Morphological structure was observed by scanning electron microscopy (SEM) (SUPPATM 55, Zeiss, Germany). Fourier transform infrared spectroscopy (FT-IR) spectrum was recorded on an FT-IR spectrometer (Nicolet 710 IR, California, USA). X-ray diffraction (XRD) data was conducted on a Siemens D500 diffractometer (Karlsruhe, Germany). The Magnetic hysteresis loops were studied on a PPMS 9 vibrating sample magnetometer (VSM) (Quantum Design, USA). The GC–MS/MS analysis was carried out on a Thermo Scientific TRACE 1310 gas chromatograph equipped with a Thermo Scientific TSQ 9000 triple quadrupole mass spectrometer with an electron ionization (EI) source, and a TriPlus RSH auto sampler and a split/splitless injector (Thermo Fisher Scientific,Waltham, USA). The operation, data aquisition and data analysis were performed on Chromeleon Software Version 7.2.8. The GC–MS/MS parameters are detailed in Supplementary Material . The molecular structure, GC retention times, optimized mass spectrum parameters and log P of seven PAEs are showed in Table S1 .
Split splitless injector
Manufactured by Thermo Fisher Scientific
Sourced in United States
The Split/Splitless Injector is a key component in gas chromatography (GC) systems. It is designed to introduce liquid samples into the GC column for analysis. The injector can operate in either split or splitless mode, allowing for flexibility in sample introduction and optimization of chromatographic results.
Automatically generated - may contain errors
Lab products found in correlation
D500 diffractometer, by Siemens (1 mentions)
Trace 1310 gas chromatograph, by Thermo Fisher Scientific (1 mentions)
Suppa 55, by Zeiss (1 mentions)
Tsq 9000 triple quadrupole mass spectrometer, by Thermo Fisher Scientific (1 mentions)
Triplus rsh autosampler, by Thermo Fisher Scientific (1 mentions)
Trace gc ultra, by Thermo Fisher Scientific (1 mentions)
Pyridine, by Merck Group (1 mentions)
Polaris q, by Thermo Fisher Scientific (1 mentions)
3 protocols using split splitless injector
1
Analytical Characterization of Phthalate Esters
2
Methyl Esterification of ATB Oil
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The methyl esterification of ATB oil was carried out by alkali catalysis. ATB oil (0.1 mL) was added to the test tube, n-hepatane (2 mL) was added to dissolve the ATB oil, and 0.5% KOH/CH3OH (2 mL) was added to the test tube. The mixture was shaken to make the solution fully react. The reaction was carried out in a water bath at 80 °C for 5–10 min, and the supernatant was taken and subjected to on-board determination. The chemical composition of ATB oil was analyzed with a GC-MS equipped with a quadrupole MS detector, split/splitless injector, autosampler (Thermo Fisher, USA), and an elastic quartz DB-FFAP MS capillary GC column (30 m × 0.25 mm, 0.25 μm). The oven temperature was controlled as follows: held at 70 °C for 1 min, ramped at 10 °C/min to 200 °C, ramped at 5 °C/min to 230 °C, and held for 15 min. The nitrogen carrier gas was maintained at a constant flow rate of 0.4 mL/min. Linear velocity mode was used and set at the rate of 40 cm/s. The injector temperature was set at 230 °C with a split injection ratio of 70:1, and the detector temperature was 230 °C. Electron-impact ionization (EI) mode was used and set to 70 eV. The ion source temperature was 240 °C. The mass scan range was 40–600 amu, retention time was 10 min, and scan mode was full scan. The injection volume was 1 μL, and each sample was injected in triplicate (Figure 1 d).
3
GC-MS Analysis of Trimethylsilyl Derivatives
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An aliquot (ca. 1 mg) of each dry extract was derivatized with 200 µL of bis-(trimethyl) trifluoroacetamide (BSTFA) including 1% trimethylchlorosilane (TMCS) (Sigma-Aldrich, Milan, Italy) and 200 µL of pyridine (Sigma-Aldrich, Milan, Italy) for 2 h at room temperature (RT). The silylating reagent was removed under a nitrogen stream and the sample re-dissolved in 1 mL of nheptane. The GC-MS analysis of the trimethylsilyl derivatives was carried out using a Trace GC Ultra coupled to an ion-trap mass spectrometer detector Polaris Q and equipped with a split/splitless injector (Thermo Scientific, Italy). The column was a Supelco SLB-5ms, 30 x 0.25 mm, 0.1 µm film thickness (Supelco, Sigma-Aldrich, Milan, Italy). Column oven temperature was programmed as follows: 80 °C held for 2 min, up to 280 °C at 10 °C min -1 , held for 10 min, up to 300 °C at 10 °C min -1 and held for 10 min. Helium was used as carrier gas at a flow rate of 1 mL min -1 . The
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