Powder X-ray diffraction data were collected on a Bruker D8 Advance Eco diffractometer equipped with a Cu Kα radiation source (λ = 1.541874 Å), in the Debye-Scherrer geometry. The microcrystalline samples were sealed in glass capillaries and measured in the 5-50°2θ range at room temperature. The reference powder patterns from SC-XRD measurements were generated using Mercury CSD 4.3.1 software. 29 Elemental analyses of CHN were performed on an ELEMENTAR Vario Micro Cube CHNS analyser. IR spectra were collected on a Bruker Alpha II spectrometer with a diamond ATR add-on. The thermogravimetric data were collected using a Netzsch TG 209 F1 Libra apparatus. The water sorption/desorption processes were characterized by the dynamic vapor sorption method using the SMS DVS Resolution apparatus. The isotherm was measured in a 0-90% relative humidity range at a temperature of 25 °C. Every measurement step was performed until a stable Dalton Transactions Paper mass was achieved. Magnetic susceptibility measurements were on a Quantum Design MPMS-3 Evercool magnetometer in magnetic fields up to 70 kOe. The experimental data were corrected for diamagnetism of the sample and the sample holder. The magnetic data were fitted using the PHI programme. 31
Vario micro cube chns analyser
Manufactured by Elementar
Sourced in Germany
The Vario MICRO cube CHNS analyser is a laboratory instrument designed for the determination of carbon, hydrogen, nitrogen, and sulfur content in solid and liquid samples. It provides accurate and reliable results for a wide range of materials, including organic and inorganic substances.
Automatically generated - may contain errors
Lab products found in correlation
Alpha 2 spectrometer, by Bruker (1 mentions)
Mpms 3 evercool magnetometer, by Quantum Design (1 mentions)
Tg 209 f1 libra apparatus, by Netzsch (1 mentions)
D8 advance eco diffractometer, by Bruker (1 mentions)
Nano zs instrument, by Malvern Panalytical (1 mentions)
Vertex 70, by Bruker (1 mentions)
Agilent 8900 icp qqq, by Agilent Technologies (1 mentions)
Spectro genesis eop 2, by SPECTRO Analytical Instruments (1 mentions)
Ethos easy, by Milestone (1 mentions)
Su8020 electron microscope, by Hitachi (1 mentions)
Vertex 80, by Bruker (1 mentions)
Stadi p, by STOE (1 mentions)
Mythen 1k detector, by Dectris (1 mentions)
Avance 2 600, by Bruker (1 mentions)
1100 lc msd, by Agilent Technologies (1 mentions)
Drx 400, by Bruker (1 mentions)
5 protocols using vario micro cube chns analyser
1
Comprehensive Characterization of Microcrystalline Samples
2
Characterization of DOTA-Functionalized Cellulose Nanocrystals
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The elemental compositions of both DOTA-CNC (ald.) and DOTA-CNC (OH) were analyzed with a vario MICRO cube CHNS analyser (Elementar Analysensysteme, GmbH, Germany). The results were reported as a percent composition (C, H, and N). The Fourier Transform Infrared Spectroscopy (FTIR, Vertex 70, Bruker, MA, USA) with attenuated total reflectance (ATR, MIRacle, PIKE Technologies, WI, USA) was used to confirm the conjugation of the DOTA chelator to the CNCs surface in both DOTA-CNC (ald.) and DOTA-CNC (OH). The surface charge (ζ-potential) of unmodified CNC, DOTA-CNC (ald.), and DOTA-CNC (OH) was determined from the NP electrophoretic mobility by Zetasizer Nano ZS instrument (Malvern, Worcestershire, UK) at 500 µg/ml in aqueous solution.
Moreover, the morphology and dimensions of unmodified and modified CNCs were characterized by 120 kV transmission electron microscopy (Tecnai 12 Bio-Twin FEI, Hillsboro, OR, USA). The unmodified and modified CNCs were dissolved in ultrapure water at 1 mg/ml and sonicated for 5 min.
Then, 5 µl of each CNC solution were applied on glow discharge treated carbon support film hexagonal 300 mesh copper grids (Electron Microscopy Sciences, PA, USA) and further negatively stained with 1% uranyl acetate for 2 min before leaving for 2 h of air-drying prior to the measurements.
Moreover, the morphology and dimensions of unmodified and modified CNCs were characterized by 120 kV transmission electron microscopy (Tecnai 12 Bio-Twin FEI, Hillsboro, OR, USA). The unmodified and modified CNCs were dissolved in ultrapure water at 1 mg/ml and sonicated for 5 min.
Then, 5 µl of each CNC solution were applied on glow discharge treated carbon support film hexagonal 300 mesh copper grids (Electron Microscopy Sciences, PA, USA) and further negatively stained with 1% uranyl acetate for 2 min before leaving for 2 h of air-drying prior to the measurements.
3
Comprehensive Leaf Nutrient Analysis
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The pulverized dried leaf material (0.2 g) was microwave digested with 3 ml concentrated HNO3 + 2 ml H2O2 for 1 h in a microwave oven (ETHOS EASY, Milestone Srl, Sorisole, Italy). The concentration of Si was determined by the inductively coupled plasma optical emission spectrometry (ICP-OES; Spectro Genesis EOP II, Spectro Analytical Instruments GmbH, Kleve, Germany) equipped with Spectro hydrofluoric acid (HF) resistant sample introduction system after incubation of the digested samples with 1 ml concentrated HF for 12 h. The concentrations of P, K, Ca, Mg, B, Fe, Cu, Mn, Zn, Mo, and Ni in the digested samples were determined by the inductively coupled plasma mass spectrometry (ICP-MS; Agilent 8900 ICP-QQQ, Agilent Technologies, Inc., Santa Clara, CA, USA). The concentrations of N and S were determined by direct combustion of the dried leaf samples in a Vario Microcube CHNS analyser (Elementar Analysensysteme GmbH, Hanau, Germany). The certified reference material (GBW10015 Spinach; Institute for Geophysical and Geochemical Exploration, Langfang, China) was used to evaluate the precision and accuracy of the mineral analyses.
4
Comprehensive Characterization of Cu-based Nanomaterials
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Powder X-ray diffraction (PXRD) patterns were collected with a transmission-geometry diffractometer Stadi P (Stoe) equipped with a Mythen 1K detector (Dectris) using Ge(111)-monochromated Cu-K α1 radiation (λ = 154.056 pm). The powder samples were placed between two layers of adhesive tape. Crystallographic data from the Inorganic Crystal Structure Database was used to calculate reference powder patterns for Cu (CSD 627114), Cu 2 O (CSD 180846) and Cu(OH) 2 (CSD 68459). Fourier-transform infrared (FT-IR) spectra were measured with a Vertex 80 (Bruker) spectrometer in attenuated total reflectance mode in the wavelength range 4000-500 cm -1 . Scanning electron microscopy (SEM) was performed using a SU8020 electron microscope (Hitachi) equipped with a tripledetector system for secondary and low-energy backscattered electrons with an acceleration voltage of 3 kV. DTA-TG curves were recorded with a STA 409 thermal analyser (Netzsch). The samples were heated under air in an alumina crucible with a rate of 5 K min -1 up to 600 °C. Elemental analysis was carried out with a Vario MICRO cube CHNS analyser (Elementar). Magnetisation measurements were conducted with a Heliumcooled vibrating sample magnetometer (Cryogenic) in DC mode in the range 2-300 K.
5
Comprehensive Analytical Characterization of Synthesized Compounds
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Liquid chromatography-mass spectrometry (LC/MS), NMR spectroscopy, and elemental analysis methods were applied to confirm the structure and purity of all synthesised compounds.
LC/MS analysis was performed on an 1100 LC (Agilent Technologies) with ELSD, UV (DAD 200–400 nm), and mass detection (1100 LCMSD, Agilent Technologies, APCI, and ES positive ionization). The most used column was the Onix C18 50 × 4.6 mm; eluent 1–0.1% TFA in water; eluent 2–0.1% TFA in acetonitrile, gradient—eluent 1–2.9 min, eluent 2–0.2 min, eluent 1—rinsing, flow rate—3.75 mL/min.
The structures of key target final compounds were unambiguously confirmed by 1H, 13C{1H},13C apt, COSY, HSQC, and NOESY NMR spectroscopy. For structure confirmation of intermediates, 1H NMR spectroscopy was applied, and in some cases, if it was necessary, 13C{1H} NMR spectra were also registered. NMR spectra were registered on spectrometers Bruker DRX 400 (400.13 MHz for protons, 100.61 MHz for carbons, 376.50 MHz for fluorine), Bruker Avance II+ 600 (600.11 MHz for protons, 150.93 MHz for carbons), Avance IIIHD 500 (500.13 MHz for protons, 125.78Mhz for carbons), and spectrometer Bruker Avance III 400 UltraShield Plus (400 MHz). CDCl3 and DMSO-d6 were used as solvents.
Elemental analysis was performed on Vario MICRO cube CHNS analyser (Elementar Analysensysteme GmbH, Hanau, Germany).
LC/MS analysis was performed on an 1100 LC (Agilent Technologies) with ELSD, UV (DAD 200–400 nm), and mass detection (1100 LCMSD, Agilent Technologies, APCI, and ES positive ionization). The most used column was the Onix C18 50 × 4.6 mm; eluent 1–0.1% TFA in water; eluent 2–0.1% TFA in acetonitrile, gradient—eluent 1–2.9 min, eluent 2–0.2 min, eluent 1—rinsing, flow rate—3.75 mL/min.
The structures of key target final compounds were unambiguously confirmed by 1H, 13C{1H},13C apt, COSY, HSQC, and NOESY NMR spectroscopy. For structure confirmation of intermediates, 1H NMR spectroscopy was applied, and in some cases, if it was necessary, 13C{1H} NMR spectra were also registered. NMR spectra were registered on spectrometers Bruker DRX 400 (400.13 MHz for protons, 100.61 MHz for carbons, 376.50 MHz for fluorine), Bruker Avance II+ 600 (600.11 MHz for protons, 150.93 MHz for carbons), Avance IIIHD 500 (500.13 MHz for protons, 125.78Mhz for carbons), and spectrometer Bruker Avance III 400 UltraShield Plus (400 MHz). CDCl3 and DMSO-d6 were used as solvents.
Elemental analysis was performed on Vario MICRO cube CHNS analyser (Elementar Analysensysteme GmbH, Hanau, Germany).
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