ÐÏà¡±á>þÿ :<þÿÿÿ9ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿì¥Á`ð¿rbjbjæ‡æ‡ 4"„í„íI (ÿÿÿÿÿÿ¤¶¶¶¶^^^ršššš¶rg(2ÞÞÞÞÞ½½½þ'((((((™)h,â(!^¹½(¶¶ÞÞÛ!(¸¸¸4¶Þ^Þþ'¸þ'¸¸ª²$Ê ”^n&ÞÒ`Ÿ"Çš@Lº%Â&<7(0g(Ì%¢ã,Œã,$n&ã,^n&T½0í"¸+á½½½((œ½½½g(rrrv$rrrvrrr¶¶¶¶¶¶ÿÿÿÿINTERLABORATORY CROSSOVER STUDY AND VALIDATION OF SEC METHOD T.Tomi1, N.Uzorinac Nasipak1, N. `egudovi1, A. Juki2 1 INA d.d, Lovin ieva bb, 10000 Zagreb, Croatia 2 Faculty of Chemical Engineering and Technology, Maruliev trg 19, 10000 Zagreb, Croatia The size-exclusion chromatography (SEC) is a liquid chromatographic technique in which, ideally, molecules are separated according to their size in corresponding solutions. SEC is an irreplaceable technique in characterization and molecular mass distribution determination (MMDD) of polymers. As in all chromatographic techniques, separating columns are the "heart" of the SEC system and they dictate the measured efficiency, as well as accuracy. The choice of column packing depends on the analytical or preparative purpose of separation. Better column efficiencies and separations are obtained with small particle packing and solutes having high diffusion rates. Pore size is one of the most significant parameters to be considered, since it dictates the range of molecular mass (MM) separation [1]. For separating sample components that extend over more than two decades of MM a set of bimodal pore size or multimodal pore size distribution columns (mixed gel columns) are the most desired. Even though SEC has been applied in polymer characterization for a long period of time, the method can show a lack of interlaboratory consistency, as results obtained in one of the IUPAC Round Robin Tests have shown [2]. The aim of this work was to make an interlaboratory crossover study and validation of SEC method. For this purpose measurements were done in two different laboratories, on three different types of equipment, on three different column sets covering nominal MM separation range 103 – 107 Da. Samples of PS standards with narrow or wide MM distribution, as well as commercial polystyrene and other (co)polymer were used for these measurements. A number of validation parameters was defined: repeatability of measurements, repeatability of the standards preparation, intermediary precision, accuracy, selectivity. Based on the criteria of acceptability, validation values were within the tolerance range leading to the conclusion that the method was acceptable for polymer characterization. However, the relationship between MM and column porosity ranges used in characterization has to be taken into account. [1] W.W.Yau, J.J.Kirkland, D.D.Bly; Modern size-exclusion liquid chromatography, John Willey & Sons, 1997. 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