Limited studies have been done on silk fibroins of wild silkworm species owing to their relative insolubility in many solvents. In this study, the solubility of Argema mimosae wild silk fibroin in different salts (LiBr, LiCl, Ca(NO3)2, and CaCl2) dissolved in formic acid under varying temperatures was investigated. The dissolution conditions under which the solubility was optimum were optimized using a central composite design approach. The optimum range for solvation of the fibroin were visualized using contour plots. The influence of temperature and salt concentration were found to significantly influence the solvation of the fibroin. Following the successful dissolution of the fibroin, the regenerated silk fibroin solutions were cast to obtain water insoluble films which were used in investigating optimum electrospinning conditions. Average nanofiber diameters in the 110–141 nm range were obtained under optimum electrospinning conditions. The silk forms were characterized using the FTIR, TGA, XRD, and SEM to understand their properties. The investigations revealed that formic acid—salt solvents were effective in the solvation of the wild silk fibroin. Some of the dissolution conditions induced mild effects on the silk fibroin while others were harsh. Furthermore, processing to nanofibers resulted in the degradation of the β-sheets producing nanofibers rich in α-helices. However, post-treatment using methanol and water vapor were effective in restoring β-sheet crystallinity.
This study aims to compare iso-rank vitrinite-rich and inertinite-rich coal samples to understand the impact of coal-forming processes on pyrolysis chemistry. A medium rank C bituminous coal was density-fractionated to create a vitrinite-rich and an inertinite-rich sub-sample. The vitrinite-rich sample has 83 vol% total vitrinite (mineral-matter-free basis), whereas the inertinite-rich counterpart has 66 vol% total inertinite. The vitrinite-rich sample is dominated by collotelinite and collodetrinite. Fusinite, semifusinite, and inertodetrinite are the main macerals of the inertinite-rich sample. Molecular chemistry was assessed using a pyrolysis gas chromatograph (py-GC) equipped with a thermal desorption unit coupled to a time of flight mass spectrometer (MS) (py-GC/MS) and solid-state nuclear magnetic resonance ( 13 C CP-MAS SS NMR). The pyrolysis products of the coal samples are generally similar, comprised of low and high molecular weight alkanes, alkylbenzenes, alkylphenols, and alkyl-subtituted polycyclic aromatic hydrocarbons, although the vitrinite-rich sample is chemically more diverse. The lack of diversity exhibited by the inertinite-rich sample upon pyrolysis may be interpreted to suggest that major components were heated in their geologic history. Based on the 13 C CP-MAS SS NMR analysis, the inertinite-rich sample has a greater fraction of phenolics, reflected in the py-GC/MS results as substituted and unsubstituted derivatives. The greater abundance of phenolics for the inertinite-rich sample may suggest a fire-related origin for the dominant macerals of this sample. The C 2 -alkylbenzene isomers (p-xylene and o-xylene) were detected in the pyrolysis products for the vitrinite-rich and inertinite-rich samples, though more abundant in the former. The presence of these in both samples likely reflects common source vegetation for the dominant vitrinite and inertinite macerals.
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