Hp 5ms ui capillary column

A GC/MS analysis of phthalates was performed on an Agilent 7890B GC in tandem with an Agilent 7000C MS in selective ion monitoring (SIM) mode, according to US EPA method 8270D, with slight modifications. An Agilent HP-5MS UI capillary column (30 m × 0.25 mm × 0.25 μm) was used with 6.0 grade helium (He 99.9999%) as a carrier gas at a flow rate of 1 mL/min. The oven temperature program was as follows: 60 °C for 1.0 min; to 220 °C at 20 °C/min and hold for 1.0 min; to 280 °C at 5 °C/min and hold for 2.0 min. Injection was in split mode (5:1), with an injection volume of 1 μL, an injection port temperature of 280 °C; and an interface temperature of 280 °C in electronic ionization (EI) mode with an electron energy of 70 eV (Table S2).
An appropriate concentration of a standard solution was spiked into each sample to estimate the recovery and the performance of the methods. A procedural blank and a triplicate sample were determined in each batch of samples. PAE concentrations were adjusted for spiked, procedural, and solvent blanks.

Samples were extracted with 100% methanol and centrifuged for 5 min at 4,500 rpm (Centrifuge MiniSpin plus, Germany). The supernatants were characterized by GC–MS without derivatization using an Agilent 7890A GC–MS instrument (Agilent Technologies, United States) equipped with an Agilent HP-5MS UI capillary column (0.25 μm, 0.25 mm × 30 m). The carrier gas was helium, and the flow rate was 2 mL/min. The injector temperature was 260°C, and the G4513A auto-injector was used with 1 µL injections in splitless mode. The oven was preheated to 50°C; the temperature was then elevated to 310°C at a rate of 10°C per minute, for a total of 25 min. The MS intake temperature was set to 260°C, the MS ion source temperature was 230°C, and the interface temperature was 280°C.

Chemical analyses were performed with a TRACE 1310 gas chromatograph (GC), interfaced to an ISQ single quadruple mass spectrometer (MS) (GC-MS, Thermo Scientific, Waltham, MA, USA), and the system was controlled by the Xcalibur 2.2 software. The GC oven was fit with an HP-5 MS UI capillary column (30 m length × 0.32 mm inner diameter × 0.25 μm film thickness, Agilent Technologies, Santa Clara, CA, USA). Sample injection was performed in splitless mode with helium as the carrier gas at a constant flow of 1 ml min⁻¹. Hexane samples (1 μl) were injected by a TriPlus RSH autosampler (Thermo) and SPME samples were manually injected by inserting the fibers into the GC inlet. Specifically for SPME samples, a narrow-bore glass inlet liner (0.75 mm inner diameter) was used to desorb the loaded SPME fibers. The inlet temperature was maintained at 270°C for 65 μm PDMS/DVB, 280°C for 85 μm PA and 100 μm PDMS, 310°C for 85 μm CAR/PDMS, and 320°C for 7 μm PDMS and hexane samples. The GC running of the column oven was programmed from 60°C for 2 min, then ramped at 30°C min⁻¹ to 200°C (0 min hold) and ramped at 5°C min⁻¹ to 320°C with a 10 min hold. The transfer line was set at 280°C and the mass spectrometer was operated in EI mode with a 70 eV ionization energy. Scanning was recorded from 45 to 650 atomic mass units, at a rate of 5 scans/s.

Acetonitrile (0.5 ml) was added to 0.5 ml purified DynF protein (40 mg ml⁻¹) and rotated at room temperature for 2 h. The mixture was centrifuged using a protein concentrator (3000 molecular-weight cutoff; Millipore, Cork, Ireland) at 4000 rev min⁻¹ for 20 min, and the acetonitrile extract (100 µl) was filtered to remove any remaining insoluble debris. Gas chromatography–mass spectrometry (GC-MS) analysis was performed using an Agilent 7890 GC with a 30 m × 250 µm × 0.25 mm HP-5ms UI capillary column and an Agilent G7081B MSD. Helium was the carrier gas at a flow rate of 1 ml min⁻¹. The temperatures of the injector, the interface and the liner were 523 K. Injections of 5 µl were performed in splitless mode. The column temperature was initially 343 K and was held for 2 min, increased to 513 K at 277 K min⁻¹ and run for a total run time of 59.5 min. For GC–MS detection, an electron-impact ionization system was used. The mass range was set to 50–500 m/z with a filament delay of 4 min. The sample-injection volume was 1 µl.

The brittle star hydroalcoholic extract was subjected to the 7890B Agilent Gas Chromatography–Mass Spectroscopy (GC-MS, Agilent Technologies, Santa Clara, CA, USA). Electron ionization (EI) mass spectra (scan range, m/z 50–500, Agilent19091s-443, Agilent Technologies, Santa Clara, CA, USA) were obtained using electrons with an energy of 70 eV, and a filament emission of 0.5 mA. The GC separations were carried out using an HP-5MS UI capillary column ((30 m × 0.25 mm × 0.25 µm) i.d., film thickness 0.5 µm)). Helium was used as the carrier gas (flow: 0.8 mL/min) for EI. The GC oven was programmed with an increase in temperature of 5 °C/min from 80 °C starting 3 min after sample injection, and then held at 250 °C for 10 min. The injection ports of the gas chromatograph, transfer line, and ion source of the 5977MSD were maintained at 240, 250, and 270 °C, respectively. The separated compounds were identified by matching them with the compound data from the National Institute of Standards and Technology (NIST MS database, 2014) library, and the relative (%) amount of each component was measured by comparing its average peak area to the total areas.

Nicotine was collected on a 47 mm Pallflex
Tissuquartz air monitoring
filter (Pall Corporation, Cortland, New York). The filter collection
efficiency of the aerosol on average was ∼85% for both 3rd
and 4th gen devices when comparing the aerosol mass collected and
the total mass loss of the device (Figure. S5). Filters were extracted by sonicating with 5 mL of toluene (≥99.5%,
obtained from Sigma-Aldrich). The filter extracts were diluted by
10 before analysis. Nicotine was separated on an Agilent 6890 gas
chromatograph with an HP5-ms UI capillary column (30 m, 0.25 mm ID,
0.25 μm film, Agilent Technologies Inc., Santa Clara, CA) and
analyzed with an Agilent 5973N mass spectrometer. The injection mode
was splitless with an injection volume of 1 μL, an inlet temperature
at 250 °C, purge flow at 15 mL/min for 1 min. The oven program
was as follows: 70 °C for 2 min, 20 °C/min ramp to 230 °C,
hold for 1 min. Quantification was performed using nicotine analytical
standards (Figure S6).