a QUALITATIVE INORGANIC ANALYSIS eT Ce CTR OM, FG HCI IE HE RCIA, THES, Sb & Bi AE salts BL oxy-salt form Tea ae cere a She reA oxidizing agent HC are Hea 4 insoluble Pf aqua regia soluble~ Tor Teer Hi Hes ae a SelB, MSc(Organic. Sp) Ph. 9064543951 Hela(red) a Regier ~ i) Allthe salts of sodium, potassium and ammo: ates of all metals are soluble in water (e: lorides are generally soluble in water (excep ~ AgC ld water, but easily soluble in hot water. iv) The solu v) lodides are generally sol /) Except the fluorides of Na, K & NH«~ al ity of bromides of Pb, Bi, & Sn(II) are sparingly soluble in water. iphates of Agt, Hg?* & Ca2* are slightly soluble in water. -Sare insoluble in water. water. Those of other metals are insoluble in water. ates of metals (& NH«*) are generally soluble in water (exce} es of Na, K, Mg, Ca, Ba, Sr -are soluble in water. Other metal ix) The phosphates, arsenates and arsenates of sodium, potassium are sol x) Thiosulphates are soluble in water (except ~ Ag* and Ba®* thiosulphates). / xiv) Sample of BASIC RADICALS Gri | crv Grv as, INI, Cor, Mne*, Zn* | Cate, Bas, Sri Nar, Ke, Mges, Nw Poet, Hire, = Bi __] I _ ACID RADICALS LRICE Br, 1 SCN: S% $0.2, SOx", S10: POs! Ass’,QUALITATIVE INORGANIC ANALYSIS Seperate different coloured sample} KASH PORIA if possibl solubility test is PRA\ (if possible) _ Test for interfering BSc(M), MSefOrgonic. Sp jertorm Hot #0] ‘one. | / + Ph, 9064543954 lame test HC | [Fenoaoon Lsnocons}fnaione Dry test] Dry acid Basic ‘TT heating C.HClext. HC. H,SO, test] Sulphide = Lferransienonce] ge ae ; j Ciupt Group IIIA Group IIB [c. HNO; ext} Specral test sulphide Tworescence Test some special test Perform flame test with seperated sample & with saturated water extract/, ee QUALITATIVE INORGANIC ANALYSIS eo Test for basic radi a lo 1 Colour change: Tit for baste radicals —_ Cold Compounds Conclusion White Zn** or ZnO Yellow Pb?* or PbO ish brown Yellow sn**, Bist Brown Brow Ca?* or CaO Red to black Brown Fe,03 oe oven, Green Cr3* or Cr03 | lackeniny ¢ * 2+ Mn? Ni2+, Co?* | 2sublinateormation 8 f black Cu?*, Mn?*, Ni?*, Co § * White sublimate: may be NH}, HgCk, HgBrs, HgiCl, As,0s, Sbx0s 2 Sublimate + ConcHCl + HaS Black > Hg2+, Hg3* ; t a Yellow ~ Asi03 | 2 ~ Orange ~ Sb203, a % £ ~ No change of colour NHf salt 1 & Sublimate + NaOH + Nessler reagent + water Brown -» NH{ bb + Yellow sublimate: May be As7Ss, Hglz or free sulphur. [Yellow sublimate turns red when rubbed with a glass rod > Hglz] ss * Black Sublimate: May be HgS. [Black sublimate turns red when rubbed with glass rod] a * Gray sublimate: Hg?* salt. (Gray sublimate gives globules on rubbing with a moist glass rod] 2 3. Gas evolution: Pa | o * Issuing gas + K2Cr207 paper > Green + S03~, S,03-, SO}. PRAKASH PORIA 8 «Issuing gas (smell of rotten eggs) + Pb(OAc)2 ~ paper ~ Black -» S?~ (SCN° interfere the test). | BSc), M.Se(Grgenie. S23) 2 = Issuing gas + mercurous nitrate paper > Black > NH. | Ph. 9064843951 { 3 + Greenish yellow gas + starch-iodide paper ~ Blue > unstable chloride (like CuCl,), CI", I>. is Be + Issuing gas + starch-iodide paper ~ black > Br~. A 4, No colour change on heating: + White colour remains unchanged on heating — salt of Mg, Ca, Bs + Melts on heating & becomes solid on cooling ~ salt of alk. On heating sample first swell up then melts and finally solidi * Black colour remains unchanged ~ CuO, MnO2, NiO, Cos04, * Green colour remains unchanged ~> Cr203. + Dry test tube heating - 9 BY ~ BE MST BW > Pb(NOs)>. = CdS SRP ICS TAC ACA WOT BCI A. Al ine earth metals, PbX2, PbCrOs, ~ borax or any alums.N — @ _ > QUALITATIVE INORGANIC ANAL YSIS Sia Conclusion > Nat(col Iss) : aK Scat onc mple, S Green flame = Cu®* / BO} / HsB0s @ Bish green freon tke sake tong) ~ Sa-compounds Sree racemes + carpanr mage aww connect pesar ene ee Bee ee er eer ene eek he "SSgolden yellow through naked eye —» Nat os ka, +a litle bit ow Con 7. HClextract + Ki[F(CN)s] > Blue colour — Fe* 2. HClextract + Ks[Fe(CN)é] > Blue colour -» Fee 3. Solution + (NHsHF2 or NaF if Fe3+) + NH 4. HClextract + (solid tartaric acid if Fe) + NH4OH (excess) + DMG,(dropwise) > Red rose NF* 5. HClextract + KI (solid) or K2CrO4(soln) > Yellow ppt > Pb?* ‘ & Icohol (shaken well) + con€ HCl (2 drops) > Blue green solution, few drops ona filter & HCl extract + NH«SCN (solid) + little acetone or amyl al > paper, dry it over burner > Nice blue colour > Co?* 7. HClextract + HS — Orange ppt ~ Sb } = Brown ppt > Bi?*- ’ - PRAKASH PORIA * BSc(H), M.Se(Organic. Spl) . ~+ Yellow ppt on dilution ~ Cd?* = Yellow ppt > As, Ph. 9064543951 8 4c. slon poured into a beaker containing large volume of water — Mi colate Cit (Felt areca NH,OH CaM wa ppt. B filter wea test 1 Tee] = dis ed, soluble in excess KI mn ppt — Bi? tests are performed] jlumbite soln [ Pb(OAc)z soln + conc NaOH soln shake to get [If not dissolve the following i) Residue + dil HCl, shaken to dissolve + KI soln ~ Brown ppt was soln to give a yellow ppt + Na2COa(solid) ~rcolourless soln + passed ~ Brow One part of residue + minimum conc HCI shaken to dissolve + sodium p colourless soln) = Black ppt > Bi?* : se) + water -» pink colour ~> Co? [A blank test must be performed without using the sample extract} he soln on spot plate + 1 drop of Na,S soln ~ Yellow ppt ~ Cdz+ 9. Solution HCl extract + NHsOH + warm + 1 drop of t 1. take filtered & add NHsOH & 2 drop K:Cr0, > Lemmon yellow ppt ~Baz* ‘nd, rosidue 4 ACOH (to dissolve) + amfmonium oxalate - white ppt ~ SEY Soln + K2CrOs (excess) + filter & reject pp' "After lomon yellow ppt filter ~ filtrate + NH,OH + solid (NH«)2COs > pot plate + 1 drop of soln ~ colour discharged ~Sn’* Go a mirror of metallic cadmium with brown edge (C40) was formed + cool + litte S-powder _ C.HClextract test: & st: Sample + C onc. HCl + A + cooled + fitered, | Flame test: Pt wire in & 12. Adrop Methylene blue solution on s 13. Sai ina dry test tube + solid sodium Gxalate + + heat + mirror becomes orang n cooling becomes yellow ~ Cd?* _ @ soln + SnCly + aniline ~ Black or brown ~ Hg [Dry solid + 1-2 drops NH,OH — Gray or black -> ge) —__ _ pet - gute, Wot at gad > CUBA eT + dis offs ae a) “Sy eofout mol eboney ie Gl Wel cubtact + 1 drop kt = Gil Pd eubracl & 3chop let —rrgoddout peer ky[iiNO, [1. 2cc.soin + 6 cc ammoniin ; Us exttest: |2 bd QUALITATIVE INORGANIC ANALYSIS sample + |? ‘ low -+ POR Condlusion | In + water for dit cone. + dil HCLin exce = tered {A} + solid NHS ss and filtered ~ [A] | acer Pau ICN + Co(NOs)2 crystal shaken well & scratch the side ofthe test tube with glass rod- Blue ppt. + + cooled {B] + H20 + shaken + KI H aken + Kl excess ~» Red pptn which on treatment with o - : + NH.OH (dropwis th excess KI ~ Light green + excess Kt ~ soluble + filtered {HOH (dropwise) + solid NaOH (shaken well) ~+ brown or orange or yellow ppt. +Hg3" : oR sola Solution + ACOH + Hs a - - iS pass = Wiite ppt > Zn 1 i — Be Cfbtack is Pree 1 PRAKASH PORIA | Conctusion gas Yellow ppt Asay be | B.Sc, MSe(Grganic. 8 £28. Orange ppt > Sb¥ maybe | Ph, 9064543951 ¥ 3 +3 ez Solton + NERC (excess) + & > Getatinous vie ppt ALYY * ¢ ‘S's & 5/3 7 d —_ at 4 B® Solon on spot plate (2 drops) +2 drops Alizafin-S + dil AcOH (rubbing with a glass rod tintl violet colour just disppears— Red ppt — Gee a f ce GO BE 4 NaOH extract (12rop on filter nape) 4.1 drop KeFe(CH)es 1 drop of te dlp of ai HCl 1 drop Alearin held over Nis ote then ry ee it over burner ~ violet red colour > Al*+ * ; & GB |S. NaOH extract (1-2 drops on a spot plate + dil HCl + very di soln of C(NO})s oF CuSO4 + ammonium mercurithiocyanate (H:0+ HeCls | solid + NH«SCN solid shake to dissolve) + rubbing on spot plate ~ Violet or blackish ppt» Zn?+{Blank test must be performed] | yg | aWellow mass = Cr+ =F) ] Condusion a SE Z| 7 Green mass — Manis, MnOz & © S | roured into 20m! water] 2 8 £5 | 1. Soin (ellow) + dil ACOH + Pb-acetate ~ Yellow ppt > Cr'* | 5% BE | 2. Soin + ail Aco ~ Pink colour Mn, MnOz{ add few drops of onc HNO3} BS = 4G Soln + dil AcOH + NaNOs (to discharge pink colour) + Pb-acetate ~ Cr3+ [when both Mn & Cr are present] ES +14, Soln+ dil HaS0«-+ 2cc amyl alcohol + H202-+ shaken ~ Orange certurns blue ~> Cr, Cr0?” | G2 | 5. Green mass 2 Cait C1 WE ACOH RRA pink colour SHOT Ie Pret whl —+ MnO I Fluorescent | A mixture of 0.2 gm of the solid sample, tin free zinc granules & 10 ml cone, HCl taken in clear beaker, is stirred with the outside end ofa test | Conclusion Test fort | tube hal-filled with cold water and then the test tube is held near the Runsen lame ~ a blue fluorescent o9n the outer wall of the test tube ~ 2, Sample + U2Hs0H + Br AsO3" interfere this test] 1 L_ ccSlicals | 3. Paste the solid sample 4 7 BO}. [Cur ae BOS” = 4, Sample + silica + conc. He S BF Sample + borax + Idrop o ;ouch) ~ green flame -» 6QUALITATIVE INORGANIC ANALYSIS: Conclusion ww ppt Ca? LOH 41S > } PRAKASH PORIA in + sample + Blue ppt» Sn? 3 “+ NH4OH (excess if required) — getatinou: é of NH which turn moist HCI gh ite smoky NAS | ascan O , Z|. testlor Onde: Sample + NHsCI» sinell of NH (arms H rod Smokey) ~ Oxide j BSC, MBOrgonic. Sol), z L9- Sample extract in conc HINOs + dil H2SOs (Slight excess) + NH ; Ph, 9064543951 E Residue: White (BaSO,, $1504, CaSO4, PbSO4) in atest tube + saturated syln of (NH):SO4 (excess) +O —__+ Resiue: white (BaSOy, SrS0,, PbSO«) + saturated soln of Hcl untilacidic, shaken well + 4+ iftrate:fitrate + dll AcOH + saturated soln f _é of (NH4):C204 + dil NHAOH until alkaline ~ Residue: Flame test performed — crimson red — Sié* jaterfitrate + KiCrO,> white ppt filter ~ flame test done ~ transient ~ apple green flame — Bat* low ppt Pb2 brickred lame Cat*_> a i Test for acid radicals oe - + Brown fumes turning starch-KI paper bluish black NOz. P Condusion + Smell of H2S lead acetate paper black +57. = + Smell of burning sulphur turning acidified K2Cr207 paper green > soye H2SO« + & + Same as above with deposition of sulphur ~ 5,03”. i a = Brown colour intensified on addition of Cu-turning> NO; =f Conclusion Concacidtest: | + Reddish brown vapour tugning starch-Kl paper blue > Br-,BO; fw Sample + conc. | * Violet vapour turning starch-KI paper blue — I~, 103. tn HiSO.+, | * Pungent smelling gas producing dense white fumes with NH _ + _Colourless gas with oily appearance of the liquid on the inner wall ofthe test tube —> F- Chomp chtonde | SABE # KeCn0) + Cone. HeS0« + 2 Evolution ‘of brownish red vapour of CrO.Cle oa Q joride | “produced vapour + NaOH + AcOH + Pb(OAc)2 > yellow ppt. Cl” {Chlorides of Pb, Ag Sn & Sb partially repond this test / Hg-chlorides do not rest: respond this test] A » [ . | Nabil bead +a few drops of water +B — smell of NH; (urns HCI moist glass rod smokey) —~ NH. Conclusion _Testfor [+ Sample +a-napthyl amine + sulphanil acid in a spot plate > Red colouration > NO. NOz,NO3 & NH: | -yRed coouration after addition of Zn-dust > NO3.[Sample-& * NOs + NOz SE GF TAsample f AF AKA) Special test for | Sample + Zn-granules + dil-H2SO« + heat + moist Ph-acetate paper held at the mouth ofthe test tube —> Lead acetate paper turned black | conesion sulphides: _ _ ——— = = — + GallsOH + A = Green edged flame + B03”, HB0s. Conclusion Test for | 1. Sample + conc. HzSOs interfering | 2. Sample + CzHsOH + 4 ~ Green egged flame ~ HaBO. radicals | 3. Paste the solid sample + CaF2 + 1 drop of conc. HzS0., taking on a Blass rod, held ver BOS”. [Cur* MRA BOF” 421 NO flame TA] + silica + conc. H2SOs-+.4 + 1 drop of water lie ina glass ro x close to the flame ~> Green colouration of the flame > held on the mouth of the test tube + water drop becomes opaque > 4. Samp! pS Sample + borax + 1 drop of cone, HzS0« stirring with glass rod + paste taken on the tip ofthe glass rod + held very close to the flame (don't le > red colour discharged > F> __ . ———EEEE 4NazCO3 Extract test: 1 gm sample + Water extract test: + 2 Ez < + S a 2 E & ‘TT. Soln (1-2 drops) on spot plate + si for 10-15 min with continuous i) Sample + NaOH bead + Zn-dust + 4 — Smell of Ny + N03, NO i) Test for NOS in the absence of NO} : (red co ur gives alter addition of Zn-dust) iii) Test for NO¥ in presence of NOz: (same test done after decompose of NOz by boiling with urea) \ GB Ring test: Sample soln (NazCOs oF H20 extract) + FeSO, + conc. H2S04 (slowly) -+ Brown ring at the junction of two I Gip the test tube into beaker water) ; (if NOz present perform the test after boiling with sulphamic acid) v) Solid saniple + NaOH (bead) + Zn-dust + 1 ml HO + A ++ Nessler’s reagent » brown -> NOs vi) Solid sample + conc H2SO, (1-2 drops) + KI soln ~ violet colour appear > NOz 2. Solution + 4-5 drops FeCls > Red colour > SCN* Solution + Zn-urinyl acetate + scratched vigorously > Y t— Nat Solution + Na-cobaltinitrate solid (a pinch) +.dil ACOH + 1-2 drops AgNOs + scratch ~ Yellow ppt > K* Solution + NH«CI (solid) + NazHPOs soln + scratching > White ppt > Mg?+_ Solution + titan yellow (2-3 drops) + NaOH soln on a spot plate. rubbing with glass rod.-> Red colour» Mg?* Soln + oxalic acid or ammonium oxalate + shaken — White ppt ~» Ca’* ‘a § Solution + Na-nitropruside — violet or pink colour > S?~ “4 2. Solution + dil HNO + boiled + cooled + AgNOs soln > White ppt soluble in NH4OH — Cl Yellow ppt soluble in excess NHsOH— Br~ = Yellow ppt insoluble in NH«OH — I~ White to yellow to brown to black ~» 5,037 Solution + dil HCI + heat + cool + 4-Sdrops of BaClz — — White ppt insoluble in HCl > S03 = White ppt soluble in HCl -» S02 ‘The solution of white ppt in HCl + 2 drops of lz + Brown colour of Iz is discharged > S03~ {SO2- + $03 see ae white ppt 42 HCI soln filter Wa + Bacle - AFI colour Wa XA SOF J 4. Mixture of CL“, Br=, J": » curdy white ppt soluble in NHyOH >CI~ ii) 5 c.c. of NazCOs extract + dil HCI + 1 c.c. CCls or CHCls + Cl add drop wise with gradual shaking, = Violet colouration of the organic layer ~> I~ ___ = Viloet colour disappear & Brown colour appear ~> Br7 (if both Br & I” present) PRAKASH PORIA B.Sciti), M.Se(Grganic. Sp!) Ph. 9064543951 i) 3 cc. of NazCOz + ACOH or C.HNOs + PbO2 + boil (to expel Br2 & Iz completely), filtered, filtrate is acidified with HNO: + AgNOs > = NOs QUALITATIVE INORGANIC ANALYSIS Conclusion Conclusion | Neutral soln test: 1. Soln + CaCl: White ppt > F~, POZ~, AsO3~ NaxCOs extract + d HNO ( checked by NHAOH (unti Nits) + boil to remove in ACOH > F>) 2. Soln + dil FeCl: (freshly prepared, drop wise) ntly acidic, | 3. Soln 4 excess AgNOs ~» White or yellow ppt > halides mus) + — Scarlet ppt > CrO? mell of ~ Yellow or brown ppt > °0}~, AsO}, AsO}, Si03- NH, ConclusionIf cation is: Li’, K", Na’, Rb’, Cs* or NH." Otherwise, check anion Solubility Chart [Yes Soluble Se = = = always //*~]_Yes NOs (nitrate) and C,H30, (acetate) No z ° PRAKASH PORIA | If antionis..... penance ga coe a ee = CI (chloride) SO,” (sulfate) | cO;* (carbonate) OH (hydroxide) Br (bromide) ‘| pO,? (phosphate) | I- (iodide) «| S* (sulfide) | | | ¥ Soluble, except for: AgCl, PbCly, He2Cl, Ager, PbBr2, Hg2Br2, Pblz, Hézl, which are insoluble Insoluble always Soluble, except for: CaSOq, Ag2SOu, BaSO,, HgSOz, PbSOs which are insoluble (except with soluble cations) Insoluble, except for: © Ba(OH)2 which is soluble, and © Ca(OH), which is slightly soluble