Analytical Separations 44 withthe liquid, and, afer agitation solid Lateia ‘centrifugation oF filtration, Most for 4 by deenmatons own in Pig: 304, Soxhlet °s CODtinNoyy save analyst me, tractions jy used for analysing biological and other f inorganic extraction procedures, Fig. 204 ; Soxholt extractor C = condenser, E = extractor, S = Siphon, B = boiling 30.13 Applications of Extraction Procedures ‘An extraction is often more attractive than a classic precipitation for separating i ‘The processes of equilibration and separation of phases in a separatory funnel are inherently ey and time-consuming than precipitation, filtration, and washing. In addition, problems of copre postprecipitation are avoided. Finally, and in contrast to the precipitation process, extraction tre ideally suited for the isolation of trace quantities of a species. 1. Inorganic Separations Ether extractions of metal chlorides. The data in Table 30.3 indicate that a substantial metal chlorides can be extracted into ether from 6 M hydrochloric acid solution; equally imporian number of metal ions are either unaffected or extracted only slightly under these conditions, useful separations are possible, One of the most important of these is the separation of iron ll extracted) from a host of other cations. The greater part of iron from steel or iron ore samples removed by extraction prior to analysis for such trace elements as chromium, aluminium, titanium 06 The species extracted has been shown to be the ion pair H,O* FeCl,~. It has also been percentage of iron transferred to the organic phase is dependent upon the hydrochloric acide» the aqueous phase (litle is removed from solutions that are below 3 M and above 9 M HCl) adi Involving Solvent Extraction fn 2.561 io content. Unless special precautions are taken, extraction of th ase es of on Is of nitrates. Certain nitrate salts are selectively extracted by ether as well as othe Je, uranium is conveniently separated from such elements as lend and (het ys ee solution that is saturated with ammonium nit nrolum by ether ofa pe uranium must be in the +6 oxidation state, Bi rate under these conditions, » ate and has @ nitric acid concentration ismuth and iron(II) nitrates are also Elements and Oxidation State Fe(Itl), 99%; Sb(V), 99%; Ga(II1), 97%; Ti(II1), 95%; Au [III] 95% * Mo(V1), 80-90%; As(II1), 80%; Ge(IV), 40-60% iw Te(IV), 34%; Sni(Il), 15-30; Sn(1V), 17%, In IV), 5%; Sb(ITI), 25% «po As(V), Cu(II), In(III), Hg(ll, PuLV), Se(IV), V(V), V(IV), Z(t) ' ACI), Bi(II1), Ca(I1), Co(tt), Be(tt), Fe(I1), Pb(H}), Mn(i}), Ni(I}, Ox VIN), PACH) RII), Ag(l), Th(V), Ti(IV), WCVI), ZA(1V) Eitraction of chelate compounds. Many of organic reagents form chelates with various metals ions, feechelates are frequently soluble in such solvents as chloroform, carbon tetrachloride benzene, and ‘tx Thus, quantitative transfer of the metals ions to the original phase is possible, A reagent that has widespread application for extractive separation is 8, hydroxyquionoline, Most ‘ismetal chelates are soluble in several organic solvents. The reaction which occurs when an aqueous ‘ison of a divalent metals ion M2* is extracted with an organic solvent containing 8-hydroxyquinoline ‘stolzed as HQ) can be formulated as 2H org + (M?*)oq FE (MQ)org + 20H aq ‘ter the subscript indicates the phase. The equilibrium is clearly pH dependent thus, separations among as having different formation constant with the ligand are possible through control of the pH of the ‘u phase. The latter has proved particularly useful for separation of traces of metals. gg fDether useful reagent for separating minute quantities of metal ions is dithiozone (diphenylthio- ). Its reaction with a divalent metallic ion can be written as HOCH, ‘Ae H N-N-CH, | Me2H" M™ +25 = = ICH -N-N=C ss ~ ‘ dithizone CH, : metal i ; ith 8-hydroxy- asia pees ruble in a variety of organic solvents. As wit MH of a, Me eaUl sraettecoe alia it the reagent is pH dependent; thus, by controlling the Fhe aqueous phase, various separations of metalic i jons are possible. 4 'M* dithizone complexes of many metal ions are intensely colored: Spectrophotometric measun extract often serves to complete the analysis 4 enna fter the separation has been performed " ents for separations by extraction can ve aration concerning the use of other organic chelating #8 paeeeee oe Inotate + It is possible to extract ferric jon from aqueous Dra re ern Shares? “Guinoline in chlorofoem by double extraction, The optical$62 Analytical Separations Involving Solvent fu, density of chloroform layer is determined the using a spectrometer. This process May be cere, further oxine solutions and the optical density is again measured, ‘ It is important to remember that the pH of the aqueous solution should lie between 7 ade Determination of uranium as 8—hydroxy quinolate : It is possible to determine Uranine hydroxquinolate in the presence of some EDTA at pH 8.8. The EDTA masks the interfering ions tips AL etc. Now the optical density is determined as usual. Similarly it is possible to estimate other cations by using suitable organic reagents. For orange (®) Determination of nickel as dimethyl-glyoximate complex. (@) Determination of molybdenum by thiocyante methods, (2) Determination of lead by dithizone method. ({~) Determination of copper as diethyldithiocarbamate, etc.