Introduction. Sueli P. Quináia and Maria do Carmo E. Rollemberg *

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1 J. Bz. Chm. S., Vl. 12, N. 1, 37-41, 21. Pitd i Bzil 21 S. B. Quími $6.. til Slti duti f i Spi Hdid Gti tmi pti Sptmt. Pt 2 Smpl Stg d i Dtmiti i Ntul Wt Suli P. Quiái d Mi d Cm E. llmg * Dptmt d Quími, Uiidd Etdul d Migá,. Clm, 579, 872-9, Migá - P, Bzil êi ttl,, (V) áid dimtilíi (DM) fm dtmid ltimt m águ tui pl téi d gçã d hidt ptmti d çã tômi, m dift mi d duçã. P mt d águ d i itigd ultd mtm t fm il pdmit. O limit d dtçã td p (tmpã itt), DM (áid éti ) (V) (áid lídi) fm, ptimt,.6, mg L -1. O tud d tilidd d fm ii m mt d águ tui lu m pópi mi ii it p um pçã dqud d mt. Ttl i, it, it d dimthlii id (DM) w ltil dtmid i tul wt hdid gti tmi pti ptmt, uig dium tthdt(iii) dutt ut i difft duti mdi. i wt mpl fm th th gi f Pá Stt, Bzil, w ld d hwd t th piipl il fm. Dtti limit fud f (itt uff), DM (ti id) d (V) (hdhli id) w.6, 1.1 d.5 mg L -1, ptil. Smpl tg th pp ti mdi ld t uful w t p th wt mpl. Kwd: tul wt, i piti, tmi pti ptmt, mpl tg Itduti i ighmil l u mtl i th quti imt d it iumulti i imptt txilgil pt 1,2. Bid thi, i tmiti i tul wt h ltd t difft di i m uti; hg i th ki pigmtti, kt d im h itd t th itk f tmitd wt f lg tim, th umulti th gim i m pid th it xti 3,4,5. i fud i tul wt dild gi d igi fm. M pi with difft txilgil d hmil htiti fmd dpdig t th ph, lkliit m th il. Fm glgil u i i fud i tw l tt: lt f th i id ((V)) d f th u id (); th ti tw th fm dpd th ph lu d xidiig duig ll diti. I th imt, th p f mthltd i mpud uh mmthli id (MM) d dimthlii id (DM) i ft ud hum idutil tiiti d giultu. Hw, gi pi m l pdud til itfmti f igi i fm 6. Biti tfmti i quti tm dpd th kid f gim pt, d l gil mpud fmd 1,7. I tul fhwt it, t, dimthlit d mthlt pi h dttd, ut i gl it, t d dimthlit th mi il fm 8. Mitig mthd f dtmiig th difft hmil fm f i i th imt mig iigl imptt du t thi difft txiit d hmil hiu, uh luilit i wt d dpti t dimt 9. Cqutl, iu piti pdu h ppd d iwd 1. Dpit th it f iti ltil thiqu f t lmt dtmiti, tmi pti ptmt i till th mthd f hi f uti dtmiti f lg um f lmt. tmi pti ptmt with hdid gti llw d iti dtmiti f ttl i, uull ft mplt duti f th difft fm t it; l piiliti h ppd f th i piti i difft mpl I piu wk th ltil diti f th lti duti f i pi hdid gti tmi pti ptmt w tudid 18. Bifl, it l

2 PB 38 Quiái & llmg J. Bz. Chm. S. w mud i.4 ml L -1 itt uff (ph = 4.4); it plu t w dtmid tgth i 6. ml L -1 hdhli id ft p-duti with ptium idid, d it plu dimthlit pi w dtmid i.12 ml L -1 ti id. Ttl i uld dtmid i 6. ml L -1 hdhli id fllwig p-duti tp f th t d dimthlit pi with ptium idid - tu hlid mixtu. Thi pp di th dtmiti f i dild pi i fhwt uig th ti mdi piul ppd d impl mpl tg pdu. Expimtl pptu Vi Tht -175 tmi pti ptphtmt, quippd with hdg hllw thd lmp kgud t d i hllw thd lmp w mpld; th lit width th ptphtmt d th wlgth w t t 1 d m, ptil. Th hm-md hdid gti pptu ud w piul did 18. gt i xid 99.5, f igi (idl D H), i ptxid 99.3, f igi (V) (Bk l), dimthlii id, dium lt, 98 (Sigm) d dium tthdt 95 (Mk). ll th gt ud w f ltil gt gd: Th 1 mg L -1 quu tk luti f t d dimthlit pi w tddizd git it, uig flm tmi pti ptmt. Pdu Glw lig. ll glw w kd ight i 1 / iti id d id with ditilld wt f u. Smpl pti. I d t lut th mpl pti kw qutiti (3. µg/l -1 ) f h i pi w ddd t tul wt mpl piul djutd t th ltd ti mdi d mitid i gl flk t 4 C. Th difft i fm w dtmid pid f i d. i dtmiti i i wt mpl. Th uf i wt mpl w lltd i plthl flk, filtd, djutd pil t th pppit ti diti d mitid ud figti i gl flk util th l. Figu 1 ummi th pdu f th lti dtmiti f it, t d dimthlit i tul wt mpl 18. SMPLE 125 ml mpl 125 ml HCl 5 ml 1 KI 25 ml mpl 1.8 ml ti id 25 ml mpl with.4 ml L -1 dium itt d 1 ml L =1 iti id 125 ml mpl 125 ml HCl 5 ml 1 KI.3 ml 1 ml L -1 SCl 2 18 ml mpl luti 8 ml mpl luti 18 ml mpl luti 18 ml mpl luti HG-S HG-S HG-S HG-S (V) DM (V) DM Figu 1. Pdu f, (V) d DM lti dtmiti i tul wt mpl

3 Vl. 12 N. 1, 21 Slti duti f i Spi Hdid Gti 39 ult d Diui I piu tud 18 ilig l i, it-f fft i th i dtmiti w td i hdhli id mdium, mtl du t mg, hmium, tim, mu d imuth. Itf w l d i itt uff d ti id mdi, du t i, zi, pp, ikl, hmium d lium, wh th i w idiidull ddd t impl quu luti; hw, tul wt hw muh lw ll f uh i th thi itf thhld, xludig F(III). piul d (V) DM p-duti i pid d mplt, d th pi gi th m p i th ltd mdi 18. Thu itfig fft i th li f l mpl w lutd ddig kw qutiti f it t filtd wt mpl, djutd t th ltd duti mdi. O th lp f th lt dditi u w imil t th f th pti quu luti, itf w dttd. S, igl u uld tlihd f h duti mdium, with gd lti (Figu 2-4). tt ddig it t i wt mpl xhiitd gd m lu, lw l t 1 (Tl 1). S, i pit f m itf fft f idiidul i dttd i impl quu luti, th ll mtix tiuti did t m t u wh dtmiig i i l wt mpl. Tl 1. f i i Ntul i Wt (=3). ti mdi i ddd, i d,, µg L -1 µg L -1 Hdhli id 6 ml L ± ± ±.4 12 Citt uff.4 ml L ± ± ±.4 99 ti id.12 ml L ± ± ±.7 97 imptt pt f piti i th tud f th diti f mpl pti th phihmil htiti f th tm mut mi ultd. Th iu quilii uig i tul wt ilig mtl i mk th mpl pti itil, hg tw t d it ud til tiit, wll xidiig duig mpt i th tul wt 19. I gl, th dditi f id h mmdd f tul wt Ctti /g ml -1 Figu 2. ltil u f i 6 ml L -1 HCl.2 KI quu luti lt dditi t th wt mpl. g u: =.1.276C ( 2 = 1); quu luti u: = C ( 2 =.9969); lt dditi u: =.1.271C ( 2 =.9882) Ctti /g ml -1 Figu 3. ltil u f i.12 ml L -1 ti id quu luti lt dditi t th wt mpl. g u: = C ( 2 =.9944); quu luti u: = C ( 2 =.9874); lt dditi u: = -.3.1C ( 2 =.987) Ctti /g ml -1 Figu 4. ltil u f i.4 ml L -1 itt uff luti quu luti lt dditi t th wt mpl. g u: = C ( 2 = 1); quu luti u: = C ( 2 =.9974); lt dditi u: = C ( 2 =.9).

4 PB Quiái & llmg J. Bz. Chm. S. pti 7 ut thi pdu t ud f i piti, it wuld fft th i fm pt. O th th hd td mpl withut tiliti ultd i t duti t it withi fw d 2. Smpl tg t th duti mdi h ppd f piti hwd t pppit t p th wt mpl f i piti, dig t Figu 5-7. i pi tti i ll th duti mdi tudid did t hw igifit hg pid f th d, iditig mpl tilit f t lt thi pid f tim. i pi i ight wt mpl fm difft i (th d th-wt gi f th Pá Stt, d uth gi f th Sã Pul Stt, Bzil) w dtmid uig th lti dtmiti pdu ppd; ll ut tw mpl hwd i ll lw th limit f dtti. Th mpl, lltd d filtd, w udiidd d dfid liqut w djutd t th pp ti mdi (Figu 1). Tiplit l, f h ptiul tm, w pfmd. Th i pi it, t d dimthlit w qutifid th uig quu ltil u d th lt dditi liti mthd d Tl 2 hw th ult tid f th tw mpl. Ttl i it plu t tti w idtil, wht th liti mthd idd, pitd ut th ttitil t tt (p=.95). Th ult fim tht piti tudi i 6. ml L -1 hdhli id, ft pppit p-duti, d impl ltil u fm it tdd; f thi mdium, th dtti limit w.47 µg L F th ptiul i wt mpl ltil igl w dttd i ti id itt uff mdi, ut thi g with th dtti limit fud f th duti mdi 1.5 µg L -1 d.6 µg L -1, ptil d with th diff mg ttl i d th um it plu t. Th ult idit tht t w th pdmit il dild fm f th mpl ld. O th mpl w djutd t th pp ti mdi, ll th piti tud id ut withi l th thit miut, iludig tiplit mumt f h duti tm. Figu 5. Smpl tilit i 6 ml L -1 hdhli id (3. mg /L) (V) Tim / d Figu 6. Smpl tilit i.12 ml L -1 ti id (3. mg L -1 ) DM Tim / d Tim / d Figu 7. Smpl tilit i.4 ml L -1 itt uff (3. mg L -1 ) Tl 2. i Spiti i i Wt Smpl, g ml -1 lt dditi (=3) ltil u (=2) Smpl () () () () () () () () Tigi i 1.5± ±.2.42±.11.76± ±.7.82±.25 Ciz i.87± ±.3.58±.3.95± ±.9.86±.1 () plu (V) () ttl

5 Vl. 12 N. 1, 21 Slti duti f i Spi Hdid Gti 41 Clui Slti duti t difft id mdi llwd th piti tud f i i tul wt, uig it quu ltil u f liti. N itf fft w d i th tudid tul wt mpl, til u th itfig mtlli i ll w lw th itf thhld d l u th pl w pt mplxd pi; thu, th u f impl quu ltil u withut piu pti mkig tp w pil. Th mpl tg t th duti mdi ppd f th lti duti piti ld tg pid f up t d f th difft pi tudid. Th ppd pdu hwd t ut, pi d lw tim umig jut impl mpl ttmt i quid. kwldgmt Th uth thk CNPq f fiil uppt. f 1. d, L. C. D.; Buld, K. W. Ei. Si. Thl. 1991, 25, Lii, L. I Txilgi; Ed. Ml, Sã Pul, Chttj,.; D D.; Mdl B. K.; Chwdhu, T..; Smt, G.; Chkti, D. lt 1995, 12, D, D.; Chttj,.; Mdl, B. K.; Smt, G.; Chkti, D. lt 1995, 12, Sumi, K; Mg, J. C. l. Chim. t 1981, 124, Bwll,. J.; Ml, N. H.; Di, V. K. ppl. Ghm. 1994, 9, Hi, T.. lt 198, 15, Chkti, D.; Djgh, W.; dm, F. l. Chim. t 198, 12, Hkl, E.; P, L. J. l. tm. Spt. 1992, IUPC. Pu ppl. Chm. 1992, 64, gtd, J. l. Chim. t 1987, 197, d,. K.; Thmp, M.; Culd, E. lt 1986, 111, d,. K.; Thmp, M.; Culd, E. lt 1986, 111, Ch, H.; Bidl, I. D.; L, X. l. Chm. 1992, 64, Hgw, H.; Shi, Y.; Mtui, M.; Hj, M.; Kwhim, M. l. Chm. 1994, 66, St, S. J. l. Chim. t 199, 237, Y, X.; Ni, Z. l. Chim. t 1994, 291, Quiái, S. P.; llmg, M. C. E. J. Bz. Chm. S. 1997, 8, Cutiu,. J. Quim. N 1986, 9, Stumm, J.; Hzi, B.; Wippm, T. Fiu J. l. Chm. 1996, 354, 344. id: Ot 13, 1999 Pulihd th w: Ot 13, 2

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