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{\upr{\title Dugi niz godina tragovi selena(+4) u vodenim otopinama (i prirodnim uzorcima) odredivani su na \'9eivinoj elektrodi katodnom akumulacijom s otapanjem}
{\*\ud\uc0{\title Dugi niz godina tragovi selena(+4) u vodenim otopinama (i prirodnim uzorcima) odre{\uc1\u273 divani su na \'9eivinoj elektrodi katodnom akumulacijom s otapanjem}}}}{\author Marina i Renata}{\operator Marina i Renata}
{\creatim\yr2004\mo2\dy17\hr12\min37}{\revtim\yr2004\mo3\dy15\hr13\min47}{\version31}{\edmins464}{\nofpages4}{\nofwords694}{\nofchars3956}{\*\company IRB}{\nofcharsws0}{\vern71}}\paperw9979\paperh14175\margl1985\margr1418 
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{\pntxtb (}{\pntxta )}}\pard\plain \s15\qc\nowidctlpar\widctlpar\adjustright \fs28\lang1050\cgrid {\b ELEKTROKEMIJSKA REDUKCIJA SELENA(+4) U PRISUTNOSTI RODIJA(+3)
\par }\pard \s15\nowidctlpar\widctlpar\adjustright {
\par }\pard \s15\qc\nowidctlpar\widctlpar\adjustright {\b ELECTROCHEMICAL REDUCTION OF SELENIUM(+4) IN THE PRESENCE OF RHODIUM(+3)
\par }\pard\plain \nowidctlpar\widctlpar\adjustright \lang2057\cgrid {\b\lang1050 
\par }\pard \qc\nowidctlpar\widctlpar\adjustright {\f16\lang1050 MARINA ZELI\'c6
\par }\pard \nowidctlpar\widctlpar\adjustright {\lang1050 
\par }{\f16\lang1050 Zavod za istra\'9eivanje mora i okoli\'9aa, Institut Ru\'f0er Bo\'9akovi\'e6, Bijeni\'e8ka cesta 54, 10000 Zagreb; zelic@rudjer.irb.hr 
\par }{\lang1050 
\par UVOD
\par }\pard \qj\nowidctlpar\widctlpar\adjustright {\f16\lang1050 Dugi niz godina tragovi selena(+4) u vodenim otopinama (i priro- dnim uzorcima) odre\'f0ivani su na \'9eivinoj elektrodi katodnom aku- mulacijom s otapan}{\lang1050 
jem. Akumulirao se (kao prvi produkt elektro- dne reakcije) slabo topljivi HgSe ili Cu}{\lang1050\sub 2}{\f16\lang1050 Se (ako je  otopini dodana dovoljna koli\'e8ina Cu}{\lang1050\super 2+}{\f16\lang1050 
) i mjerio signal koji odgovara redukciji tako stvorenog depozita. Prije desetak godina, me\'f0utim, u jednom je (vrlo optimisti\'e8ki intoniranom) radu [1] opisano mjerenje koje se bazira na (pretpostavljenoj) akumulaciji Rh}{\lang1050\sub 2}{\lang1050 
Se}{\lang1050\sub 3}{\f16\lang1050 . Tako modificirana metoda, zbog visoke je osjetljivosti, djelovala vrlo obe\'e6avaju\'e6e, ali se njena primjena u kasnijoj literaturi spominje samo jednom [2] i to u bitno druga\'e8ijem svjetlu. Umjesto jednog opa\'9e
ena su dva sig- nala, odziv se pokazao vrlo osjetljivim na prisutnost kloridnih iona, a sve je skupa opisano kao neka vrsta kataliti\'e8kog procesa. Direktni dokazi pretpostavljenih elektrokemijskih reakc}{\lang1050 i}{\f16\lang1050 ja, kao ni u prvom slu
\'e8aju, nisu dani, a optimizam je bio mnogo slabije izra\'9een. 
\par U spomenuta dva rada kao najpovoljniji elektroliti spominjale su se otopine sumporne [1] i klorovodi\'e8ne kiseline [2] uz napomenu da su u perkloratnoj sredini rezultati lo\'9aiji. Kako su se raniji vlastiti zaklju\'e8
ci bazirali na voltametrijskim mjerenjima u 0.1 mol/L HClO}{\lang1050\sub 4}{\lang1050  (uz dodatak Cu}{\lang1050\super 2+}{\lang1050  [3] ili bez njega [4]) bilo je zanimljivo utjecaj otopljenog rodija ispitati ba\'9a
 u ovom mediju. Kao tehnika je odabrana pravokutnovalana voltam}{\f16\lang1050 etrija zbog njene osjetljivosti na  karakter elektrodnog procesa i dobro razvijenu prate\'e6
u teoriju. (Spomenuti literaturni rezultati [1,2] dobiveni su uglavnom voltametrijom s linearnom promjenom potencijala.)    
\par }\pard \nowidctlpar\widctlpar\adjustright {\lang1050 
\par }\pard \qj\nowidctlpar\widctlpar\adjustright {\lang1050 EKSPERIMENTALNI DIO
\par Za pripremu otopina kori\'9ateni su Na}{\lang1050\sub 2}{\lang1050 SeO}{\lang1050\sub 3}{\lang1050 \'b7xH}{\lang1050\sub 2}{\lang1050 O, RhCl}{\lang1050\sub 3}{\lang1050 \'b7xH}{\lang1050\sub 2}{\lang1050 0, koncentrirana HClO}{\lang1050\sub 4}{
\f16\lang1050  i redistilirana voda. Svi rezultati dobiveni su na elektrodi tipa stati\'e8na \'9eivina kap (PAR 303) uz platinsku \'9eicu kao protuelektrodu i referentnu Ag/AgCl (zasi\'e6eni NaCl) elektrodu. Polarografski ana}{\lang1050 
lizatori bili su PAR 384B i BAS 100A.
\par 
\par REZULTATI
\par }{\f16\lang1050 Dodatak malih koli\'e8ina Rh(+3) zaista pove\'e6ava osjetljivost metode u usporedbi s rezultatima dobivenim uz Cu(+2) ili bez \ldblquote stranih\rdblquote  metala. Nakon akumulacije dobivaju se dva signala ( na  - 0.75 i   -1.1 V). \'c8
itav odziv sli\'e8an je onom koji se obi\'e8no opa\'9ea pri mjerenjima razli\'e8itih sumpornih spojeva u prisutnosti iona kobalta, nikla, \'9eeljeza ili platinskih metala, \'9ato nije neobi\'e8no kad se uzme u obzir sli\'e8nost izme\'f0
u sumpora i selena. Kod sumpornih spojeva (od }{\lang1050 s}{\f16\lang1050 ulfida do metalotioneina) rezultati se interpretiraju u smislu kataliti\'e8
kih procesa premda ni danas, nakon mnogo godina primjene, ne postoji slaganje o (elektro)kemijskim reakcijama koje iza svega stoje.
\par }{\lang1050 U sustavu Se(+4) \endash  Rh(+3) pozitivniji signal odgovar}{\f16\lang1050 a potpuno ireverzibilnom procesu, \'9ato slijedi iz oblika \ldblquote gornje\rdblquote  i \ldblquote donje\rdblquote  struje u pravokutnovalnoj voltametriji, koje \'e8
ak i pri frekvenciji od 5 s}{\lang1050\super -1}{\f16\lang1050  \ldblquote gledaju\rdblquote  u istom smjeru. Produ\'9eena akumulacija rezultira porastom tog signala i njegovim pomakom prema negativnijim potencijalima \'9ato na prvi pogled upu\'e6
uje na redukciju iz adsorbiranog (ili \ldblquote istalo\'9eenog\rdblquote ) stanja. Ovisnost o koncentraciji selena(+4) u otopini - do 20 nmol/L - nije pravac koji ide kroz ishodi\'9ate ve\'e6 sve skupa djeluje kao dio sigmoidalne kriv}{\lang1050 u}{
\f16\lang1050 lje \'e8iji plato nije dostignut. Negativniji (i vi\'9ai) signal nakon linearnog dijela dosti\'9ee struju zasi\'e6enja ve\'e6 pri koncentraciji od oko 10 nmol/L (pri  frekvenciji od 100 s}{\lang1050\super -1}{\f19\lang1050 
, akumulaciji od 60 sekundi i koncentraciji Rh(+3) od 8 \'ecg/L) \u353\'73}{\lang1050 to je prikazano na }{\f16\lang1050 slici 1. Ovaj tip ovisnosti osim kod adsorpcijskih pojavljuje se i kod kataliti\'e8
kih procesa gdje se ovisnost struja - koncentracija formalno mo\'9ee opisati Langmuirovom izotermom.
\par }\pard\plain \s16\qj\nowidctlpar\widctlpar\adjustright \lang1050\cgrid {Da sve skupa nije nimalo jednostavno vidi se po ovisnosti visine i  potencijal
a obaju vrhova o primijenjenoj frekvenciji. Dok kod pozitivnijeg obje vrijednosti pokazuju sigmoidalnu ovisnost o f, kod negativnijeg struja porastom frekvencije prvo pada gotovo do nule, a zatim ponovo raste. Strogo uzev\'9a
i niti jedna od navedenih ovisnost}{\f16 i ne uklapa se u teoriju premda je sli\'e8an utjecaj brzine na visinu signala  opa\'9een (u voltametriji s linearnom promjenom potencijala) u sustavu cistein \endash  Fe(+2) pri vi\'9a
em pH i negativnijem potencijalu [5]. O\'e8igledno je da se dublji uvid u karakter elektro}{d}{\f16 nog procesa mo\'9ee dobiti samo dodatnim mjerenjima.
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\par }}\dpx0\dpy0\dpxsize6975\dpysize5653\dpfillfgcr255\dpfillfgcg255\dpfillfgcb255\dpfillbgcr255\dpfillbgcg255\dpfillbgcb255\dpfillpat0\dplinehollow}}}}{\lang1050 Slika 1. Ovisnost visine prvog (\u9675\'3f) i drugog signala (\u9679\'3f
) o koncentraciji selena(+4) u otopini
\par 
\par 
\par }\pard\plain \s16\qj\nowidctlpar\widctlpar\adjustright \lang1050\cgrid {\f16 S prakti\'e8ne strane tj. uzimaju\'e6i u obzir mogu\'e6u primjenu metode za odre\'f0ivanje tragova selena u prirodnim uzorcima kao problem se pojavljuje nala\'9e
enje uvjeta pod kojima se ovisnost struje o koncent-raciji mo\'9ee prikazati pravcem kroz ishodi\'9ate. Osim toga, pri vi\'9aim se razinama otopljenog rodija prvi, dobro definirani signal, smanjuje i nestaje. Kod drugog, me\'f0utim, njegov polo\'9e
aj na uzlaznom dijelu osnovne struje donekle ote\'9eava to\'e8no o\'e8itavanje  visine.  
\par }\pard\plain \nowidctlpar\widctlpar\adjustright \lang2057\cgrid {\lang1050 \column LITERATURA:
\par 
\par {\pntext\pard\plain\lang1050\cgrid \hich\af0\dbch\af0\loch\f0 1.\tab}}\pard \fi-360\li360\nowidctlpar\widctlpar\jclisttab\tx360{\*\pn \pnlvlbody\ilvl0\ls1\pnrnot0\pndec\pnstart1\pnindent360\pnhang{\pntxta .}}\ls1\adjustright {\lang1050 
J. Wang and J. Lu, Anal. Chim. Acta 274(1993)219-224.
\par {\pntext\pard\plain\lang1050\cgrid \hich\af0\dbch\af0\loch\f0 2.\tab}}\pard \fi-360\li360\nowidctlpar\widctlpar\jclisttab\tx360{\*\pn \pnlvlbody\ilvl0\ls1\pnrnot0\pndec\pnstart1\pnindent360\pnhang{\pntxta .}}\ls1\adjustright {\lang1050 
B. Lange and C. M. G. van den Berg, Anal. Chim. Acta 418(2000) 33-42.
\par {\pntext\pard\plain\f16\lang1050\cgrid \hich\af16\dbch\af0\loch\f16 3.\tab}}\pard \fi-360\li360\nowidctlpar\widctlpar\jclisttab\tx360{\*\pn \pnlvlbody\ilvl0\ls1\pnrnot0\pndec\pnstart1\pnindent360\pnhang{\pntxta .}}\ls1\adjustright {\f16\lang1050 M. Zeli
\'e6 and M. Branica, Electroanalysis 2(1990) 455-462.
\par {\pntext\pard\plain\f16\lang1050\cgrid \hich\af16\dbch\af0\loch\f16 4.\tab}}\pard \fi-360\li360\nowidctlpar\widctlpar\jclisttab\tx360{\*\pn \pnlvlbody\ilvl0\ls1\pnrnot0\pndec\pnstart1\pnindent360\pnhang{\pntxta .}}\ls1\adjustright {\f16\lang1050 M. Zeli
\'e6, L. Sipos and M. Branica, Croat. Chem. Acta 58(1985)43-55.
\par {\pntext\pard\plain\f16\lang1050\cgrid \hich\af16\dbch\af0\loch\f16 5.\tab}}\pard \fi-360\li360\nowidctlpar\widctlpar\jclisttab\tx360{\*\pn \pnlvlbody\ilvl0\ls1\pnrnot0\pndec\pnstart1\pnindent360\pnhang{\pntxta .}}\ls1\adjustright {\f16\lang1050 
M. Heyrovsky and S. Vav\'f8i\'e8ka, Electroanalysis 11(1999)653-655. 
\par }\pard \nowidctlpar\widctlpar\adjustright {\lang1050 
\par ABSTRACT
\par }\pard \qj\nowidctlpar\widctlpar\adjustright {\lang1033 Electrochemical reduction of selenium(+4) on mercury electrode was studied in the presence of rhodium(+3) using perchloric acid (0.1 mol/L) as a basic electrolyte. At a relatively lo
w rhodium concentration (8}{\f19\lang1033 \'ecg/L) two signals were obtained in square wave voltammetry. They are both higher than the peak, which corresponds to the same solution without rhodium.  
\par }{\lang1033 Atypical dependence of the peak height and potential on square wave frequency, selenium concentration etc. prevents the deeper insight into the character of the electrode processes, which are both  totally irreversible. 
\par From the practycal point of view the problem is current concentration relationship which is (mainly) nonlinear and the corresponding curve(s)  do(es) not pass through the origin.        
\par }}