The total amount of Zn was measured in each tested solution (ZnCl2, Zn-t CNS, CNS only and ASW), at time zero (T0) (soon after preparation) and after 24 h (T24h), as follows: 10 L of mussels’ exposure water was removed from each tank, placed in polyethylene plastic tubes and stored at 4 °C. Analysis was performed by ICP-MS using the Perkin Elmer NexION 350 spectrometer (Waltham, MA, USA). The analytical accuracy was checked through the determination of Zn(II) concentration in SLRS-6 (river water certified reference materials for trace metals and other constituents) and CASS-4 (nearshore seawater certified reference materials for trace metals and other constituents) of the National Research Council of Canada. Analytical precision was evaluated by means of the percentage relative standard deviation (% RSD) of five replicate analyses of each exposure water sample. Zn levels were expressed as mg L−1. Variations in pH in exposure waters were also recorded at time zero and after 24 h.
Nexion 350 spectrometer
Manufactured by PerkinElmer
Sourced in United States
The NexION 350 is an inductively coupled plasma mass spectrometer (ICP-MS) from PerkinElmer. It is designed to perform high-performance elemental analysis, providing accurate and reliable measurements of trace-level elements in a variety of sample types.
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5 protocols using nexion 350 spectrometer
1
Determining Zinc Levels in Mussels' Exposure Water
2
Elemental Analysis of Plant Samples
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The samples (250 mg of dry weight material) were mineralized with a mixture of 3 mL of 70% HNO3 and 1 mL of 30% H2O2 in a microwave digestion system (Milestone Ethos 900) at 280 °C and 55 bar. The content of major, minor, essential, and non-essential trace elements, as well as rare earth elements (REEs), was determined by inductively coupled plasma mass spectrometry (Perkin Elmer NexION 350 spectrometer; Waltham, MA, USA) and expressed on a dry weight basis (either mg/kg or μg/kg dw). The analytical quality was checked with the certified Standard Reference Material GBW 07604 “Leaves of Poplar” and showed recoveries in the range 94–106%. The analytical precision was >95% for all elements. For each sample, five technical replicates were measured.
3
Comprehensive Characterization of M/CeO2 Catalysts
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Powder X-ray diffraction (PXRD) of all M/CeO2 catalysts was measured from 2θ = 20–80° on a Bruker D8 Discover Vario diffractometer by using Cu Kɑ (L = 1.54 Å) radiation that was operated at 40 kV and 40 mA. X-ray photoelectron spectroscopy (XPS) measurements were carried out on an Axis Supra (Kratos Analytical) using the monochromated Ka X-ray line of an Aluminium anode. The pass energy was set to 40 eV with a step size of 0.15 eV. The samples were electrically insulated from the sample holder and an electron flood gun was used to neutralise the charges. The binding energy scale was then referenced at 284.8 eV using the aliphatic line of the C1s orbital. Inductively coupled plasma mass spectrometry (ICP-MS) was performed on a Perkin Elmer NexIon 350 spectrometer for elemental analysis. Scanning transmission electron microscopy (STEM) images for Rh/CeO2, Pd/CeO2 and Ir/CeO2 were captured on a FEI Tecnai Osiris electron microscope at 200 KeV, while high resolution (HR) STEM images for Ru/CeO2 and Pt/CeO2 were captured on a FEI Titan Themis electron microscope at 300 keV. High-angle annular dark field (HAADF) imaging mode was used for all STEM imaging. Energy-dispersive X-ray spectroscopy (EDX) was performed at 20 KeV.
4
Inductively Coupled Plasma-Mass Spectrometry Analysis of Cerium
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The Ce of controls and exposed skin samples, together with receptor and donor solutions, were evaluated by Inductively Coupled Plasma -Mass Spectrometry (ICP -MS) using a NexION 350× Spectrometer (PerkinElmer, USA) equipped with an ESI SC Autosampler. The analysis was performed in KED mode (Kinetic Energy Discrimination) using ultra-high purity helium (flow rate of 4.8 ml min -1 ) to control and minimize cell-formed polyatomic ion interference. The ICP-MS calibration curve was linear (R 2 = 0.999 Ce) in the concentration range of 1-100 μg l -1 according to the dilution of a multistandard solution of 10 mg l -1 for ICP analysis (Periodic Table MIX 3, . Measurements of the samples were performed using the calibration curve method obtained by analyzing standard solutions for instrumental calibration. The limit of detection (LOD) was 0.0003 μg l -1 for Ce. The coefficient of variation of repeatability (RSD %) was <3%.
5
Characterization of Zinc Oxide Nanoparticles
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ZnCl2 (CAS 7646-85-7), low and normal melting point agarose, Neutral Red, phosphate buffer saline were supplied by Sigma Aldrich (Milano, Italy), Giemsa by Carlo Erba (Milano, Italy). Cellulose from cotton linters was kindly provided by Bartoli SPA (Capannori, Lucca, Italy). Deionized water (DI) was prepared with a Millipore Elix® Deionizer equipped with a Progard® S2 ion exchange resins. The other equipment employed are: Branson Sonifier 250 (Branson Ultrasonic SA, Carouge, Switzerland), 6.5 mm probe tip and a SP Scientific BenchTop Pro Lyophilizer (Perugia, Italy) and a Transmission Electron Microscope (TEM; Philips CM 200, Koninklijke Philips N.V., Amsterdam, The Netherlands). Zeiss EVO 50 EP was provided by Carl Zeiss Microscopy Gmb (Jena, Germany). Milestone Ethos 900 microwave lab station (Sorisole, Italy). Lyophilised bacteria, all Microtox® reagents, Microtox®M500 luminometer and Microtox OMNI™ v. 1.16 software were obtained from ECOTOX LDS (Cornaredo, Milan, Italy). Coupled Plasma-Optical Emission Spectrometry (ICP-OES) was performed with Perkin Elmer Optica 8300 (Perkin Elmer, Waltham, MA, USA). Zn determination in soft tissues and CNS was carried out by inductively coupled plasma-mass spectrometry (ICP-MS) using the Perkin Elmer NexION 350 spectrometer (Waltham, MA, USA).
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