Fast and simple method for determination of fatty acid methyl esters (FAME) in biodiesel blends using X-ray spectrometry

The determination of fatty acid methyl esters (FAME) in diesel fuel blends is an important aspect of production and blending process as well as quality control of distribution operations. In this study, energy-dispersive X-ray fluorescence spectrometer (EDXRF) is used for the first time for determination of FAME in biodiesel blends. The principle of the method is based on intensity difference of X-ray radiation scattered from hydrocarbons and from FAME. The experiment shows that coherent and incoherent radiation, commonly applied for evaluation of the average atomic number of the sample with light matrix, cannot be applied for FAME determination. However, the application of scattered continuous radiation gives excellent correlation between FAME concentration and intensity of scattered radiation. The best results are obtained if continuum is collected in the range of energy between 10.5 and 15.0 keV for rhodium X-ray tube, operated at 35 kV. Linear relationship between the FAME concentration and the inverse of scattered continuous radiation is obtained with the correlation coefficients of 0.999. Standard deviation of measurement is ca. 0.46% (v/v) of FAME and detection limit is 1.2% (v/v) for 600 s counting time and 50% dead-time loss using Si-PIN detector. The investigation shows that crucial issue in determination of FAME in biodiesel blends using EDXRF spectrometer is the precision of measurements resulting from the counting statistics. Therefore, much better results (0.20% (v/v) standard deviation and 0.52% (v/v) detection limit) can be expected if higher intensity of primary radiation is applied and X-ray spectrum is collected by silicon drift detector of high input count rate. For concentration of FAME from 10 to 100% (v/v), the differences between reference method (Fourier transform infrared spectrometry) and the proposed method usually do not exceed 1% (v/v) of FAME. The proposed method is fast, simple and enables FAME determination in wide range of concentration up to 100% of FAME without any sample treatment.     

Synthetic studies on dicyclopenta[a,d]cyclooctane terpenoids: construction of the core structure of fusicoccins and ophiobolins on the route involving a Wagner-Meerwein rearrangement

The total diastereoselective synthesis of dicyclopenta[a,d]cyclooctane core skeleton of tricyclic terpenoids, fusicoccins, and ophiobolins is reported. The synthesis commences from 2-methylcyclopent-2-en-1-one and leads first to the easily accessible intermediary cyclopenta[8]annulene 18. The subsequent steps include two key transformations: shifting the angular methyl group from the angular to the neighboring position employing a carbocationic rearrangement (26 → 28) and construction of a quaternary stereogenic center via alkylation of α-methylcyclooctanone intermediate (38 → 48). In the context of the latter transformation, a series of model experiments on alkylation of 2-methylcyclooctan-1-one were conducted. The stereochemical assignments were verified by X-ray analyses of the key structures 39 and 50.     

Application of Levan-Rich Digestate Extract in the Production of Safe-to-Use and Functional Natural Body Wash Cosmetics

The study focused on the evaluation of the possibility of using a levan-rich digestate extract in the production of safe and functional body wash cosmetics. Model shower gels were designed and formulated on the basis of raw materials of natural origin. Prepared prototypes contained various extract concentrations (16.7; 33; 50%). A gel without extract was used as a reference. The samples were evaluated for their safety in use and functionality. The results showed that the use of high-concentration levan-rich digestate extract in a shower gel resulted in a significant reduction in the negative impact on the skin. For example, the zein value decreased by over 50% in relation to the preparation without the extract. An over 40% reduction in the emulsifying capacity of hydrophobic substances was also demonstrated, which reduces skin dryness after the washing process. However, the presence of the extract did not significantly affect the parameters related to functionality. Overall, it was indicated that levan-rich digestate extract can be successfully used as a valuable ingredient in natural cleansing cosmetics.     

Direct Synthesis of Double Hydrophilic Statistical Di‐ and Triblock Copolymers Comprised of Acrylamide and Acrylic Acid Units via the MADIX Process

Double hydrophilic statistical, diblock and triblock copolymers comprised of acrylamide and acrylic acid units have been synthesized in aqueous medium using the MADIX process. Starting from an either monofunctional or difunctional xanthate, the resulting AB and ABA‐type double hydrophilic block copolymers (DHBC) exhibited molar masses predetermined by the initial monomer/xanthate precursor molar ratio and polydispersity indices in the range 1.2–1.5. Batch copolymerizations yielded well‐defined statistical copolymers that were chain‐extended for the synthesis of novel poly‐ (acrylic acid‐stat‐acrylamide)‐block‐polyacrylamide DHBC.