Gc ms qp2010 spectrometer

Gas chromatography–mass spectrometry (GC–MS) analysis was carried out on a GC–MS–QP2010 spectrometer (Shimadzu, Kyoto, Japan) equipped with a fused silica capillary column for the analysis of the degradation products. The temperature program was set to an initial oven temperature of 50 °C, and was increased at a rate of 20 °C min⁻¹ to 700 °C using helium as a carrier gas. The profiles of products with different retention times were gained and the background noise was subtracted. The mass spectrometry of degradation products in samples were obtained by electron ionization at 70 eV, and the data was evaluated by employing total ion count for product identification and quantification. Quantitative analysis of pyrolysis products was performed by the area normalization method [46 (link)].

All chemicals and solvents were purchased from Sigma-Aldrich and Merck unless stated otherwise. Melting points were measured using a Stuart SMP10 melting point device (Bibby Scientific Ltd., Staffordshire, UK) and are uncorrected. ATR-FTIR spectra were recorded on a Shimadzu IRAffinity–1 (Shimadzu Corp., Columbia, USA). The ¹H and ¹³C NMR spectra were run on a BRUKER DPX 400 spectrometer (Bruker, Billerica, USA) operating at 400 and 100 MHz, respectively, using DMSO–d₆ and CDCl₃ as solvents and TMS as internal standard. Elemental analyses were performed on a Thermo Finnigan Flash EA1112 CHN elemental analyzer (Thermo Fischer Scientific Inc., Madison, USA) and the values are within ±0.4% of the theoretical values. The mass spectra were recorded on a SHIMADZU–GCMS–QP 2010 spectrometer (Shimadzu Corp., Kyoto, Japan) with an electronic impact source operating at 70 eV. Thin layer chromatography (TLC) was performed on 0.2 mm pre-coated aluminum plates of silica gel 60 F₂₅₄ (Merck_, Dramstand, Germany) and spots visualized with ultraviolet irradiation. The single-crystal X-ray data were collected in a Diffractometer Bruker D8 Venture (Bruker Daltonics GmbH & Co. KG, Bremen, Germany) at “Centro de Instrumentación Científico y Técnico”, (CICT) in “Universidad de Jaén” (UJA).

All solvent and reagents were obtained from commercial sources and were used without purification. Thin layer chromatography analyses were performed on 0.2 mm pre-coated aluminium plates of silica gel 60 F254 (Merck, Darmstadt, Hesse, Germany). Melting points were taken on a Stuart SMP10 melting point device (Cole-Parmer Ltd., Stone, Staffordshire, UK) and are uncorrected. FTIR spectra were determined on an IRAffinity-1 spectrophotometer (Shimadzu, Columbia, MD, USA). ¹H and ¹³C NMR spectra were measured on a Bruker 400 Ultrashield Avance II spectrometer (Bruker, Billerica, MA, USA) operating at 400 and 100 MHz, respectively, using DMSO-ɗ₆ and CDCl₃ as solvents and TMS as internal standard. Mass spectra were obtained on a Shimadzu-GCMS-QP2010 spectrometer (Shimadzu, Kyoto, Honshu, Japan) equipped with a Rxi-1HT GC Capillary Column (30 m, 0.25 mm ID, 0.25 um df, phase: dimethyl polysiloxane) and operating at 70 eV. Elemental analyses were performed on a Thermo Finnigan Flash EA1112 CHN elemental analyzer (Thermo Fischer Scientific Inc., Madison, WI, USA) and the values are within ±0.4% of the theoretical values.