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Avance 2 400 mhz nmr spectrometer

Manufactured by Bruker
Sourced in Switzerland, United States

The Avance II 400 MHz NMR spectrometer is an analytical instrument designed for nuclear magnetic resonance spectroscopy. It operates at a frequency of 400 MHz and is capable of detecting and analyzing the magnetic properties of atomic nuclei within a sample. The core function of the Avance II is to provide high-resolution data on the chemical structure and composition of various materials.

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14 protocols using avance 2 400 mhz nmr spectrometer

1

Synthesis and Characterization of PAAN, PAAND, and PAANS

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PAAN, PAAND and PAANS were precipitated with ethanol for 12 h and washed three times with acetone, thus removing the unreacted monomer. The products were dried at 40 °C. Then, PAAN, PAAND and PAANS were removed from the precipitated sample by Soxhlet extraction with a 60 : 40(v/v) mixture of ethylene glycol and acetic acid. Finally, PAAN, PAAND and PAANS were washed with ethanol, and were dried in a vacuum oven at 40 °C until the samples reached a constant weight.
1H nuclear magnetic resonance (1H NMR) analysis was used to determine the molecular structures and functional groups. 1H NMR analysis was conducted on an Avance II 400 MHz NMR spectrometer (Bruker Instrument Co. Ltd., Switzerland) to obtain proton nuclear magnetic resonance spectra. D2O was used for the field-frequency lock, and the observed 1H chemical-shifts were reported in parts per million (ppm). The elemental analysis of PAAN, PAAND and PAANS was conducted on an EA 2400II elemental analyzer (PerkinElmer Instrument Co. Ltd., USA) to determine the carbon, nitrogen, oxygen and sulfur content. Determination of the molecular weight distributions of PAAN, PAAND and PAANS was conducted through static light scattering (SLS) measurements (Wyatt Technology Inc., Canada) using a Gs-As laser (658 nm and 40 mW).
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2

NMR Spectroscopy of Urea-TMAO Solutions

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Stock solutions were prepared by dissolving crystalline samples of TMAO dihydrate and urea (sourced from Sigma Aldrich and Thermo Fischer Scientific respectively) in ultrapure water. These solutions were then further combined with ultrapure water to create mixed solutions of urea, TMAO and water containing 0.2-4.0 moles TMAO per kg water and 0.2-8.0 moles urea per kg water.
Each sample was transferred by pipette into a 5 mm NMR tube. Where a spectral measurement was taken, a sealed 1 mm This journal is © the Owner Societies 2022 X-ray capillary tube, containing dimethyl sulfoxide (DMSO, Sigma-Aldrich), was inserted into the NMR tube (DMSO generates a reference 1 H NMR signal at 2.50 ppm 29 ). Three spectral measurements were made with a Bruker Avance II 400 MHz NMR spectrometer at each concentration and the average result is reported. 1 H NMR T 1 data were captured with a Magritek Spinsolve 43 MHz NMR spectrometer without a DMSO standard. All measurements were made at 300 K.
The following measurements were taken for each solution mixture: (i) the spectral peak location (ppm) for 1 H (water, urea, TMAO), (ii) proton NMR T 1 relaxometry (water) and (iii) the diffusion co-efficient of water (D).
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3

Bovine Milk Uricase Enzymatic Assay

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The bovine milk for the study was sourced from a reputable dairy farm located in Laghouat, Algeria. Uricase and peroxidase enzymes were purchased from BioLab. The substrate (xanthine), K2HPO4, KH2PO4, HCl, DMSO (dimethyl sulfoxide), EDTA (ethylene diamine tetraacetic acid), trisaminomethane (C4H11NO3), and all other reagents were purchased from Sigma–Aldrich. Allopurinol (control) was purchased from a local pharmacy. All reagents utilized in the experiment were of analytical grade. Fourier transform infrared (FTIR) spectra were recorded using a Thermo Fisher Scientific Nicolet IS50 FTIR spectrometer. 1H NMR and 13C NMR (APT) spectra were recorded on a Bruker Avance II 400 MHz NMR spectrometer (chemical shift in ppm downfield from TMS (tetramethylsilane) as an internal reference). The mass spectra were obtained by MALDI-TOF/MS (Bruker UltraFleXtreme). A Thermo Fisher Scientific microplate reader was used. A refrigerated centrifuge from HETTICH ROTANTA 460R was used.
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4

1H NMR Spectroscopy of Aqueous Humor in Glaucoma

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1 H NMR spectra of AH were acquired at 25°C using an Avance II 400 MHz NMR spectrometer equipped with a 5 mm [ 1 H, 13 C] inverse-detection dual-frequency probe (Bruker Biospin, Rheinstetten, Germany) as previously reported (Croitor-Sava et al., 2015) . Samples were thawed, 0.3 to 0.4 mL of D2O (containing sodium 3-(trimethylsilyl) propanesulfonate as a chemical shift reference, δ = 0ppm, Euroisotopes, Saint-Aubin, France) was added to 0.1 to 0.15 mL of AH and transferred to a 5 mm NMR tube (Euroisotopes, Saint-Aubin, France). One-dimensional 1 H NMR spectra were acquired with a spectral width of 12 ppm and using 16k data points. Free induction decays were averaged over 8k accumulations. A relaxation delay of 2s was allowed. Residual water was suppressed using a 1D NOESY presaturation sequence. An exponential function was applied prior to Fourier transformation, resulting in a line broadening of 0.1 Hz. NMR spectra were phase-and baseline-corrected using the Topspin software (Bruker Biospin). NMR spectral quality was assessed after each measurement and seven samples (8%) were excluded due to low spectral quality (either with a signal-to-noise ration < 5 or line widths > 3Hz). Further analysis was thus performed on 27 POAG, 27 NTG, 29 controls.
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5

Synthesis and Characterization of Pyrene-Based Hydrazinecarbodithioic Acid Esters

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All chemicals and solvents were reagent-grade and used without further
purification. Reagents, such as pyrene-1-carbaldehyde and hydrazine
hydrate, were obtained from commercial sources and used without further
purification. The starting materials S-methyldithiocarbazate30 (link) and S-benzyldithiocarbazate31 (link) were prepared as previously reported. The final
compounds N′-pyren-1-ylmethylene-hydrazinecarbodithioic
acid methyl ester (PS1) and N′-pyren-1-ylmethylene-hydrazinecarbodithioic
acid benzyl ester (PS2) were synthesized as previously reported.32 (link) Elemental analyses were performed on a PerkinElmer
Series II CHNS/O analyzer 2400. 1H and 13C NMR
spectra were measured on a Bruker AVANCE II 400 MHz NMR spectrometer.
Infrared spectra were recorded using a PerkinElmer 983 model FT-IR
spectrophotometer with compounds dispersed as KBr discs. Electronic
spectra were recorded on an Agilent-8453 diode array spectrophotometer.
ESI-mass spectra were recorded using an Agilent 6200 series Q-TOF
LC-MS instrument.
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6

Spectroscopic Characterization of Compounds

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FTIR (Fourier Transform Infrared Spektrofotometre) spectra were recorded using a ThermoFisher Scientific Nicolet IS50 FTIR spectrometer. 1H NMR and 13C NMR (APT) spectra were recorded on Bruker Avance II 400 MHz NMR spectrometer (chemical shift in ppm downfield from TMS (tetramethylsilane) as an internal reference). The mass spectra were obtained at MALDI‐TOF/MS (Bruker‐UltrafleXtreme). The reactions were monitored by TLC using silica gel coated plates and different solvents solutions as the mobile phase. The synthesis of the reaction was carried out in the ISOLAB Ultrasonic bath. Commercial grade reagents were purchased from Alfa Aesar (Kandel, Germany) and used without further purification.
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7

Chiral Schiff Bases Synthesis and Characterization

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Chiral Schiff bases were synthesized by treating commercially available aldehydes with chiral amine by grinding in a mortar and pestle for a period of 5–10 min at room temperature without the addition of any solvent or catalyst. The reaction progress was monitored by TLC. A paste was obtained upon grinding. After the completion of the reaction, water from the mixture was evaporated until dryness. The powder product obtained was finally recrystallized in absolute methanol [34 ]. The synthesized compounds were characterized through different spectroscopic techniques, including Proton Nuclear magnetic resonance spectroscopy (1H NMR) and infrared Spectroscopy. The 1H NMR was carried out in deuterated chloroform (CDCl3) on Bruker Avance II 400 MHz NMR Spectrometer using 300 MHz frequency for all compounds, except compound H1 which was run on 400 MHz frequency. The spectra were resolved through Topspin-4 (Bruker, London, UK) software. The IR spectroscopy was performed on Spectrum 3™ FT-IR Spectrometer.
As mentioned, all the synthesized compounds were successfully characterized through H NMR and IR Spectroscopic techniques. The technical details are described as follows:
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8

Comprehensive Characterization of Nanoparticles

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Proton nuclear magnetic resonance (1H NMR) measurements were performed with an Avance II 400 MHz NMR spectrometer (Bruker, USA). Molecular weights were determined by electrospray ionization mass spectrometry (ESI-MS) (Agilent, USA). The physical features of nanoparticles were observed with a JEM-1400 Flash electron microscope (JEOL, Japan) at 120 kV. Absorption spectra were obtained with a NanoDrop 8000 spectrometer (Thermo Fisher Scientific, USA). Fluorescence imaging was performed using a laser scanning confocal microscope (Zeiss, Germany).
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9

Characterization of Organic Compounds

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All of the reagents were purchased from commercial sources and were used without any additional purification. Precoated Merck TLC plates were utilized for monitoring the progress of the reaction (Merck & Co., Inc., Kenilworth, NJ, USA). Melting points were measured with a Stuart melting point apparatus (SMP-11) with an open glass capillary tube and are uncorrected (Cole-Parmer Ltd., Stone, UK). Infrared (IR) spectra of compounds were recorded on a Bruker FT-IR spectrophotometer (Bruker BioSpin Corp., Billerica, MA, USA). Mass spectra were recorded on a Shimadzu GCMS-QP2010 with EI mode (Shimadzu Corp., Kyoto, Japan). 1H NMR (proton nuclear magnetic resonance) and 13C NMR (carbon nuclear magnetic resonance) spectra were recorded with the help of a Brucker Avance II (400 MHz) NMR spectrometer using CDCl3 as a solvent (Bruker BioSpin Corp.). TMS (tetramethylsilane) was used as an internal reference standard (δ = 0). IR, NMR and mass spectra of the synthesized compounds are provided as supplementary information.
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10

Chiral Analyte Separation and Characterization

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All chiral analytes were separated on an LC-20AT high-performance liquid chromatograph (Shimadzu, Kyoto, Japan) equipped with an SPD-20A UV-VIS detector (Shimadzu). The 13C NMR spectra were collected on Bruker Advance III WB 400M (Bruker Daltonics, Bremen, Germany). The 1H NMR spectrum was collected on the AvanceII 400 MHz NMR spectrometer (Bruker, Switzerland). Scanning electron micrograph were obtained using Zeiss Sigma 300 field emission scanning electron microscopy (Zeiss, Germany). Thermogravimetric analysis was performed on an STA 449C synchronous thermogravimetric analyzer (Netzsch, Selb, Germany). Mass spectrometry (MS) analysis was performed on a 6540 TOF high-resolution mass spectrometer (Agilent, Santa Clara, CA, USA). C, H, N, and S contents were determined using a VarioEL III element analyzer (Elementar Analysensysteme GmbH, Langenselbold, Germany). IR analysis was performed on an FTIR-8400S Fourier Transform IR Spectrometer (Shimadzu). The synthesized bridged bis(β-CD) chiral ligand was packed using a CGY-100B chromatographic column packing machine (Beijing Fusiyuan Machinery Processing Department, Beijing, China). Ultrapure water was obtained using the VE-AS water purification system (Shenzhen Vamia Environmental Protection Co, Shenzhen, China).
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