J w gc db 5 ms column

HMF content and yield were determined with a GC/MS-QP 2010/AOC 5000 AUTO INJECTOR/Shimadzu Gas Chromatograph/Mass Spectrometer equipped with a 30 m Agilent J&W GC DB-5 MS column. Direct insertion spectra were measured at 70 eV. Quantitative analyses were performed on a Shimadzu GC-2010 gas chromatograph equipped with a flame ionization detector^{37 (link)}. ¹H- and ¹³C-NMR spectra were recorded on Bruker Avance 400 Spectrometers^{37 (link)}. All reactions were monitored by TLC using Silica Gel 60 F 254 on aluminum. The chromatograms were visualized by UV light or by using the ethanolic vanillin developing agent^{37 (link)}. The purification of the products was made by chromatographic column flash chromatography using a mixture of hexane/ethyl acetate in a 9/1 proportion as eluent^{37 (link)}. The MW reactions were carried out in 10 mL G-10 vials of an Anton Paar single-mode MW synthesis reactor Monowave 300, powered by an 850 W magnetron, and equipped with temperature sensor and magnetic stirring.

SEM micrographs were performed on a Zeiss VEVO 50, EDS analyses with an IXRF Systems 500. XRD patterns were collected in a RIGAKU diffractometer at 30 kV and 20 mA using CuK_α radiation. DTA was carried out using a Perkin Elmer 1700 analyzer. The infrared spectra of solid samples were recorded as KBr pellets in the 4000–400 cm⁻¹ range on a Varian 640 spectrometer operating in the FT mode. Esters contents and yields were determined with a GC/MS-QP 2010/AOC 5000 AUTO INJECTOR/Shimadzu Gas Chromatograph/Mass Spectrometer equipped with a 30 m Agilent J&W GC DB-5 MS column. Direct insertion spectra were measured at 70 eV. Quantitative analyses were performed on a Shimadzu GC-2010 gas chromatograph equipped with a flame ionization detector. ¹H- and ¹³C-NMR spectra were recorded on Bruker Avance 400 and Avance 500 Spectrometers. All reactions were performed under atmospheric pressure and were monitored by TLC with Silica Gel 60 F 254 on aluminum; the chromatograms were visualized by UV or using the ethanolic vanillin developing agent. Silica gel (Merck 230–400 mesh) was used for purification of products by flash column chromatography using hexane and ethyl acetate (9:1) as eluent.