Untreated and treated JP-8 samples were analyzed using two gas chromatographs (6890N, Agilent) equipped with either a pulsed flame photometric detector (PFPD) (5380, O.I Analytical) or a flame ionization detector (FID). Both GCs were equipped with capillary columns (0.32 mm ID, 5 μm film thickness) with non-polar, 100% dimethylpolysiloxane as the stationary phase (CP-Sil 5 CB, Agilent) and autosampler injectors. GC-PFPD analysis was performed with a 60 m long column, while the GC-FID tests were run with a 30 m long column. Helium (UHP, Airgas) was used as the carrier gas, while hydrogen (UHP, Airgas) and air (Zero grade, Airgas) were used as the combustion gases. The inlet temperature was kept at 275 °C and the column temperature was programmed as follows: Hold at 35 °C for 6 min, heat to 170 °C at 10 °C/min, raise the temperature to 300 °C at 20 °C/min and hold at 300 °C for 20 min. The injection volume was 0.05 μL. For the GC-PFPD tests, we used two different split ratios and ranges depending on the total sulfur concentration of the samples. For samples with high sulfur content (above 500 ppmw), we used a 150:1 split ratio and 10 range. For samples with low-sulfur content (lower than 500 ppmw) a 100:1 split ratio and 1 range were used. The PFPD detector was used in the sulfur mode and kept at 250 °C.
Cp sil 5 cb
Manufactured by Agilent Technologies
Sourced in United States
The CP-Sil 5 CB is a capillary column designed for gas chromatography (GC) analysis. It features a 5% phenyl-methylpolysiloxane stationary phase, which provides a medium polarity for the separation of a wide range of analytes. The column dimensions and technical specifications are suitable for use in various GC applications, but a detailed description of its intended use is not available.
Automatically generated - may contain errors
Lab products found in correlation
Cp sil 19cb, by Agilent Technologies (2 mentions)
Supel q plot, by Merck Group (2 mentions)
Delta plus xp irms, by Thermo Fisher Scientific (1 mentions)
Chromback, by Agilent Technologies (1 mentions)
Gc 3800, by Agilent Technologies (1 mentions)
Supelco wax, by Merck Group (1 mentions)
Cp wax 52 cb, by Agilent Technologies (1 mentions)
Carboxen 1010 plot, by Merck Group (1 mentions)
Gc fid, by Agilent Technologies (1 mentions)
Galaxie workstation software, by Agilent Technologies (1 mentions)
Cp 3800 gas chromatograph, by Agilent Technologies (1 mentions)
Fe 2 chloride, by Merck Group (1 mentions)
Gcms qp2010 ultra, by Shimadzu (1 mentions)
11 protocols using cp sil 5 cb
1
Quantifying JP-8 Fuel Components by GC-PFPD
2
GC-MS and GC-C-IRMS Analysis of FAMEs
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FAMEs were analyzed on a gas chromatograph (GC) with flame ionization detector (FID) (HP 6890 series) for concentrations and GC-mass spectrometry (MS) (Finnigan Trace GC Ultra) for identification on a non-polar analytical column (Agilent, CP-Sil5 CB; 25 m x 0.32 mm x 0.12 μm). Samples were injected cold-on-column. The GC oven was programmed from 70‒130°C at 20°C/min and subsequently at 4°C/min to 320°C, at which it was hold for 20 min. The GC–FID was operated at a constant pressure of 100 kPa, whereas the GC–MS was operated at a constant flow of 2.0 mL min-1. The MS was operated in Full Data Acquisition mode, scanning ions from m/z 50–800. The 13C/12C isotope ratios of individual FAMEs were determined by analyzing samples in duplicate on a GC-combustion-isotope ratio mass spectrometer (IRMS) consisting of a HP 6890N GC (Hewlett-Packard) connected to a Delta-Plus XP IRMS via a type-III combustion interface (Thermo Finnigan), using identical GC column and settings as for GC-MS.
Retention times were converted to equivalent chain length (ecl) based on the retention times of C12:0, C16:0, and C19:0 FAMEs. C19:0 FAME was also used to quantify the concentrations of individual FAMEs (μg g-1 DW) [36 ]. The δ13C values obtained by GC-C-IRMS were corrected for the added C atom of the methylation agent. The data were analyzed and plotted in R [37 ] with R-package RLims [36 ].
Retention times were converted to equivalent chain length (ecl) based on the retention times of C12:0, C16:0, and C19:0 FAMEs. C19:0 FAME was also used to quantify the concentrations of individual FAMEs (μg g-1 DW) [36 ]. The δ13C values obtained by GC-C-IRMS were corrected for the added C atom of the methylation agent. The data were analyzed and plotted in R [37 ] with R-package RLims [36 ].
3
Soil Microbial PLFA Extraction and Analysis
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Soil microbial PLFAs were extracted as part of the total lipid extract from subsamples of freeze‐dried, ground organic soil, using a chloroform‐methanol extraction modified from White, Davis, Nickels, King, & Bobbie (1979 ). Identification of PLFAs was carried out on a gas chromatograph (Agilent Technologies 6890) fitted with a CP‐Sil 5CB fused—silica capillary column (50 m × 0.32 mm i.d. × 0.25 μm) and a flame ionization detector. Sample PLFA peaks were identified based on known relative retention times calculated as a proportion of the internal standards (C13—methyl tridecanoate and C19—methyl nonadecanoate [Avanti Polar Lipids, Inc.]). The terminal and mid‐chain branched fatty acids C15:0i, C15:0a, C16:0i C17:0i, and C17:0a were used as indicators of gram‐positive bacteria (Whitaker et al., 2014 ). Cyclopropyl saturated and monounsaturated fatty acids 16:1ω7c, 7,8 cyclic C17:0, C18:1ω7c, and 7,8 cy‐C19:0 were used as indicators of gram‐negative bacteria (Rinnan & Baath, 2009 ). The fatty acids C18:2ω6,9c and C18:1ω9c were taken as indicators of fungi (Kaiser, Frank, Wild, Koranda, & Richter, 2010 ). Total microbial biomass was taken as the total of all identified PLFAs (C14:0, C15:0, C16:1, C16:1ω5c, C16:0, C17:1ω8c, 7Me—C17:0, br17:0, br18:0, C18:1ω5c, C18:0, C19:1 plus those listed above).
4
Alkenone Profiling via GC-FID
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Bands of alkenones extracted from TLC and standard alkenones were analyzed using GC (GC-2014 AFsc, Shimadzu Seisakusho Co., Kyoto, Japan) equipped with FID attached to a capillary column (length, 50 m; internal diameter, 0.32 mm; CP-Sil5 CB; Agilent Technologies Inc., Santa Clara, CA). Helium was used as a carrier at a constant flow rate of 1.25 ml min−1 in split-less mode. Temperature was programmed as follows: 60 °C for 1.5 min, an increase to 130 °C at 20 °C min−1, a further increase to 300 °C at 4 °C min−1 and holding at 300 °C for 25 min.
5
GC-MS Analysis of Organic Compounds
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The GC–MS investigation was performed utilizing a gas chromatograph connected with a VG Analytical 70-250S mass spectrometer (VG Analytical Ltd., Manchester, UK). A fused silica capillary column (CP-Sil 5 CB, 25 m × 0.25 mm i.d., film thickness 0.4 μm, from Chromback, Varian) was the used stationary phase. As a carrier gas, helium was utilized at a flow rate of 1 mL/min. The temperature of the injector was 200 °C. The oven temperature was raised from 80 °C to 270 °C at 10 °C/min, and finally held isothermally for 20 min. An electron impact mode of 70 eV was utilized for the detection with a mass scan range from 35 to 600 amu.
6
Quantitative Analysis of Polysaccharide Composition
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25 µL of 4 mM inositol solution were added as internal standard to 500 µL of purified pellicles. Samples were freeze-dried and submitted to 16 h methanolysis at 80°C with 200 µL of 1 M methanolic-HCl. After evaporation of methanol, samples were re-acetylated by addition of 20 µL anhydrous acetic anhydride and 20 µL pyridine. The resulting N-acetyl methyl glycosides (methyl ester) were dried, converted into their trimethylsilyl derivatives and separated by gas chromatography (GC). The gas chromatograph (Varian GC3800, Les Ullis, France) was equipped with a flame ionization detector, a WCOT fused silica capillary column as stationary phase (Varian CP-Sil 5 CB length 25 m, i.d. 0.25 mm, film thickness 0.25 µm) and helium as gas vector (constant pressure 20 psi). The oven temperature program was: 2 min at 120°C, 10°C/min to 160°C, and 1.5°C/min to 220°C and then 20°C/min to 280°C. Sugar quantification was done by integration of peaks and determination of the corresponding molar values using response factors established with standard monosaccharides. Quantity of each carbohydrate is expressed in molar percentage from derivatization of 1 mg of total sugars and results from the analysis of three pellicles from each strain and a technical duplicate.
7
Optimization of Solid-Phase Microextraction
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IT-SPME was essentially performed as described in our previous works [31 (link),32 (link)]. A GC capillary column (60 cm × 0.32 mm i.d.) as an extraction device was connected between the injection needle and injection loop of the autosampler. The capillary column was threaded through a 1/16 inch polyetheretherketone (PEEK) tube with a length of 2.5 cm long and an inner diameter of 330 μm and connected using standard 1/16 inch stainless steel nuts, ferrules, and connectors. CP-Sil 5CB (100% polydimethylsiloxane, film thickness 5 μm), CP-Sil 19CB (14% cyanopropyl phenyl methylsilicone, film thickness 1.2 μm) (Varian Inc., Lake Forest, CA, USA), Supelco-Wax (polyethylene glycol, film thickness 1.0 μm), Supel-Q PLOT (divinylbenzene polymer, film thickness 17 μm), and Carboxen 1006 PLOT (carbon molecular sieve, film thickness 15 μm) (Supelco, Bellefonte, PA, USA) were used to compare extraction efficiencies. Extraction, desorption, and injection parameters were programmed by the autosampler software (Table S1 ) [31 (link),32 (link)].
8
In-Tube SPME: Optimizing Extraction Efficiency
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In tube, SPME was essentially performed as described in our previous works [24 (link),29 (link)]. A GC capillary column (60 cm × 0.32 mm i.d.) as an extraction device was connected between the injection needle and injection loop of the autosampler. The capillary column was threaded through a 1/16 inch polyetheretherketone (PEEK) tube with a 2.5 cm long, 330 μm inner diameter and connected using standard 1/16 inch stainless steel nuts, ferrules and connectors. Supel-Q PLOT (Supelco, Bellefonte, PA, USA), Carboxen 1010 PLOT (Supelco), CP-Sil 5CB (Varian Inc., Lake Forest, CA, USA), CP-Sil 19CB (Varian), CP-Wax 52CB (Varian), and Quadrex 007-5 (Quadrex Corporation, Woodbridge, CT) were used to compare extraction efficiencies. The control of extraction, desorption, and injection was programmed by the autosampler software (Table S2 ) [24 (link),29 (link)].
9
Quantifying Carbon Tetrachloride by GC-FID
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CCl4 was quantified using a CP 3800 gas chromatograph connected to a flame ionization detector (GC-FID; Varian, Palo Alto, CA, USA). Headspace aliquots (500 μL) were collected from sealed Hungate culture tubes with a gastight 1750 syringe (Hamilton, Franklin, MA, USA) and injected onto the GC column (CP-Sil 5 CB, length 15 m; Varian). Separation of volatile compounds was achieved by isothermal elution at 30 °C for 1 min, followed by a linear temperature gradient (20 °C min−1) up to 220 °C. Injector and detector were maintained at 220 °C (splitless mode) and 300 °C, respectively, with nitrogen (N2) as the make-up gas (Linde Gas). Peak areas were analyzed with Galaxie Workstation software (Varian) and expressed as percentage of CCl4 compared to an abiotic reference tube prepared under the same conditions.
10
Analytical Techniques for Organic Compound Characterization
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GC analyses were carried out on a Varian CP-3800 gas chromatograph equipped with a capillary methylsilicone column (30 m × 0.25 mm × 25 μm) Chrompack CP-Sil 5 CB. NMR spectra were recorded on a Bruker AC300 (300 MHz) spectrometer and were internally referenced to the residual proton solvent signal. HR-MS were acquired with a Thermo Scientific Orbitrap Fusion Mass Spectrometer equipped with an ESI ion source. UV analyses were carried out with HP HEWLETT PACKARD 8453 spectrophotometer. All reagents and solvents were purchased at the highest commercial quality and were used without further purification unless otherwise stated. Fe(CH3CN)2(OTf)2 (−OTf = CF3SO3−) was prepared according to a literature procedure12 (link) from Fe(ii ) chloride (Sigma Aldrich). Solvents were purchased from Sigma Aldrich and used as received.
5-Triisopropylsilyl-pyridine-2-carboxaldehyde11,13 (link) and 5-triisopropylsilyl-2-picolylamine11b were prepared according to literature procedure and spectral data were in accordance with those reported. Menthyl acetate14 (link) and 2,6-dimethylcyclohexanol15 (link) were prepared according to literature procedures and spectral data were in accordance with those reported.
5-Triisopropylsilyl-pyridine-2-carboxaldehyde11,13 (link) and 5-triisopropylsilyl-2-picolylamine11b were prepared according to literature procedure and spectral data were in accordance with those reported. Menthyl acetate14 (link) and 2,6-dimethylcyclohexanol15 (link) were prepared according to literature procedures and spectral data were in accordance with those reported.
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