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1.
Enzyme Microb Technol ; 175: 110409, 2024 Apr.
Article in English | MEDLINE | ID: mdl-38335559

ABSTRACT

The solvent-free esterification of the free fatty acids (FFAs) obtained by the hydrolysis of castor oil (a non-edible vegetable oil) with 2-ethyl-1-hexanol (a branched fatty alcohol) was catalyzed by different free lipases. Eversa Transform 2.0 (ETL) features surpassed most commercial lipases. Some process parameters were optimized by the Taguchi method (L16'). As a result, a conversion over 95% of the FFAs of castor oil into esters with lubricants properties was achieved under optimized reaction conditions (15 wt% of biocatalyst content, 1:4 molar ratio (FFAs/alcohol), 30 °C, 180 rpm, 96 h). The substrates molar ratio had the highest influence on the dependent variable (conversion at 24 h). FFAs/2-ethyl-1-hexanol esters were characterized regarding the physicochemical and tribological properties. Interestingly, the modification of the FFAs with 2-ethyl-1-hexanol by ETL increased the oxidative stability of the FFAs feedstock from 0.18 h to 16.83 h. The biolubricants presented a lower friction coefficient than the reference commercial mineral lubricant (0.052 ± 0.07 against 0.078 ± 0.04). Under these conditions, ETL catalyzed the oligomerization of ricinoleic acid (a hydroxyl fatty acid) into estolides, reaching a conversion of 25.15% of the initial FFAs (for the first time).


Subject(s)
Castor Oil , Fatty Acids, Nonesterified , Hexanols , Esterification , Esters/chemistry , Fatty Acids/chemistry , Lipase/metabolism , Ethanol , Catalysis , Enzymes, Immobilized/chemistry
2.
J Chromatogr Sci ; 47(9): 789-93, 2009 Oct.
Article in English | MEDLINE | ID: mdl-19835690

ABSTRACT

A method developed for the extraction and analysis of polycyclic aromatic hydrocarbons (PAHs) in the asphalt binder using a matrix solid-phase dispersion (MSPD) and gas chromatography is presented. The MSPD method was proposed as a rapid and easy approach to determining PAHs present in the maltenic phase of asphalt binder extracted through a mechanical shaking and sonication of the material. The recovery rates ranged from 62.77-89.92% (shaking) and from 56.54-93.6% (sonication) with relative standard deviations lower than 8.8%. The study shows that the recovery rates using shaking and sonication extractions are not significantly different at the p < 0.05 level. The limits of detection and quantification ranged from 0.7-1.8 mg/kg and 2.2-5.6 mg/kg, respectively. The proposed analytical method was applied to determine PAH levels in an asphalt binder from Brazil. The main PAHs found were BbF, BaP, Per, IncdP, DahA, and BghiP, with average concentrations of 10.2-20.7 mg/kg, but the PAHs Ace and Acy were not detected. However, Nap, Fl, Phen, Ant, Flr, Pyr, Chry, BaA, and BkF were present in average concentrations amounting to less than 10 mg/kg. The results showed that the MSPD method is potentially a valuable tool for the determination of PAHs in the asphalt binder.


Subject(s)
Chromatography, Gas/methods , Hydrocarbons/analysis , Polycyclic Aromatic Hydrocarbons/analysis , Solid Phase Extraction/methods
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