IR was carried out on an EQUINOX 55 spectrometer in the range from 4,000 to 400 cm–1. The solid samples were grounded with dried KBr powder and compressed into a disk prior to analysis. 1H NMR and 13C NMR spectra were acquired on a Unity Inova 600 at 50°C using DMSO‐d6 as solvent and tetramethylsilane as internal standard. The quantitative analysis of the reaction product was performed on a LC‐100 PLUS HPLC equipped with reversed‐phase Novapak‐C18‐100 silica column (4.6 × 150 mm, 4 μm) and UV detector. The mixture of acetonitrile: 1 wt% phosphoric acid solution (12:88, V/V) was employed as mobile phase at the flow rate of 1.2 ml/min with column temperature at 32°C. The product was also qualitatively analysis by LC‐HRMS and GC‐MS. LC‐HRMS was performed on a UFLC‐20A high‐performance liquid chromatography (Shimadzu) and AB SciexTripleTOF 5,600 mass spectrometer equipped with an Agilent XDB‐C18 (2.1 × 100 mm, 3.5 μm). GC‐MS was performed on a Varian 450 GC‐320 MS equipped with a VF‐5 MS capillary column (30 m × 0.32 mm × 0.25 μm).
Vf 5ms capillary column
Manufactured by Agilent Technologies
Sourced in United States
The VF-5ms capillary column is a high-performance fused silica column designed for gas chromatography analysis. It features a 5% phenyl-95% dimethylpolysiloxane stationary phase, which provides good separation for a wide range of organic compounds. The column is inert, thermally stable, and suitable for a variety of applications.
Automatically generated - may contain errors
Lab products found in correlation
7890a gas chromatograph, by Agilent Technologies (2 mentions)
450 gc 320 ms, by Agilent Technologies (1 mentions)
Xdb c18, by Agilent Technologies (1 mentions)
450 gc chromatograph, by Agilent Technologies (1 mentions)
Gc 2030, by Shimadzu (1 mentions)
Gcms qp2020nx, by Shimadzu (1 mentions)
Varian cp 3800, by Agilent Technologies (1 mentions)
Chloroform, by Merck Group (1 mentions)
Hplc system, by Bio-Rad (1 mentions)
Gc cp3800, by Agilent Technologies (1 mentions)
Rxi 5sil ms capillary column, by Restek (1 mentions)
Mps 2xl, by Gerstel (1 mentions)
5975c mass selective detector, by Agilent Technologies (1 mentions)
6890 gas chromatograph, by Agilent Technologies (1 mentions)
5973n mass selective detector, by Agilent Technologies (1 mentions)
7683b automatic liquid sampler, by Agilent Technologies (1 mentions)
17 protocols using vf 5ms capillary column
1
Characterization of Organic Reaction Product
2
Fatty Acid Methyl Ester Analysis in Bacteria and Worms
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Analysis of fatty acid methyl esters (FAMEs) in bacteria and worms was performed as previously described with minor modifications [17] (link). For bacteria, 3 mL of an overnight culture was centrifuged and the bacterial pellet collected. For worms, 50 gravid adults were picked into S-basal, washed in 3 volumes of S-basal, and snap frozen in a 10 µL volume. To generate FAMEs, samples were re-suspended in 1 mL methanol containing 2.5% H2SO4 in glass tubes and incubated in a water bath at 80°C for 1 h. After addition of 1.5 mL water and 200 µL hexane, the samples were vortexed twice for 1 min and the hexane layer transferred to a glass vial until analysis.
1 µL FAMEs in hexane were analyzed using an Agilent 7890A GC 240 MS ion trap system operating in split mode (split ratio 10∶1) with a VF-5ms capillary column (30 m×0.25 mm i.d., 5% phenyl-95% methyl polysiloxine, 0.25 µm film thickness; Varian, Inc., Walnut Creek, CA). The GC conditions were: injector 240°C, initial column temperature 120°C for 0.1 min, temperature ramp 15°C per min to 190°C, 2°C ramp to 220°C, 20°C per min to 250°C, 7 min hold, with a flow rate of 1.1 mL/min. FAMEs were analyzed in EI mode and data were collected using Agilent MS workstation software system control version 7.0.0.
1 µL FAMEs in hexane were analyzed using an Agilent 7890A GC 240 MS ion trap system operating in split mode (split ratio 10∶1) with a VF-5ms capillary column (30 m×0.25 mm i.d., 5% phenyl-95% methyl polysiloxine, 0.25 µm film thickness; Varian, Inc., Walnut Creek, CA). The GC conditions were: injector 240°C, initial column temperature 120°C for 0.1 min, temperature ramp 15°C per min to 190°C, 2°C ramp to 220°C, 20°C per min to 250°C, 7 min hold, with a flow rate of 1.1 mL/min. FAMEs were analyzed in EI mode and data were collected using Agilent MS workstation software system control version 7.0.0.
3
Pyrolysis and GC-MS Analysis of h-BN
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A Pyroprobe 5000 pyrolyzer (CDS analytical, Oxford, PA, USA) was used to pyrolyze the different h-BN samples under helium. This pyrolyzer used an electrically heated platinum filament. The samples (<1 mg) were introduced in a quartz tube between two pieces of rockwool and were pyrolyzed using a coil probe. The samples were heated at 600 °C for 15 s, and the gases were then drawn by the GC for 5 min. The pyrolyzer was interfaced to a 450-GC chromatograph (Varian) by means of a transfer line heated at 270 °C. In the GC apparatus, the initial temperature of 70 °C was raised to 310 °C at 10 °C/min. The column used was a Varian VF-5ms capillary column (Paris, France) (30 m × 0.25 mm; thickness of ¼ 0.25 μm). Helium was used as the carrier gas (1 l/min), and a split ratio of 1:50 was chosen for the analyses. The gases were introduced from the GC to the 240-MS mass spectrometer (Varian, Paris, France) through the direct-coupled capillary column.
4
Characterization of Organic Compounds by FT-IR and GC-MS
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Attenuated total reflectance FT-IR spectra were recorded using an FT-IR Shimadzu IR-8000 spectrophotometer. The spectral range collected was 400–4000 cm−1 with a spectral resolution of 4 cm−1 using 100 scans.
GC-MS analyses were performed using a Varian system GC/MS Saturn 2100 equipped with a VF-5MS capillary column (30 m × 0.25 mm i.d., 0.25 μm). The spectrometer operated in electron-impact mode with ionization energy of 70 eV, the scan range was 40–400 amu, the scan interval was 0.5 sec, and the scan speed was 1000 amu sec−1. The injector and MS transfer line temperatures were set at 250 and 280 °C, respectively. Pure helium was used as the carrier gas at a flow rate of 1 mL min−1. The GC programmer used was 60 °C (5 min) to 180 °C (5 min) at a rate of 8 °C min−1 and to 280 °C (10 min) at 6 °C min−1. Two μL of the diluted samples (n-hexane) were injected in split mode 1:10. Identification of components was achieved by using the stored mass spectra libraries NIST and Wiley and literature data and by comparing their retention indices with published data. The relative quantity of the chemical compounds present in each sample was expressed as the percentage based on their peak area in the chromatogram. The percentage values are the mean ± SD (Standard Deviation) of three injections of the sample.
GC-MS analyses were performed using a Varian system GC/MS Saturn 2100 equipped with a VF-5MS capillary column (30 m × 0.25 mm i.d., 0.25 μm). The spectrometer operated in electron-impact mode with ionization energy of 70 eV, the scan range was 40–400 amu, the scan interval was 0.5 sec, and the scan speed was 1000 amu sec−1. The injector and MS transfer line temperatures were set at 250 and 280 °C, respectively. Pure helium was used as the carrier gas at a flow rate of 1 mL min−1. The GC programmer used was 60 °C (5 min) to 180 °C (5 min) at a rate of 8 °C min−1 and to 280 °C (10 min) at 6 °C min−1. Two μL of the diluted samples (n-hexane) were injected in split mode 1:10. Identification of components was achieved by using the stored mass spectra libraries NIST and Wiley and literature data and by comparing their retention indices with published data. The relative quantity of the chemical compounds present in each sample was expressed as the percentage based on their peak area in the chromatogram. The percentage values are the mean ± SD (Standard Deviation) of three injections of the sample.
5
Preen Oil Extraction and GC-MS Analysis
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All samples were first defrosted and then extracted by adding 500 µl of dichloromethane as a solvent to the vials containing the microcapillary and the preen oil. After briefly vortexing each sample, we transferred 100 µl of the solution (preen oil and dichloromethane) into a glass vial (2 ml, Rotilabo®) containing a 100 µl glass inset, using a blunt point glass syringe (which was washed with dichloromethane between each sample). For chemical analyses, we performed GC-MS, using a gas-chromatograph (GC-2030, Shimadzu, Kyoto, Japan) equipped with a VF-5ms capillary column (30 m × 0.25 mm ID, DF 0.25, 10 m guard column, Varian Inc., Lake Forest, CA, USA) and helium (at a 1 ml/min flow rate) as a carrier gas, coupled to a mass spectrometer (GCMS-QP2020NX, Shimadzu) in split (1/10) mode. The settings for the gas chromatography were as follows; injection temperature: 310 °C, starting temperature: 150 °C, followed by an increase in temperature of 20 °C per min until reaching 280 °C, followed an increase of 5 °C per minute until reaching the end temperature of 310 °C, which was kept for 20 min. For the mass spectrometry, ion source temperature was set at 230 °C and interface temperature at 310 °C. Seven GC blank samples (containing dichloromethane only) were analysed among the preen oil samples.
6
Soy Sauce Volatiles Identification
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The soy sauce samples (5 mL) were extracted three times via head-space solid-phase micro-extraction (50/30 μm DVB/CAR-PDMS) at 45°C for 30 min in a water bath. The gas chromatograph mass spectrometer (Varian, Walnut Creek, CA, United States) was equipped with a VF-5-ms capillary column (30 m × 0.25 mm, 0.25 μm). The experimental procedure and mass spectra comparison of gas chromatography-mass spectrometry was explored previously (Zhao et al., 2015 (link)). 2-octanol was used as the internal standardization in this study.
7
Comprehensive PAHs Analysis in Fish Muscle
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Concentrations of 51 non-substituted and methylated PAHs in fish muscle samples collected at Y5, E4, and A3 were determined as described [32 (link)] using a Varian 3800 GC/Saturn 4000 ion trap mass spectrometry (GC–MS) equipped with a 30 m Varian VF-5 ms capillary column (i.d.: 0.25 mm, film thickness: 0.25 μm) under the selected ion monitoring mode. Perdeuterated PAH surrogates (d8-napthalene, d10-fluorene, d10-fluoranthene, d12-perylene) were added to the procedural blanks, whereas d10-acenaphthene, d10-phenanthrene, d12-benz[a]anthracene, d12-benzo[a]pyrene, and d12-benzo[g,h,i]perylene were used as internal standards and added to each sample prior to analysis. The method detection limits (MDLs) and recoveries of each PAH are listed in Additional file 1 : Table S3, whereas PAH levels were not corrected for surrogate recoveries.
8
Quantification of Sterols in Plant-Derived Oils
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The unsaponifiable fraction was extracted from PSO with diethyl ether, dried, and dissolved in chloroform as described by Lukić et al. (2013) [21 (link)]. Identification and quantification of sterols were carried out by capillary gas chromatography on a Varian 3350 GC (Varian Inc., Harbour City, USA) equipped with a VF-5 ms capillary column (30 m × 0.25 mm × 0.25 μm) and FID. Injector, oven, and detector temperatures were 280, 260, and 290°C, respectively, for 40 min. One μl was injected in split mode (1 : 50). Helium was used as a carrier gas with a flow rate of 1.27 ml/min. Thirteen sterols (cholesterol, brassicasterol, 24-methylene-cholesterol, campesterol, campestanol, stigmasterol, Δ7-campesterol, Δ5,23-stigmastadienol, clerosterol, β-sitosterol, sitostanol, Δ5-avenasterol, and Δ5,24-stigmastadienol) were identified in oil based on their relative retention times with respect to the internal standard, cholestanol, according to the standardized reference method (EEC, 1991, Annexes V and VI). Relative amounts were expressed as proportions (%) of total sterols.
9
PHA Composition Analysis by GC
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To evaluate the PHAs composition, the lyophilized cells were suspended in acidified methanol containing 3% v/v H2SO4 and an equal volume of chloroform (purity ≥99.8%, Sigma-Aldrich, St. Louis, MO, USA). They were then incubated in the oven (Memmert Type SM 400, Memmert, Schwabach, Germany) for 20 h at 100 °C for esterification. The obtained methyl esters were quantified according to the method described by Furrer et al. (2007) (link) using gas chromatography (Varian CP-3800; Varian, Santa Clara, CA, USA) equipped with a Varian VF-5 ms capillary column (30 m × 0.25 mm, film thickness 0.25 μm). Known quantities of pure 3-hydroxyacids (Larodan, Solna, Sweden) were used as standards. The flame ionization detector temperature was 270 °C with the injection port temperature of 250 °C. Initial column temperature was set to 80 °C and next raised with a rate of at 10 °C/min to 240 °C. Total time for analysis of one sample amounted to 16 min.
10
Catalytic Fructose Conversion to 5-HMF
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15 mL Ace pressure tubes were charged with 2 mL PG with hydrophobized aminated silica or Janus A–B. Fructose or 5‐HMF dissolved in the aqueous phase were added to the pressure tubes and the PEs were prepared via emulsification for 1 min at 10 krpm using an IKA UltraTurrax with an S25N 10G dispersing tool. The PEs were left for reaction at 100 °C without stirring for the applied reaction time. After the reaction time was complete, the mixture was cooled to room temperature in air and 1 mL of citric acid solution was added (15 mg mL−1) and the PE was destabilized by centrifugation using a Rotina 38‐R Hettich centrifuge (11000 rpm, 4 °C, 10 min). The aqueous phase was analyzed by HPLC analysis performed on a Shimadzu HPLC system equipped with a Bio‐Rad Aminex HPX‐87H column, and a differential refractometer using citric acid as internal standard. The organic phase was analyzed on a Varian GC equipped with a VF‐5 ms capillary column and an FID detector.
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