (pinch) of (sodium | — white ppt of ZnS. bismuthate) NaBiO, > pink | Zn?* present or violet colour. CT. ‘Mn** present Cr Scanned with CamScannerSemimi ‘emimicro Qualitative Analysis Analysis of Group TV (Barium Group) Dissolve the precipitate in hot 2 «, freshly prepared sat hot 2.cm° of 4N CH,COOH, Te Chikiee rated K.CrO, XCOOH., Test 2.3 drops of the solution with 0. a solut c to the whole solution and centrifuge. W yellow precipitate forms, then add 2 crs! of Ye v Centri Ppt: Yellow ppt of ifugate: AA AN NU, _ CrO,. Dissolw solution wit cm’ OU till the solution become B:C:0,. Dissolve the pe fouaton with 0. em Of feshy prepared ne Becomes aaline. Test 2-3 drops ofthe |. 2 drops of + then treat the whole solution ated (NH,),SO, solution. Uf white precipitate soln + 3-4 drops of 4N n with (NH,),SO,. warm and centrifuge. H,SO, > white ppt of | Ppr: White prot sso, B30, 4N HCI. Centrifuge it Suede, tops of Ba?* present centrifugate +4 drops of NILOM cee) tr of saturated (NH,),C,O, soln a of S1C,0,. . Sr** present CT. Centrifugate: 2-3 drops of soln + 3-4 drops of saurted (NI).C,0, soln white Fr ofc soli white ppt Analysis of Group V: Dissolve the precipitate in 2 cm of dilute HCI. The solution is used as follows CT. for Mg**: (a) 2 drops of solution + 4N NH,OH till alkaline + 1 em? of 3% Oxine reagent in CHCl, Shake well and centrifuge —> yellowish green layer. (b) 2 drops of solution + 0.5 cm} of 10% NaOH solution + 2-3 drops of 0.1% Titan yellow reagent — centrifuge — red precipitate or colour. (c) 2 drops of solution + 2 drops of IN NaOH solution + 2 drops of 0.001% p-Nitro benzene az0 resorcinol (Magneson 1) reagent —> blue precipitate. (@) 2 drops of solution + 3-4 drops of freshly prepared Hypo iodide reagent —> reddish brown precipitate. Analysis of Group VI (Alkali Group) The cations of this Group are generally water soluble, hence they are detected from the water extract. Water extract is prepared by boiling 0.02 g of the mixture with | cm of water. Itis centrifuged after cooling and the centrifugate is used as follows: Test for NH: Take 2-3 drops of t smell of NH. he water extract and add 3-4 drops of 4N NaOH solution to it. Boil strongly .. NH; present er repared Nessler’s reagent > smell of NH. soln. Take this resultant solution on a g the original mixture with 4N 4 ly P tract + 3-4 drops of freslt (a) 2 drops of the water extr ee pa £2 s of 5% Tannic acid soln + 2 drops ©! ae ° aaipot filer paper and hold it in the fumes produced by NaOH solution > black stain on the strip. Scanned with CamScanner. College Practical Chemistry (FY. B.Sc.) Test for K*: ‘Take 5-6 drops of water extract and add 0.5 cm? of 4N NaOH solution to it. Boil strongly to remoye NHj as NH, gas. Cool the solution and use as follows: 4N CH,COOH and then 3-4 drops of 5% 2-3 drops of the solution are acidified with ww it to stand for about 10-15 seconds + , Na,Co (NO,), solution are added to it, Shake well and alloy yeliow crystalline precipitate forms, w K¢ present cr (a) 3 drops of the solution (free from NH,) are treated with 4-5 drops of saturated pictic acig solution, On shaking well, a yellow crystalline precipitate forms. (b) drops of solution (free from NH )+3-4 drops of 50% ethyl alcohol + 4-5 drops of saturated tartaric acid solution — white precipitate. (c) A drop of soln on a paper containing 1% Dipicrylamine reagent —» orange red spot. Confirmatory Tests (C.Ts) (1) Lead (Pb?*): (i) 2 drops of solution (W.E.) + 4-5 drops of 4N H,SO, — white precipitate. (ii) 2 drops of solution on a tile + 2-3 drops of freshly prepared 10% sodium rhodizonate reagent — purple colour. (2) Bismuth (Bi**): (i 2 drops of solution + 4N HNO, till acidic + 2 drops of 10% thiourea solution. Shake well + yellow precipitate. (ii) 2 drops of solution + sodium stannite solution (SnCl, + NaOH till initial white precipitate just dissolves) — black precipitate. (3) Copper (Cu): (i) 2 drops of solution + 4N NH,OH till alkuline > blue colour, put one drop of it on 5% a benzoin oxime reagent paper > green colour, (ii) A drop of solution on a tile + 2-3'drops of 1% Zn acetate solution +2 drops of 5% NH,SCN in solution — violet colour. . (4) Cadmium (Cd**): (i) 2 drops of solution + 2 drops of HO + 5 drops of 0.25% Ferrous dipyridyl iodide reagent. > silky red precipitate. (ii) A drop of solution on a tile + a drop of freshly prepared 0.1% dinitro p-diphenyl carbazide reagent — violet or pink colour, (5) Antimony (Sb**): ()2 drops of solution + 2 drops of 2% NaNO, solution + 0.5 cm? of 0.01% Rhodamine B reagent > violet colour or precipitate. (ii) 2 drops of solution + 0.01 g of Zn dust or Sn metal and warm it + black precipitate. Scanned with CamScanner1 Semimicro Qualitative Analysis (iii) Take a crystal of NaNO, in a dry test tube. Add 2-3 drops of 4N HCI to dissolve NaNO,,. Add 2- 4 drops of 0.01% Rhodamine B reagent and then 2-3 drops of test solution, Dilute the resultant solution Aah excess of HO, shake gently -> lavender colour . (@ Stannous (Sn™): (i) 2 drops of solution + a drop of 0.25% Cacotheline reagent ~> violet precipitate (ii) 2 drops of solution + 4 drops of 30% Tartaric acid solution + 5 drops of H,O + 6 drops of 1% N Benzyl phenyl amine reagent > white precipitate. (0) Ferric (Fe**): (i) 2 drops of solution + 2-3 drops of 5% K Fe(CN), solution —> blue colour or precipitate (ii) 2 drops of solution + 2 drops of 4N HCI + 2 drops of 2% Cupferron reagent reddish brown precipitate. (8) Manganese (Mn?*): (i 2 drops of solution + 0.001 g of Na,S,0, + 2-3 drops of 2N H,SO, + 2 dr0P of 0.1N AgNO; solution — boil — reddish violet or purple colour. (ii) 2-3 drops of solution + 0.002 g of PbO, + 5-6 drops of conc HNO, to settle —> violet colour. —+ boil strongly and allow it (9) Aluminium (AF*): (i) 2 drops of solution + 2-3 drops of cone. HCI + 2-3 drops of 0.1% ‘Aluminon reagent — shake well + $ cm? of alkaline (NH), CO, solution > (NH,OH: (NH,); C03 = 14) “> red colour. slightly acidic + 5 drops of 2M CHyCOONH, solution + 5 > centrifuge — after sometime, upper layer turns intense ii) 2 drops of solution + 4N HCl till Grops of 0.1% Solochrome cyanine reagen purple. (10) Chromium (Cr): (@ 2 drops of solution + 4N H,SO, till acidic, cool +a drop of 20 Volume H,0, + 0.5 cm} of 1% Ether-butanol mixture. Shake well —> blue organic layer. (ii) 2 drops of solution + diphenyl carbazide -> violet spot (11) Nickel (Ni**): (i 2drops of solution + 2-3 drops of & nitroso B naphthol reagent — brown precipitate soluble in dilute HCl. (12) Cobalt (Co**): ({) 2 drops of solution + 3-4 drops of 4N CH,COOH +3 drops of 2% c nitroso B naphthol reagent — red precipitate. acidic + 0.5 cm of 4M CH,COONH, solution + 3 drops of (ii) 2 drops of solution + 4N HCI till 0.5% Nitroso R reagent — red colour. (iii) 2 drops of solution + 0.002 g of NHLSCN + 4-5 drops of amyl alcohol —> shake well > blue organic layer. Scanned with CamScanner8 (13) Zine (Zn**): () 2drops solution + 4N H,SO, till ac (ii) 2.drops solution + 2 drops of 0.1% CuSO, solution College P! vigorously — violet precipitate forms slowly. (14) Barium (Ba?*): () 2 drops of solution + 3 drops of freshly prepared 10% sodium rhodizon: colour, (15) Strontium (Sr?*): (i) 2 drops of solution + 5 drops o yellow coloured precipitate. Gi) 2 drops of solution on a tile + 3'drops of fre: brownish red colour. (16) Calcium (Ca**): mractical Chemistry (EY. B.Se.) 4.4.5 drops of 5% K,Fe(CN), solution —» white precipitate, 1 +2drops of 5% NH,HgSCN solution, f 5% K,CrO, solution + 4N NH,OH solution till alkaline + shly prepared 10% Sodium thodizonate reagent ~ (i) 2 drops of solution + 4 drops of 1% Glyoxal bis reagent + a drop of 2N NaOH +a drop of 10% Na,CO, solution + 4 drops of CHCl, Shake well and allow it to settle — red organic layer. Note: For confirmatory tests of Mg*, K* and NH; , refer to page Nos. 75 and 76. Model Analysis of a Given Mixture Tests Observations Inferences I. Preliminary Tests Colour Blue Cu** salts Nature Crystalline Cl, Br, F-, NO3, NO;, SO}, and CO¥- of alkali salts II. Dry Tests for Cations (1) Heating in a dry test tube (i) Substance melts i) Smell of NH, ii). White sublimation Fusible salts of alkalies NH} salt NH}, Sb* salts (2) Charcoal cavity test (Fumes and incrustations NH}, Sb, I, ete. (ii) Red scales Curt salts 3) Flame tes Without Through geste, Sealer | ovate (4) Borax bead test Light Blue Cu? salts (5) Sodalime test Smell of NH, NHj salt Scanned with CamScanner ate reagent —» bright req‘Semimicro Qualitative Analysis UL. Dry Tests for Anions 9 ‘ation of AN HCL six + il HCI and heat it © Noetfervescence , scence and no acto - onlime water" | CO}" absent ()_No brown fumes NO} absent ‘action of conc. H,SO, (@) Mix.+ cone. H,SO,and heat (No brown fumes Gi) No violet fumes Br, NO3 absent ( Mix. + Cu foil + cone. eee H,SO, and heat it No brown fumes " NO} absent (@ Mix+MnO,+cone.H,S0, | (Yellowish green fumes and heat it bleaches blue litmus paper | Cl Present (ii) No brown fumes (iii) No violet fumes Proven Chromyl Chloride Test Mix. + solid KCr,0, Yellow precipitate Cl present and confirmed (1:2) + conc. H,SO, 4, gas is passed through dilute NaOH solution and then add Pb(NO), solution Ul. Dry Tests for Anions Conclusion: From dry tests, given mixture may contain Cations: Anions: cr Cu and NH, IV. Wet Tests for Cations Preparation of Original Solution — (O.S.) 0.1 g of mixture +5 cm? of H,O> Soluble — Water extract is O.S. Scanned with CamScanner7 practical Chemistry (FY. B.Sc.) College V. Separation ‘of cations into Gi (Without using 11, Gas) OLS, + Lem? of 4N HCI > No precipitate. oups (Table No. 1) < heat to boil ~» No precipita Lad 2nd ‘0.8. is tested as follows: absent | Sulphate |-test for Fe™*: 2 drops of solution +2 Poe | Group | 2. Fe absent ops of 5% K,Fe (CN), Solution 9 No blue colour or preci, Boil and add 1 cm? of 5% (Ni, | WsMp, absent | ae | Tet for PO, 2 drops of sotion + 1 em? of cone. HNOs * Ba, | solution to it. -» No canary yellow precipitate absent PO, absent - ard Ow Solution fs coloured blue. To te solution, ald 2-3 em of 6 M NsOH soa Hydroxide | and centrifuge it sent, | Preepltate: ; vans, | White insoluble in excess of NaQH | For testing K* and NH, use water ex, Ferm, | solution directly Mn? c+ Cut present, Dissolve the absent | precipitate in a few drops of conc. HCI and perform C.T. For Cu. V. Separation of cations into Groups (Table No. 2) (Using H,S Gas) Divide water extract into two parts and test as follows: O'S. + dilute HCI — No precipitate. Ist OS. + dilute HCI, heat and pass H,S gas and centrifuge. | group | Black] Cenrifigate: Fe fom ID group's boiled io remove H,S completely Testa litle poron lr | absent | ppt | nd L. Test for Fed ~ centefugate + K,Fe(CN), — no blue colour ~> Fe?* absent. | 00 1. Testfor IPA group > centtfugae + NHCI (exces) + NH,OH, till there is smell of NH, | present 1 | A group No pptitt™* | Centrfugare: + NH,CI-+ NH,OH til there is smell of NH, and then pass HS. absent No pptittt' | Centrifugate: + [Boil off H,S (if any)] + NH,C1 + NH,OH + saturated B_ group | freshly prepared (NH,);CO, solution. NopptV® | Centrifugate: + NH,Cl + NH,OH + Na,HPO,, beat. absent group absent Noppt ve group absent NaOH, boil it, Centrifugate: Reject it. Water Extatt* ‘Smell of NH, NH, present VI" group] present WEE, + NaOH boli ‘Then add CH,COOH and Na,Co(NO,}s No prt Ke absent Scanned with CamScanner81 Semimicro Qualitative Analysis VI. Analysis of Groups Analysis of II" group - Separation into II" A and Ii" B Groups Black precipitate + yellow (NH,),5 + KOH boil it and centrifuge. Precipitate: 1" A group Centrifugate: 1" B group. Centrifugate + conc, HCI —> no coloured solution o ppt. 11” B group absent. Analysis of II" A group Precipitate + 4N HNO, -> boil -» solution. Test a little portion with 2N H,SO,. No precipitate Centrifugate: Add NH,OH till it becomes alkaline and boil it. pov absent No white precipitate Centrifugate: Boil it with N2,S,0, solution and centrifuge. B Bi? absent Precipitate: Metallic Cu. | Centrifugate: Acidified with Dissolve it in conc. HNO, | 4N HCl, dilute it with HO by boiling. Add NH,OH | and pass H,S — No yellow and then CH,COOH. Add | ppt K,Fe(CN)g — reddish | cq? absent brown ppt. Cu?* present cr Solution + 4N NH,OH > put one drop of it on Alpha Benzoin oxime paper > green colour. Analysis of VI"* group Divide water extract into two parts and test as follows: 2nd Part Ist Part WE, + NaOH — boil it and cover the mouth of test tube with moist turmeric paper. salt present. Smell of NH, and paper turns brown NH cr WE. + freshly prepared Nessler's reagent —> brown ppt WE. + NaOH - boil it to remove NH, completely. ‘Then add CH,COOH and NajCo(NO,), — no yellow PPL — K¢* absent. Scanned with CamScanner® College Practical Chemistry (F-¥. B.Sc.) VII. Wet Tests for Anions * Preparation of Water Extract: Mix, + 11,0 — soluble — W.E. Tests Observations Inferences 2 WE. + Ba(NO,), solution White ppt S04" present WE. + CH,COOH White ppt SOF present —45 +Ph(CH,COO), solution | WE. + dil, HNO, + AgNO, White ppt Halogens present | solution | a F absent | WE. + CHC), + No violet layer Br absent Chlorine water No brown layer Cl present - | WE. + dil. HzO, heat and cool it. | No formation of brown ring NO, absent | Then add freshly prepared FeSO, solution . WE. + cone. H,S0, —45 No formation of brown ring NO} absent cool it. Then add freshly prepared FeSO, solution VIII. Results The given mixture contains | Cations: Cu?*, NHy | Anions: Cl-, SO” Probable composition CuSO,, NH,CI ooo Scanned with CamScanner