Silica gel (230–400 mesh, Merck KGaA, Darmstadt, Germany) column chromatography was performed with dichloromethane and methanol as eluents. HPLC was performed with a Gilson system (Gilson Inc., Middleton, WI, United States) using a Shim-pack ODS (21.5 × 250 mm, Shimadzu, Kyoto, Japan) column. NMR spectra (1H and 13C) were recorded on a Bruker Avance DPX 250 Spectrometer (Bruker, Billerica, MA, United States) using CD3OD. LR-ESI-MS was performed on an Agilent 6120 series LC-MS (Agilent Technologies, Santa Clara, CA, United States).
Avance dpx 250 spectrometer
Manufactured by Bruker
Sourced in United States
The Avance DPX-250 spectrometer is a nuclear magnetic resonance (NMR) spectrometer designed for routine analysis and research applications. It operates at a proton frequency of 250 MHz and is capable of performing various NMR experiments to study the properties and characteristics of chemical compounds. The Avance DPX-250 is a compact and versatile instrument that can be used in a wide range of research and industrial settings.
Automatically generated - may contain errors
Lab products found in correlation
Silica gel 60, by Merck Group (2 mentions)
Silica gel, by Merck Group (1 mentions)
Em208s transmission electron microscope, by Philips (1 mentions)
Pw1730, by Philips (1 mentions)
Vns600, by Agilent Technologies (1 mentions)
Agilent 1260 series hplc system, by Agilent Technologies (1 mentions)
Dip 1000 polarimeter, by Jasco (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Dtg 60h, by Shimadzu (1 mentions)
Alpha ftir spectrometer, by Bruker (1 mentions)
Quanta 650f, by Thermo Fisher Scientific (1 mentions)
Flash ea 2000 chns, by Thermo Fisher Scientific (1 mentions)
Jem 1400, by JEOL (1 mentions)
Tensor 27 ftir, by Bruker (1 mentions)
7500ce icp ms, by Agilent Technologies (1 mentions)
7 protocols using avance dpx 250 spectrometer
1
Silica Gel Column Chromatography and Analytical Techniques
2
Characterization of Iron-Based Nanomaterials
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Ferric chloride hexahydrate (FeCl3·6H2O, > 99%) and ferrous chloride tetrahydrate (FeCl2·4H2O) were used as an iron source. Pectin with the degree of esterification of 76% and other materials used in this article were from Merck (Germany) and Sigma Aldrich and were used without further purification. The reaction progress and purity of the products were determined using TLC on silica‐gel Polygram SILG/UV254 plates. FT‐IR spectra were recorded with a Nicolet system 800 beam splitter KBr SCAL = 800 in the 400–4000 cm−1. Transmission electron microscope (TEM) investigations were performed using a Philips EM 208S Transmission Electron Microscope. Thermogravimetric analysis (TGA) was also recorded under argon and air atmosphere using TGA/TDA Q600 TA Instruments. Melting points were determined using an electrothermal 9100 device. The powder X‐ray diffraction (XRD) was performed within Philips PW1730 with a Cu Kα (λ = 1.54060 Å) radiation. SEM–EDX was recorded by Fe-SEM TESCAN MIRA3. The 1H NMR (250 MHz) and 13CNMR (62.9 MHz) analyses were performed on a Bruker Avance DPX-250 spectrometer in CDCl3 and DMSO-d6 as solvent and TMS as internal standard.
3
Analytical Techniques for Natural Product Characterization
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Optical rotation was measured using a Jasco DIP-1000 polarimeter (JASCO Inc., Tokyo, Japan) coupled with a sodium lamp (589 nm). Vacuum liquid chromatography (VLC) was performed using Silica Gel 60 (230–400 mesh, Merck KGaA, Darmstadt, Germany). LR-ESI-MS was performed on an Agilent 1260 series HPLC system coupled with a 6120 series single quadrupole mass spectrometer (Agilent, Santa Clara, CA, USA). HPLC was carried out on a Gilson HPLC system (321 pump, and UV/Vis-155, Gilson Inc., Middleton, WI, USA) and a Waters HPLC system (PDA 996, and 600 controllers, Waters Corporation, Milford, MA, USA). The 1D and 2D NMR spectra were obtained using a Bruker Avance DPX250 spectrometer (Bruker, Billerica, USA) and 600 MHz Fourier transform nuclear magnetic resonance spectrometer (VNS600, Agilent) at the Core Research Support Center for Natural Products and Medical Materials.
4
Characterization of Organic Compound
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The reaction was checked with TLC using aluminum sheets with silica gel 60 F254 from Merck. The Melting point was measured using a Tottoli digital capillary melting point apparatus and uncorrected. The FT-IR spectrum was recorded with Perkin-Elmer Pargamon 1000 PC FT-IR spectrometer over the range 400–4000 cm−1. 1H and 13C NMR spectra were recorded in the DMSO‑d6 solution on a Bruker Avance DPX250 spectrometer. The chemical shifts are expressed in parts per million (ppm) from tetramethylsilane (TMS) as an internal reference. The Mass spectrum was obtained using an AB SCIEX API 3000 LC/MS/MS system equipped with an ESI source. TGA/DTA curves were recorded in a platinum crucible in a pure air atmosphere at a flow rate of 20 mL/min and over-temperature range 0–700°C with a heating rate of 10°C/min using Shimadzu thermogravimetric analyzer DTG-60H. Chemical reagents were purchased from Fluka and Sigma-Aldrich chemicals.
5
Detailed NMR and Spectroscopic Characterization
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NMR spectra were recorded on a Bruker Avance DPX 250 spectrometer at 250.0 (1H), 62.9 (13C), and 101.3 (31P) MHz or a Bruker Avance II Plus 700 spectrometer at 700.0 (1H) and 176.0 (13C) MHz. Chemical shifts are reported in ppm relative to TMS (internal standard) for 1H and 13C, and 85% phosphoric acid (external standard) for 31P. Chemical shifts are described as s (singlet), d (doublet), dd (doublet of doublets), t (triplet), q (quartet), m (multiplet), and bs (broad singlet). Coupling constants (J) are reported in hertz. IR spectra were recorded on a Bruker FT-IR ALPHA spectrometer equipped with a platinum ATR QuickSnap module. High-resolution mass spectra were obtained from a Finnigan MAT 95 spectrometer (FAB ionization) and Maldi SYNAPT G2-S HDMS (ESI ionization). MALDI-TOF spectra were recorded on an Applied Biosystems Voyager-Elite mass spectrometer. Thin layer chromatography was done on Merck 60F254 coated plates, and Merck silica gel 60 (mesh 230–400) was used for column chromatography. HPLC was performed with a Waters chromatograph interfaced with a 996 spectral diode array detector.
6
Spectroscopic Characterization of Organic Compounds
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1H and 13C NMR spectra were obtained using a Bruker Avance DPX-250 spectrometer. NMR experiments were performed at 294 K, using CDCl3 as a solvent. Coupling constants (J) were measured in Hz. LR-ESI-MS spectra were recorded using an Agilent Technologies 6120 quadrupole LC/MS system with a C18 column (Phenomenex Luna 3μ C18(2) M, 100 Å, New column; 150 × 4.6 mm) at a flow rate of 0.7 mL/min. HPLC was performed using a WATERS 1525 binary HPLC pump equipped with a WATERS 996 photodiode array detector together with a Hector C18 (250 × 21.2 mm) reversed-phase HPLC column.
7
Comprehensive Material Characterization Protocols
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All chemical reagents and solvents were purchased from commercial sources and used as received without further purification. NMR spectra were recorded on a Bruker Avance DPX-250 spectrometer and Bruker AMX-400 Wide Bore for liquid and solid-state samples respectively. Mass spectra were acquired on a micrOTOF-QII ESI-MS instrument. Purity of all bulk material batches was confirmed by X-ray powder diffraction (XRPD) patterns collected on an X'Pert PRO MPD analytical diffractometer (Panalytical) at 45 kV, 40 mA using Cu Kα radiation (λ 1.5419 Å), and compared with single crystal simulated patterns. Thermogravimetric analyses were performed under nitrogen flow using a STA 449 F1 Jupiter-Simultaneous TGA-DSC from NETZSCH with a heat rate of 5°C/min. IR spectra were recorded in transmission mode on a Bruker Tensor 27FTIR equipped with a Golden Gate diamond ATR cell. Elemental Analysis measurements were performed on a Flash EA 2000 CHNS, Thermo Fisher Scientific analyser. Inorganic Elemental Analysis measurements were performed on an ICP-MS 7500ce, Agilent Technologies. Scanning electron microscope images were acquired on a FEI Quanta 650F working at an accelerating voltage of 2 kV and a beam current of 50 pA. Transmission electron microscope images were acquired on a JEOL JEM-1400 working at an accelerating voltage of 120 kV.
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