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Ac 400 mhz spectrometer

Manufactured by Bruker

The AC-400 MHz spectrometer is a nuclear magnetic resonance (NMR) instrument designed to analyze the structure and composition of chemical compounds. It operates at a radio frequency of 400 MHz and is capable of detecting the magnetic properties of atomic nuclei within a sample.

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11 protocols using ac 400 mhz spectrometer

1

Particle Characterization Techniques

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DLS and zeta potential measurements were performed in 1 mM PBS on a Zetasizer NanoZS (Malvern Analytical) using disposable folded capillary cells. FT-IR measurements were performed on a Nicolet iS50 FT-IR spectrometer. 1H NMR spectra were recorded on a Bruker AC-400 MHz spectrometer. Samples for electron microscopy were prepared by drying 10 μL of concentrated particle solution on silicon substrates (5 × 5 mm2 for SEM) or carbon-coated copper grids (TEM). Samples were air-dried overnight and imaged using JSM-7000F (SEM, 15.0 kV) or JEM 2000FXII (TEM, 200 kV).
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2

Synthetic Methodology for Diverse Compounds

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Unless otherwise noted, chemicals were obtained from commercial suppliers and used
without further purification. NMR spectra were recorded on a Bruker AC 400 MHz
spectrometer in the indicated solvent. Chemical shifts are reported in parts per million
(ppm) and are relative to CDCl3 (7.26 and 77.0 ppm) or to CD3OD
(3.31 and 49.2 ppm). The abbreviations used are as follows: s, singlet; brs, broad
singlet; d, doublet; dd, double doublet; t, triplet; q, quartet; m, multiplet; brm,
broad multiplet. Melting points were determined by the capillary method using a Buchi
535 instrument, and they were not corrected. TLC was performed on aluminum backed silica
plates (silica gel 60 F254). Flash chromatographic purifications were performed via
Biotage Isolera Prime using the appropriate cartridge, eluent, and gradient.
Hydrogenations were performed with H-Cube apparatus (Thalesnano Nanotechnology Inc.,
Budapest, Hungary) using a 10% Pd/C cartridge (s-cart, 30 × 4 mm i.d.). With the
exception of compound 9, all of the synthesized compounds have been
previously reported, and their spectroscopic and analytical data were consistent with
the literature.33 (link),35 (link),52 (link) The purity of the synthesized compounds (>95%) was
assessed by HPLC–HRMS.
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3

Synthesis of AMG 510-alkyne Compound

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All commercially available compounds were purchased and used as received. The protocol used for the synthesis of AMG 510-alkyne was modified from reported protocols[7 (link)]. 1H and 13C NMR spectra were recorded on a Bruker AC-400 MHz spectrometer. Unless otherwise stated high-performance liquid chromatography was done with a gradient of water (0.1% formic acid) and acetonitrile (0.1% formic acid) and separated with a XTerra MS C18 Column, 125Å, 5 μm, 4.6 mm X 50 mm and mass ions were detected on a Waters 3100 Mass Detector. Reverse-phase chromatography was completed using Biotage® Sfär Bio C18 D Duo 300 Å 20 μm columns on a Biotage® Isolera with a gradient composed of water (0.1% formic acid) and acetonitrile (0.1% formic acid), starting from 5 % to 100 % acetonitrile (0.1% formic acid). Detailed information on the synthesis is provided in the supplementary methods.
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4

Electrochemical Characterization of Redox Probes

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Unless otherwise mentioned, all materials were used as received. Tetrabutylammonium bromide (TBAB, 99.0 %), sodium hydroxide (NaOH, 50wt%), anhydrous tetrahydrofuran (THF, ≥99.9%), potassium ferrocyanide (K4[Fe(CN)6], ≥98.5%), potassium ferricyanide (K3[Fe(CN)6], ≥99%), and potassium chloride (KCl, ≥99.0%) were purchased from Sigma-Aldrich. β-propiolactone (95%) and anhydrous magnesium sulfate (MgSO4, ≥99.5%) were received from Alfa Aesar and dimethyl sulfoxide (DMSO, >99.0%), pyrrole (99%) and 3-dimethylaminopropylchloride hydrochloride (98%) were purchased from TCI. Methanol (MeOH, ≥99.8%) and diethyl ether (99.0%) were ordered from VWR. D2O and CDCl3 were purchased from Cambridge Isotope Laboratories (USA). Carbon (Cat. #C110) and gold screen printed (Cat. #220 AT) electrodes were purchased from Metrohm DropSens (Spain). Both electrode types have the same dimensions: 3.4 × 1.0 × 0.05 cm3 (length × width × height). Reaction mixtures were purified using a Biotage SNAP Bio C18 25 μm 60 g on a Biotage Isolera with a gradient composed of water and methanol for reversed-phase chromatography. In all cases, water refers to MilliQ water with a resistivity of 18.2 MΩ cm−1 at 25 °C. 1H and 13C NMR spectra were recorded on a Bruker AC-400 MHz spectrometer. Electrospray ionization mass spectra were recorded using a Waters 3100 Mass Detector.
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5

NMR Characterization and Purification Protocols

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NMR spectra were recorded at room temperature
in 5 mm tubes on
a Bruker AC 400 MHz spectrometer (NMR facility, PCN-ICMG, Grenoble).
Chemical shifts (δ) are reported in parts per million (ppm)
from low to high field and referenced to residual nondeuterated solvent
relative to Me4Si. Standard abbreviations for multiplicity
were used as follows: s = singlet; d = doublet; t = triplet; m = multiplet.
High-resolution mass spectrometry (HRMS) was carried out on a Bruker
UHR-Q-TOF MaXis-ETD (time of flight) mass spectrometer using electrospray
ionization (ESI) in Institut de Chimie Organique et Analytique (CBM-ICOA)
in Orleans (France). Reversed-phase HPLC was performed with a μ-bondapak-C18
analytical column (Waters Corporation, Milford, MA). A Waters chromatographic
system was used, with two M-510 pumps and a photodiode array detector
Waters 996 using Millenium 32 software. A linear gradient from 0 to
100% methanol in H2O pH 2.5 (phosphoric acid), 2 mL/min
flow rate, was used.
N-(Prop-2-yn-1-yl)prop-2-ynamide 2 was prepared by biocatalyzed reaction as reported by us.20 (link)para-Nitrophenyl propiolate 5,33 (link)para-nitrophenyl
isonicotinate 13,22 (link) NH2EG-Biotine·TFA 21,34 (link) and dansyl and tosyl sulfonamides 21a,b were prepared following reported procedures.19 (link) Streptavidin-agarose was purchased from Thermo Scientific
Pierce (Waltham, MA).
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6

Amiodarone-Cyclodextrin Nanoparticle Characterization

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Particle size was calculated by dynamic light scattering (Malvern, Zetasizer APS) at a concentration of 5 mg/mL in PBS buffer. Scanning electron microscopy was performed on samples prepared at 200 μg/mL in water, spotted on silica wafers, freeze-dried and sputter coated prior to imaging. To examine the interaction of amiodarone with succinyl-β-cyclodextrin, 1.0 mg of amiodarone was dissolved in 100 μL DMSO, added to PBS buffer containing CDNP at a final concentration of 5.0 mg/mL and mixed overnight at 50 C. The sample was then freeze-dried to provide a white powder which was suspended in 1.0 mL of 1:9 DMSO-d6 to D2O. ROSEY spectra with solvent suppression was collected on a Bruker AC-400 MHz spectrometer.
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7

Synthesis and Characterization of ITMS Monomer

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The monomer ITMS was synthesized according to the literature, as shown in Fig. 7. Briefly, thiourea (0.21 mol) was dissolved in methanol (60 mL), followed by the addition of p-chloromethylstyrene (CMS, 0.2 mol) to the solution. The reaction mixture was then stirred at room temperature for 24 h. Diethyl ether was then added to precipitate the desired ITMS monomer. The filtered product was purified by dissolving it in ethanol and re-precipitation with ether (41.13 g, 0.18 mol, 90 %). The solid residue was analyzed by 1H and 13C NMR which showed the pure desired product.

Synthetic scheme for the ITMS monomer

Nuclear magnetic resonance (NMR) spectroscopy was performed on Bruker AC 400 MHz spectrometer. 1H and 13C NMR spectra were recorded in deuterated dimethyl sulfoxide.
1H NMR (400 MHz, DMSO-d6) δH in ppm: 4.53 (s, 2H, CH2–S), 5.28 (d, 10.8 Hz, 1H, CH2=CH [trans]), 5.85 (d, 17.6 Hz, 1H, CH2=CH [cis]), 6.73 (dd, 10.8 Hz and 17.6 Hz, 1H, CH2=CH [gem]), 7.41 (d, 8.2 Hz, Arom-CH), 7.48 (d, 8.2 Hz. Arom-CH), 9.32 (s, 4H, Isothiouronium).
13C NMR (400 MHz, DMSO-d6) δC in ppm: 34.8 (CH2–S), 114.9 (CH2=CH), 126.6 and 129.1 (Arom-CH), 133.6 and 135.8 (Arom C), 137.4 (CH2=CH), 170.3 (C-Isothiouronium).
MS (CI+): 117 (CH2CHArCH2+, 100 %), 193 (M+, 10.5 %).
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8

Synthesis and Characterization of Metronidazole Derivative

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4-(Dimethylamino)pyridine (DMAP, CAS: 1122-58-3), N,N-dicyclohexylcarbodiimide (DCC, CAS: 538-75-0), trifluoroacetic acid (TFA, CAS: 76-05-1), metronidazole (CAS: 443-48-1), furfurylamine (CAS: 617-89-0), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (EDC, CAS: 25952-53-8), N-hydroxysuccinimide (NHS, CAS: 6066-82-6), sodium hydroxide (NaOH, CAS: 1310-73-2), hydrogen chloride (HCl, CAS: 7647-01-0) were purchased from Sigma Aldrich, Alfa Aesar or Acros Organics and used without further purification. Solution NMR spectra were recorded at room temperature in 5 mm tubes on a Bruker AC 400 MHz spectrometer (NMR facility, PCN-ICMG, Grenoble). Chemical shifts (δ) are reported in parts per million (ppm) from low to high field and referenced to residual non-deuterated solvent relative to Me4Si. Standard abbreviations for multiplicity were used as follows: s = singlet; d = doublet; t = triplet; m = multiplet. High resolution mass spectrometry (HRMS) was carried out on a Waters Xevo G2-S-QTof mass spectrometer using ElectroSpray Ionisation (NMR facility, PCN-ICMG, Grenoble).
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9

Characterization of Polymer Nanogels

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Polymer functionalization was evaluated through NMR and FT-IR analyses. 1 H-NMR spectra were carried out on a Bruker AC (400 MHz) spectrometer using chloroform (CDCl3) as a solvent, and chemical shifts were reported as δ values in parts per million with respect to tetramethylsilane (TMS) as an internal reference. FT-IR spectra were recorded using the KBr pellet technique for the analyzed samples and a Thermo Nexus 6700 spectrometer coupled to a Thermo Nicolet Continuum microscope equipped with a 15 × Reflachromat Cassegrain objective, at room temperature in air in the wavenumber range 4000-500 cm -1 , with 64 accumulated scans and at a resolution of 4 cm -1 . The nanogel size, polydispersity index (PDI) and -potential were recorded using the Dynamic Light Scattering (DLS) technique and a Zetasizer Nano ZS from Malvern Instruments. Samples were dissolved in distilled water and the solution was equilibrated for 60 s before data analysis, performed at 37°C. Data shown are an average value of three measurements of each studied nanogel. NG dimensions were also studied with Atomic Force Microscopy (AFM).
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10

Synthesis and Characterization of Novel Compounds

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All the chemicals were supplied by Merck (Germany), Konark Herbal (India) and S. D. Fine Chemicals (India). Melting points were determined by open tube capillary method and are uncorrected. IR spectra were obtained on a Schimadzu 8201 PC, FT-IR spectrometer (KBr pellets). 1H NMR spectra were recorded on a Bruker AC 400 MHz spectrometer using TMS as internal standard in DMSO d6. Mass spectra were recorded on a Bruker Esquire LCMS using ESI and elemental analyses were performed on Perkin-Elmer 2400 Elemental Analyzer.
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