Přiblížení se k absolutním hodnotám molekulových hmotností technických ligninů

Determination of molecular weight parameters of native and, in particular, technical lignins are based on size exclusion chromatography (SEC) approaches. However, no matter which approach is used, either conventional SEC with a refractive index detector and calibration with standards or multi-angle light scattering (MALS) detection at 488nm, 633nm, 658nm, or 690nm, all variants can be severely erroneous. The lack of calibration standards with high structural similarity to lignin impairs the quality of the molar masses determined by conventional SEC, and the typical fluorescence of (technical) lignins renders the corresponding MALS data rather questionable. Application of MALS detection at 785nm by using an infrared laser largely overcomes those problems and allows for a reliable and reproducible determination of the molar mass distributions of all types of lignins, which has been demonstrated in this study for various and structurally different analytes, such as kraft lignins, milled-wood lignin, lignosulfonates, and biorefinery lignins. The topics of calibration, lignin fluorescence, and lignin UV absorption in connection with MALS detection are critically discussed in detail, and a reliable protocol is presented. Correction factors based on MALS measurements have been determined for commercially available calibration standards, such as pullulan and polystyrene sulfonate, so that now more reliable mass data can be obtained also if no MALS system is available and these conventional calibration standards have to be resorted to.Stanovení molekulárních parametrů technického ligninu je založeno na metodě SEC. Nicméně, bez ohledu na použitou techniku, metoda poskytuje značné chyby. Použití SEC s detekcí víceúhlovým rozptylovým fotometrem s infračerveným laserem umožňuje věrohodné a reprodukovatelné stanovené molárně hmotnostní distribuce ligninu. Otázky kalibrace a absorpce UV záření jsou kriticky diskutovány