ࡱ>     5@0lHbjbj22 NXXN~~~  T T T T \ =6 ( 555<<<<<<<$>R0A<5G5^555< O+b=7775  <75<7p7e8:NJ: ;!T 6:g<Tx=0=:,Bu7^B:B:55755555<<dD7"NISKOFREKVENTNA DIELEKTRI NA SPEKTROSKOPIJA POLISTIRENSKOG LATEKSA Tomislav Vuleti*, Bruno Frka-Peteai*+, Magdalena Ujevi**, Silvia Tomi*, Ivan Sondi^ *Institut za fiziku, Zagreb, Hrvatska + Universit Paris 7, Pariz, Francuska ** Hrvatski zavod za javno zdravstvo, Zagreb, Hrvatska ^Institut Rudjer Boakovi, Zagreb, Hrvatska Nisko-frekventna dielektri na spektroskopija (NFDS) prikladna je tehnika za istra~ivanje elektrokinetike nabijenih sustava, polielektrolita i koloida u vodenim otopinama. Kao takova, jedna je od najranije primjenjivanih metoda, a u posljednje se vrijeme sve eae koristi [Nandi et al., Chem. Rev. 100, 2013 (2000); Zoltowski, J. Electroanal. Chem. 443, 149 (1998)]. Kao nerazarajua tehnika omoguava detekciju i kvantifikaciju polarizacijskog odgovora nabijenih sistema, dok se na naboj u sistemu utje e promjenom pH i ionske jakosti elektrolita. NFDS je takoer potvrena tehnika u fizici vrstog stanja, za istra~ivanja kolektivnog elektri nog odziva valova gustoe u niskodimenzionalnim sintetskim materijalima. Niskodimenzionalnost je karakteristika i nabojnih sistema polielektrolita i koloida te smatramo da je mogue povezati naaa saznanja i iskustvo primjene NFDS u fizici vrstog stanja [Pinteri et al. Eur. Phys. J. B 22, 335 (2001)] sa istra~ivanjima meke materije. Povezanost nabijenih sustava u vodenim sredinama i valova gustoe u vrstom stanju, ilustrirana je u: Angelini et al., PNAS 100, 8634 (2003); Tuszynski et al., Biophys. J. 86, 1890 (2004). Kako bismo primijenili NFDS, projektirali smo i izgradili komoru za mjerenje kompleksne vodljivosti tekuih uzoraka (prvenstveno u vodenoj otopini). U odnosu na komore opisane u literaturi [Roldn-Toro i Solier, J. Colloid Interface Sci. 274, 74 (2004); Hollingsworth i Saville, ibid 257, 65 (2003)] ili na komercijalno dostupne (Novocontrol, Njema ka; Agilent, SAD), osnovna je prednost naae konstrukcije mala potrebna koli ina uzorka  50-200 mL te zadr~avanje i pozicioniranje kapljice uzorka kapilarnim efektom izmeu platinskih mjernih elektroda. Mjeriv je raspon vodljivosti od 1-2000 mS/cm. Postignuta je i temperaturna stabilizacija, kontrolnim ureajem kune izrade, do na 10 mK u rasponu 5 - 60 oC. Reproducibilnost mjerene vodljivosti, tj. stabilnost uzorka je u granicama 1.5%, na vremenskoj skali do 2 sata. Ta stabilnost je vie nego dovoljna s obzirom na trajanje eksperimenta, to je izvrsno s obzirom na male dimenzije uzorka. Samo mjerenje izvodi se spajanjem komore na analizator impedancija Agilent 4294A (deklariranog frekventnog opsega 40 Hz - 110 MHz). Frekventni opseg mjerenja je ograni en efektom polarizacije elektroda (pojava elektri nog dvosloja na povraini elektroda), kao i parazitskim impedancijama prisutnim u mjernom krugu. Tehnika oduzimanja eksperimentalno odreene vodljivosti pozadine je, kroz brojna testna mjerenja, omoguila prakti ni mjerni frekventni opseg od 0.5kHz - 50 MHz. NFDS mjerenjima istra~ivali smo suspenzije, u deioniziranoj vodi, monodisperznih (skoro idealno sferi nih) estica polistirena, tzv. lateks. Koloidna stabilnost estica postignuta je njihovim visokim specifi nim povrainskim nabojem. Naime, pri sintezi lateksa [Invitrogen/ Molecular Probes/ Interfacial Dynamics, SAD] povraina je funkcionalizirana karboksilnim (-COOH) skupinama, koje disociraju i ovisno o pH suspenzije generiraju naboj na povraini estica.X   " 8 : < p B ƹƫ}umcu^YT h6 hQ6 hu6h8ZhQ6H*h8Zhy{6h8ZhQ6h8Zh06h8ZhR6 h8ZhU h8Zh;k"hh8ZhQH*hu h8ZhQ h8Zh0jh8ZhU0JU h8ZhRh8Zh0>*h8Zh05CJaJh 5CJaJh?5CJaJh8ZhQ5CJaJ: B j$52D,FTGxh^hgdb$xx`a$gdy$xx`a$gd$a$gda$xx`a$gdQ$xx`a$gdu%$a$gd$a$gdR$dd[$\$`a$gd$dd[$\$`a$gd0 ,FVGjHB D T  X p   T b d r X ^ x ~ ||hQhsq55]hQhsq56]hQhsq5]hQh$^]hQh/e]hQhbyq]hQhQ]hQhq]hQh8Z]hQho] ho]h8Zh8Z]jhD?U\mHnHuh8Zh6 h6 h8Zh0 Ld.48DFHp$0>D^`vĽԹԢԹԏԇԗԏԇhhRhT75hDXhT76hsq5 hQhT7 hQhKhVh{5hVh{6h{ h8Zh{h8Zh{\hbyqhhT7ho h8Zh} h8Zh8Zh8Zho] ho]h8Zh8Z]5DFRd~(:<"NPR^`h"68DFd\h8ZhU\h8ZhY\h8ZhYH*h$^h8ZhYOJQJ h8ZhYhS h_Xh8Zh?OJQJ h8Zh?hQhxhx6hsq5h?h?5hxh{h? h8Zhu%5   Djt >dr x!!!!!!!!Ÿͦ͡yqqyhQhpw\hQhK\hQhD?\hQh'\hQh{\hQhN\ hx\ hN\h8Zh'+\ h'\h hZ(\hZ(h h' h{\ h \ h$^\h8ZhY\ h8ZhY h8ZhUh8ZhU\ h_X\, Takav je lateks izvrsno definiran nabijeni, koloidni sustav, idealan za testiranje primjenjivosti naaeg eksperimentalnog ureaja u istra~ivanjima dielektri ne relaksacije u nabijenim sustavima u vodenoj sredini. No i sama fizika lateksa daje prostora istra~ivanju, budui su originalni radovi u podru ju bili ograni eni u tehnikama eksperimenta i analize podataka [Schwann et al., J. Phys. Chem. 66, 2626 (1962)]. Upravo stoga je lateks potrebno dodatno karakterizirati mjerenjima zeta-potencijala u ovisnosti o pH, radi lociranja izoelektri ne to ke, te mjerenjima koncentracije kationa (prvenstveno Na+) a u svrhu koreliranja s rezultatima NFDS mjerenja.  Povrainski naboj, zajedno sa dobro definiranom atmosferom protuiona, stvara jasan i odrediv polarizacijski odgovor te naposlijetku vodi do pojave dvaju karakteristi nih dielektri nih modova, koje se mo~e dobro opisati poopenom Debye funkcijom. Parametri koji se tako dobivaju iz NFDS mjerenja su jakost relaksacije De i srednje relaksacijsko vrijeme t, kao i parametar koji opisuje airinu distribucije relaksacijskih vremena (povezan sa monodisperznoau lateksa). Vrijeme t se povezuje, preko difuzijske jednad~be L2H"Dt, sa karakteristi nom duljinom L, koju prelazi protuion pri polarizaciji sistema. Shodno tome, niskofrekventni (NF) mod, u kHz opsegu, uspjeano smo korelirali s dijametrom koloidnih estica [Dukhin i Shilov, Adv. Colloid Interface Sci. 13, 153 (1980)]. Naai rezultati ukazuju da taj mod nastaje relaksacijom H+ iona kondenziranih uz povrainu lateksa. Visokofrekventni (VF) mod nije mogue povezati sa modelom O'Briena [O Brien, J. Colloid Interface Sci. 113, 81 (1986)] gdje je karakteristi na duljina moda k-1, Debye-Hckel duljina zasjenjenja u elektrolitu u kojem se lateks nalazi. U naaem lateksu nisu prisutni slobodni anioni, ve samo kationi Na+ i H+, dok su COO- skupine vezane za povrainu koloida, te k-1 nije definiran. Jedna je mogunost da je VF mod posljedica kooperativne relaksacije [Swenson et al., 5th IDMRC, Lille], kada ionske atmosfere (Gouy-Chapman difuzni sloj) lateks estica dolaze u kontakt. Karakteristi na duljina bila bi puno manja od prosje ne udaljenosti estica, kao ato smo i ustanovili za VF mod. Dielektri na jakost za NF mod ovisi o brojnosti protuiona koji sudjeluju u relaksacijskom procesu, za VF mod je ovisna o vjerojatnosti pribli~avanja ionskih atmosfera, veoj za manje lateks estice, gdje je debljina atmosfere usporediva sa dimenzijom estice. Naa je glavni zaklju ak kako u NF modu sudjeluju kondenzirani protuioni, a u VF modu protuioni iz difuznog sloja. Daljnja istra~ivanja usmjerena su ka provjeri gornjeg zaklju ka, i svakako e predstavljati originalan doprinos u podru ju fizike koloidnih suspenzija. Takoer, dosad postignute rezultate smatramo potvrdom primjenjivosti naaeg eksperimentalnog ureaja.  e-mail:  HYPERLINK "mailto:tvuletic@ifs.hr" tvuletic@ifs.hr,  HYPERLINK "http://www.ifs.hr/real_science/" http://www.ifs.hr/real_science/ estice lateksa, skenirajua elektronska mikroskopija, Interfacial Dynamics, SAD kapljica kuiate Koaksijalni konektori Pt !"00V0X0l0x0z0011&1X1p111112222233*3,34363:3<3>33333R44ݽݸ~vqllglb ha] hx] hN] hfRP]hKCJaJhfRPhfRPhfRP5hfRPhfRP]hX,hX,6] hX,] h$^] hK] hpw]h8Zhpw] hpw\hQh$^\hQhN\hQhK\hQh*(p\hQhpw\hQh'\U jhQhO]UmHnHu&444 5"5$5&5(56,666677777777788888809296989:9t9v9x9z9::F:`:t:v:z::::ȶ{h>Th{h9h95h9h_OJQJh]@h]@H*h_h9h95OJQJh9hO]hx hQhK hQhVhV hD?hD?jhO]UmHnHuhKhD?CJaJ hN] ha]hahaH*]-::::::::::;;,;.;2;;;;;;< <z<~<<<<<<<"=$=.=0=4=8=P=R=====N>P>X>Z>j>r>ھڇhhh? 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