A new method for the isolation of lignin in high yield from wood and pretreated wood is presented, avoiding the liquid-solid extraction step of the classical milled wood lignin (MWL) isolation. Dissolved wood lignin (DWL) was obtained by total dissolution of ball milled wood in dimethylsulfoxide and N-methylimidazole (DMSO/NMI) followed by precipitation in dioxane/water in the course of which lignin and carbohydrate fractions were separated. The lignin fraction was purified. High lignin yields and the low number of separation steps belong to the advantages of the described method. DWL lignin was isolated from beech wood (Fagus sylvatica L.) and the sample was compared to MWL obtained by the classical Bjö rkman method. Elemental analyses, methoxyl group content, potassium permanganate oxidation, infrared spectroscopy, and 1D and 2D nuclear magnetic resonance spectroscopy indicated that both lignin preparations are quite similar. However, MWL contained significantly more phenolic hydroxyl groups than DWL. The results indicated that MWL contains higher amounts of smaller fractions with broken b-O-4 linkages than DWL.
In this study, complex coacervates of the biopolyelectrolytes chitosan and gum arabic were investigated with respect to their composition and charge compensation depending on the pH and salt concentration. Individual polyelectrolyte yields were deduced from thermogravimetric analysis and chitosan quantification via enzymatic hydrolysis/HPLC-ELSD. The polyelectrolyte mass ratio in the complex coacervate is found to remain approximately constant irrespective of the pH, despite the latter's effect on the polyelectrolyte charge ratio. Two regimes are identified, including either chitosan charges in excess (at pH < 6.0) or gum arabic charges in excess (at pH > 6.0). The amount of extrinsic charge compensation in the complex coacervates is discussed in detail. We show for the first time that the doping level, a quantity traditionally used to describe salt-induced changes of the charge compensation in polyelectrolyte complexes, is also suitable for the description of pH-induced extrinsic charge compensation in such systems.
The iron complexes of the two diastereomers of N,N′‐ethylene‐bis‐(o‐hydroxyphenylglycine) (EDDHA), racemic (R,R−S,S) and meso (R,S−S,R) were isolated from commercial Fe‐EDDHA fertilizer. Cyclic voltammetry in aqueous solution in the pH range between 4.0 and 11.5 indicated reversible behaviour at both mercury and glassy carbon electrodes and quasi reversible characteristics at a copper electrode. An E1/2 value of −642 mV (racemic diastereomer) and −615 mV (meso form) vs. Ag/AgCl 1 M NaCl reference electrode was observed at pH 9. In unbuffered solutions the complex of the racemic diastereomer shows almost pH independent redox behaviour over the whole pH range studied. The iron complex of the meso isomer hydrolyses at pH values above 9. Diffusion coefficients of the complex species were determined from the voltammograms for the meso isomer and the racemic form with 5.4 10−6 cm2 s−1 and 5.8 10−6 cm2 s−1 respectively. Bulk electrolysis experiments at pH 9 demonstrated the chemical stability of both the FeII‐ and the FeIII‐form of the complex with racemic EDDHA. Good cycling stability and current efficiency were obtained in subsequent charge/discharge experiments using a carbon felt electrode. The redox properties and the stability of FeII/III‐EDDHA complexes make them interesting candidates for future use as negative redox electrolytes in redox flow batteries (RFB).
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