Poster Session, Thursday, June 17Theme F686 - N1123Determ<strong>in</strong>ation of Critical Micelle Concentration (cmc) of PB-b-PEO Diblock Copolymer by TwoDifferent MethodsÖnder TOPEL*, Burç<strong>in</strong> ACAR, Leyla BUDAMA, Numan HODAAkdeniz University Department of Chemistry, Antalya, TurkeyAbstract- Critical micelle concentration (cmc) was measured for PB 1800 -b-PEO 4000 amphiphilic diblock copolymer <strong>in</strong> aqueous solution bytwo different methods. The fluorescent probe technique was utilized with pyrene as a probe molecule, and the <strong>in</strong>tensity of the scattered lightwas used <strong>in</strong> dynamic light scatter<strong>in</strong>g technique. The cmc values obta<strong>in</strong>ed by these two techniques are rather close each other.Micellization of block copolymers is an importantresearch area of colloid science <strong>in</strong> the last few decades.Block copolymers may have a soluble block whichconstitutes corona, and an <strong>in</strong>soluble block whichconstitutes core <strong>in</strong> selective solvents. In these solventsmicelles resemble different morphologies such as sphere,warm-like and lamellar. The self-assembled micelles havefound many applications <strong>in</strong> many areas such as drugdelivery systems, surface modification and viscosity andwater purification.Micelles are observed only above a certa<strong>in</strong> concentrationwhich is the critical micelle concentration (cmc). The cmccan, most conveniently, be def<strong>in</strong>ed as that concentrationbelow which only s<strong>in</strong>gle cha<strong>in</strong>s are present but abovewhich both s<strong>in</strong>gle cha<strong>in</strong>s and micellar aggregates can befound. There are some methods to measure cmc such astensiometry, spectrofluorometry, and dye solubilization [1-3]. DLS (Dynamic Light Scatter<strong>in</strong>g) method is a rathernew method to determ<strong>in</strong>e cmc of diblock copolymermicelles [4]. In this study we report the cmc behavior ofPB 1800 -b-PEO 4000 (Polymer Sources, Canada) <strong>in</strong> aqueoussolution us<strong>in</strong>g two different methods, DLS andfluorometry.cmc1,5A series of block copolymer solutions rang<strong>in</strong>g from1.72x10 -5 -4.31x10 -8 mol/L were prepared from aqueousstock solution of block copolymer PB-b-PEO (2%) whichwas stirred for 24 h at room temperature. These aliquotswere filtered with 0.45μm filter to get rid of largeagglomerates and dusts. The dispersion was filteredthrough a 0.45 mm filter. Size and distribution of themicelles were analyzed by means of a DLS <strong>in</strong>strument(Malvern Zetasizer Nano ZS) with a He-Ne laser beam at awavelength of 633 nm at 25°C and 173° of scatter<strong>in</strong>gangle. The results of DLS measurements are expressed <strong>in</strong>size distribution by <strong>in</strong>tensity.Intensity30025020015010050cmc00 5 10 15 20concentration x 10 7 (mol/L)Figure 2. Plot of concentration vs. DLS <strong>in</strong>tensity10,50-10 -8 -6 -4 -2 0log cI1/I3By plott<strong>in</strong>g concentration vs. <strong>in</strong>tensity data, the cmcvalue is obta<strong>in</strong>ed from the <strong>in</strong>tersection of the two curves(Figure 2). Accord<strong>in</strong>g to DLS results the cmc is found tobe 3.07x10 -7 mol/L. The cmc values by two differentmethods are rather close each other.This work was supported by Akdeniz University TheScientific Research Projects Coord<strong>in</strong>ation Unit underGrant No. 2007.01.0105.007.Figure 1. Plot of the fluorescence <strong>in</strong>tensity ratio I 374 /I 385(from pyrene emission spectra) vs. log cFirst, the critical micelle concentration of copolymer <strong>in</strong>aqueous solution was determ<strong>in</strong>ed us<strong>in</strong>g pyrene as afluorescence probe. The excitation spectra (350-450 nm)of the solutions were recorded with an emissionwavelength of 340 nm with the excitation and emissionbandwidths be<strong>in</strong>g set at 5 nm. The ratios of the peak<strong>in</strong>tensities at 374 and 385 nm (I 374 /I 385 ) of the excitationspectra were recorded as a function of block copolymerconcentration. The cmc value was taken from the<strong>in</strong>tersection of the tangent to the curve at the <strong>in</strong>flectionwith the horizontal tangent through the po<strong>in</strong>t at the lowconcentrations (Figure 1). The cmc of PB-b-PEO diblockcopolymer <strong>in</strong> aqueous solution was estimated to be2.94x10 -7 mol/L by fluorescence spectroscopy.*Correspond<strong>in</strong>g Author:ondertopel@akdeniz.edu.tr[1] Birdi, K. S., 1997. Handbook of Surface and ColloidChemistry. CRC Press, Boca Raton, FL.[2] Dom<strong>in</strong>guez, A., Fernandez, A., Gonzalez, N., Iglesias, E. andMontenegro, L, 1997. Determ<strong>in</strong>ation of critical micelleconcentration of some surfactants by three techniques. J. Chem.Educ., 74 (10): 1227-1234.[3] Nakahara, Y., Kida, T., Nakatsuji,Y. and Akashi, M., 2005.New Fluorescence Method for the Determ<strong>in</strong>ation of the CriticalMicelle Concentration by Photosensitive MonoazacryptandDerivatives. Langmuir, 21; 6688-6695.[4] App. Note: Surfactant micelle characterization us<strong>in</strong>g dynamiclight scatter<strong>in</strong>ghttp://www.malvern.com/common/downloads/campaign/MRK809-01.pdf6th Nanoscience and Nanotechnology Conference, zmir, 2010 673
PPoster Session, Thursday, June 17Theme F686 - N1123Preparation of Anion Exchange Membrane and Its Characterization by AFM and EFM111UZeynep ÇolakoluUP P*, Nilay GizliP P, Mustafa DemircioluP1PDepartment of Chemical Eng<strong>in</strong>eer<strong>in</strong>g, Ege University, Bornova, 35100, zmir, TurkeyAbstract-For the selective removal of arsenic species from water, a heterogeneous anion exchange membrane was prepared onpolyethylene backbone conta<strong>in</strong><strong>in</strong>g quaternized immobilized N-methyl-D-glucam<strong>in</strong>e (NMDG). Surface characterization and electrostaticconductivity of this material were <strong>in</strong>vestigated by atomic force microscopy (AFM) and electrostatic force microscopy (EFM). Roughnessvalues show that materials have no porosity, while positive values of surface skewness (1.398) po<strong>in</strong>t to extreme peaks on the membranesurface and surface kurtosis (2.174) lower than 3.0 to broader height distributions. Characterization of materials by AFM and EFM servedfor both optimization of preparation conditions and improvement of material properties.Safety <strong>in</strong> dr<strong>in</strong>k<strong>in</strong>g water is a challenge by climate change.Arsenic is important due to high toxicity and its high levelssome cities <strong>in</strong> Turkey. Ma<strong>in</strong> forms of arsenic met <strong>in</strong> groundwaters are arsenite or arsenate anions. Therefore theseparation by ion exchange comes as the first alternativemethod for ground waters. Removal performance of arsenicmust be enhanced for a viable <strong>in</strong>dustrial application. The aimof this study is to produce the anion exchange membranesand to characterize them by us<strong>in</strong>g AFM and EFM. Recentstudies show hopeful results <strong>in</strong> the name of us<strong>in</strong>g anionexchange membranes for the purification of water sourcesfrom hazardous ions s<strong>in</strong>ce these membranes have excellentelectrochemical properties [1].In this study, membranes were prepared by aheterogeneous method, <strong>in</strong> which powdered ion exchangeres<strong>in</strong> of NMDG was comb<strong>in</strong>ed with polyethylene, pressedand heated up till 250°C and kept for 10 m<strong>in</strong>. Then themembrane was subjected to morphological andelectrochemical characterization. The surface structure ofmembranes was observed by multimode AFM (RT-SHPM,NanoMagnetics Instruments). The membrane surfaces werescanned by alum<strong>in</strong>ium reflex coated silicon probe (Tap300AI, NanoMagnetics Instruments) hav<strong>in</strong>g the spr<strong>in</strong>gconstant of 40 N/m and the resonance frequency of 300 kHz<strong>in</strong> dynamic mode. Scan area and speed were chosen as210x10 μmP Pand 5 μ/s, respectively.The roughness parameters such as root mean squareroughness (RMS), mean roughness (Ra), average meanheight (Hav), surface skewness (Ssk) and surface kurtosis(Sku) were obta<strong>in</strong>ed by us<strong>in</strong>g built-<strong>in</strong> software SPM 1.16.13.It’s found that surface skewness was positive 1.398 which isalso numerically greater than 1.0 <strong>in</strong>dicates that it has extremepeaks on the surface [2]. Surface Kurtosis was found as2.174 which is lower than 3.0, so the membrane showsbroader height distributions [3]. Imag<strong>in</strong>g by EFM, anotherAFM technique, is used to characterize materials forelectrical properties. In this technique, a conductive AFM tip<strong>in</strong>teracts with the sample through long-range Coulombicforces. These <strong>in</strong>teractions change both oscillation amplitudeand phase of AFM cantilever, which are monitored to createEFM phase image [4]. In this study, the voltage levels werechosen as -4V and +4V for forward and backward potentials.Scan speed of 8μm/s was applied for the samples with the2area of 30 x 30μmP P.Figure 1. AFM and EFM Phase views of membranes.The image at the left <strong>in</strong> Figure 1 is an AFM image onwhich lighter regions show peaks on the sample surface, onEFM image (to the right) lighter regions representconductive areas. Various properties were observed bychang<strong>in</strong>g the parameters such as area scanned, scan speed,applied voltage, head lift, ris<strong>in</strong>g and fall<strong>in</strong>g time <strong>in</strong> order todeterm<strong>in</strong>e the optimum conditions for measurement. As aresult, before delv<strong>in</strong>g <strong>in</strong>to experimental tests andperformance studies requir<strong>in</strong>g large amount of material andlaborious tasks <strong>in</strong> a separation process, characterization ofmaterials by AFM and EFM dur<strong>in</strong>g preparation phase ofthem helps both to screen the alternatives and to optimize thepreparation conditions for the development of novelselective materials and the improvement of their properties.*Correspond<strong>in</strong>g author: HTzeynepcolakoglu@hotmail.comT[1] Punita V. Vyas, B.G. Shah, G.S. Trivedi, P. Ray, S.K.Adhikary, R. Rangarajan, Characterization of heterogeneous anionexchangemembrane, Journal of Membrane Science 187 (2001)[2] J. F. Jørgensen, L. L. Madsen, J. Garnaes, K. Carneiro, K.Schaumburg, Calibration, drift elim<strong>in</strong>ation and molecular structureanalysis, JVST B, 12(3), 1698-1701 (1994)[3] J. F. Jørgensen, N. Schmeisser, J. Garnaes, L. L. Madsen, K.Schaumburg, L. Hansen, P. Sommer-Larsen. (1994) Dynamicsand structure of selfassembled organic molecules at the solidliquid<strong>in</strong>terface, Journal of Surface & Coat<strong>in</strong>g Technology 67, pp.201-11[4] F. M. Serry, K. Kjoller, J. T. Thornton, R. J. Tench, and D.Cook. Electric Force Microscopy, Surface Potential Imag<strong>in</strong>g, andSurface Electric Modification with the Atomic Force Microscope(AFM).6th Nanoscience and Nanotechnology Conference, zmir, 2010 674
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