Separation of Triacylglycerol Species from Interesterified Oils by High-Performance Liquid Chromatography

Using a 1,3-regioselective lipase as a catalyst, soybean oil and olive oil were interesterified with the short-chain triacylglycerol tributyrin (1,2,3-tributyrylglycerol) to produce mixtures of structured triacylglycerols (SL-TAG). The SL-TAG were purified by column chromatography and analyzed by both normal-phase (silica column; NP_SIL) and reversed-phase [octadecyl silane (ODS) column] high-performance liquid chromatography (HPLC). Individual SL-TAG molecular species were detected by evaporative light-scattering detection, and characterized by mass spectrometry. NP_SIL HPLC successfully separated the newly synthesized SL-TAG into two groups of TAG: one composed of one butyryl group and two long-chain fatty acyl groups (from soybean or olive oil); the second was composed of two butyryl groups and one long-chain fatty acyl group. The SL-TAG species were further analyzed by reversed-phase HPLC which gave a more detailed separation of the TAG species present in the two SL-TAG.     

Optimization of the in Situ Transesterification of Grain Sorghum (Milo) DDGS to Fatty Acid Methyl Esters and Fatty Acid Ethyl Esters

Distillers grains and solubles generated from the ethanol fermentation of grains contain acylglycerols (AG) that can be successfully converted to fatty acid methyl esters (FAME) and fatty acid ethyl esters (FAEE), commonly known as biodiesel. However, when grain sorghum (milo) DDGS were used as a feedstock for in situ transesterification (IST) under the previously established optimal conditions for other AG-bearing substrates, the yield plateaued at only 32.2% (corrected in this study to 24.2%). Several IST studies have reported significantly higher conversions of AG-bearing substrates to FAME. Therefore, the goal of this IST study was to improve the conversion of the AG in milo DDGS to FAME and FAEE by varying the temperature of reaction, the concentrations of the base (sodium methylate, NaOMe), volume of methanol and ethanol, and the amount of moisture in DDGS. Methyl tert-butyl ester was also evaluated as a co-solvent intended to improve miscibility and reaction rate. Among these variables, the most effective change was an increase in temperature from 40 to 65 °C. The most successful reaction used a AG:NaOMe:MeOH molar ratio of 1.0:2.6:168.9. Those reaction conditions used 4.8 mmol NaOMe dissolved in 12.6 mL MeOH and resulted in a 79.8% conversion of AG to FAME.     

Control Techniques for Industrial Electrodeposition from Aqueous Solutions

JOM - Over the years, the basic aspects of electrodeposition have remained relatively unchanged. However, the need to make improved and purer metals at a more competitive price is forcing...     

Evaluation of organic additives for use in zinc electrowinning

Organic additives are used extensively in zinc electrowinning to assist in controlling the process. A cyclic voltammetry technique has been developed to provide a rapid, quantitative evaluation of the effectiveness of selected organic additives in minimizing the deleterious effects that impurities, such as antimony, have on zinc deposition. Results have indicated that animal glues are more effective than the other organic additives tested, which included several gums, enzymes, and amino acids, in relation to the current efficiency of zinc production. Of the various animal glues compared in this research, the most effective appeared to have average molecular weights in the 25,000 to 30,000 range. The effects of certain process variables on the test results have also been evaluated; these included the acid concentration of the zinc sulfate solution and the cathode preparation.     

Synthesis of absorbent polymer films made from fatty acid methyl esters,glycerol, and glutaric acid: Thermal,mechanical, and porosity analyses

In previous studies, monoglycerides (MGs) were incorporated into the matrix of poly(glutaric acid–glycerol) films to investigate their effect on the thermal, mechanical, and solvent absorption properties of the resultant films. In this study, the same properties were monitored when fatty acid methyl esters (FAME) were added to the polymer film formulation. Thermogravimetric analysis showed that, while the decomposition profile of the FAME and MG-infused films were different, the final decomposition temperatures were similar for both film types at approximately 400 °C. Degree of branching (DB%) was calculated from nuclear magnetic resonance data and was used to examine the effect of DB% on the mechanical and absorption properties of the films. Experimental results did not show any correlation with DB% and any of the physical, chemical, mechanical, or thermal properties studied. Relative to the poly(glycerol–glutaric acid) control, the incorporation of MG into the polymer matrix resulted in improved % absorption but decreased the mechanical property values. Conversely, adding FAME into the matrix improved the mechanical property values; however, there was no significant change in the % absorption values relative to the control. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47822.     

Identification of Sulfur‐Containing Impurities in Biodiesel Produced From Brown Grease

Fatty acid methyl esters (FAME) from waste grease usually contain higher concentrations of sulfur (S) than allowed to meet the specified quality standard for biodiesel (<15 ppm). Brown grease lipid‐derived FAME was produced and fractionated by two passes through a wiped‐film evaporator (WFE) to produce three fractions: (1) a 120 °C pass distillate, (2) a 170 °C pass distillate, and (3) a heavy residue. Solid phase extraction (SPE) was used to concentrate the S species from the distillate fractions so that they could be detected by a gas chromatography–pulsed flame photometric detector (GC–PFPD) and GC–mass spectrometry (MS). The ethyl acetate and methanol (MeOH) fractions obtained by SPE of the 120 °C WFE distillate and methyl tert‐butyl ether and acetone fractions obtained by SPE of the 170 °C WFE distillate had the highest concentration of S and were, therefore, the best candidates for GC–PFPD analysis. GC–PFPD methods were developed to separate the S species adequately enough for those peaks to be analyzed by GC–MS which matched fragmentation patterns identified by the MS chemical library as tetrahydrothiophenes, dithiolanes, and thiophenes. MS fragmentation patterns were used to identify other, larger, S‐bearing species as sulfides and disulfides cross‐linking between two FAME molecules. The results obtained from this study provide a foundation for developing effective purification methods to remove S‐containing impurities from waste grease‐derived biodiesel.     

Modification of absorbent poly(glycerol‐glutaric acid) films by the addition of monoglycerides

Monoglycerides (MGs) have been incorporated into the matrix of poly(glycerol‐co‐glutaric acid) films to investigate their effect on the thermal, mechanical, and solvent absorption properties of the resultant films. Solvent absorption studies revealed that poly(glycerol‐co‐glutaric acid‐co‐MG) films were able to absorb and resorb solvents better than poly(glycerol‐co‐glutaric acid) films, albeit they had higher erosion levels. Thermogravimetric analysis showed that the incorporated MGs did not affect the thermal stability of the glycerol‐based films. The MG‐incorporated films were observed to be much softer than the poly(glycerol‐co‐glycerol) films which was further proven by a 39‐fold reduction in Young's Modulus and 17‐fold reduction in fracture energy when compared to the poly(glycerol‐co‐glycerol). Mechanical property studies also revealed that the incorporation of MGs increased the elongation % and reduced the tensile strength of poly(glycerol‐co‐glutaric acid) films. Correlation analysis revealed a strong linear relationship between Young's Modulus and fracture energy (R² = 0.9962), and between Young's Modulus and tensile strength (R² = 0.9972). Our study proved that MGs can be successfully incorporated in the polymer matrix of poly(glycerol‐co‐glutaric acid) films to produce softer films with increased elongation and increased solvent absorption capacity. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45381.     

Molecular conjugate-mediated gene transfer into isolated human and transplanted rat kidneys

Technically, renal transplantation has been feasible for over four decades. However, immunological injury to the transplanted kidney continues to be the leading cause of graft loss. While current immunosuppressive protocols yield a 1-year graft survival of > 90%, the trade off is increased risks from nephrotoxicity to manifestations of long-term immunosuppression. We have developed techniques which would allow genetic manipulation of the donor kidney while utilizing current procurement and preservation protocols.