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Unity inova 400 mhz spectrometer

Manufactured by Agilent Technologies
Sourced in United States

The Unity Inova 400 MHz spectrometer is a laboratory instrument designed for nuclear magnetic resonance (NMR) spectroscopy. It operates at a frequency of 400 MHz and is capable of analyzing samples to provide detailed information about their molecular structure and composition.

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8 protocols using unity inova 400 mhz spectrometer

1

Synthesis and Characterization of Novel Compounds

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All synthetic transformations were performed under an argon atmosphere with magnetic stirring unless otherwise mentioned. Flash chromatography was performed using a CombiFlash with RediSep pre-packed silica columns (230-400 mesh) as the stationary phase, unless otherwise stated. NMR spectra were acquired on a Varian 400 MHz Unity Inova spectrometer. Chemical shifts are reported relative to residual protonated solvent (7.26 ppm for CHCl3). All reagents were purchased from Sigma-Aldrich, TCI, Santa Cruz Biotech, Gelest, or other commercial suppliers and used as received unless otherwise stated. Preparation of compounds 2 and 3 (Fig. 1) is described by Aouida et al. (37 ). Preparation of 3 was based on established procedures of analogous compounds (41 (link)). We prepared 1 from 3 using a large excess of suberic acid bis(N-hydroxysuccinimidylester) to minimize dimerization.
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2

Characterization of POMs and Gold Nanoparticles

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The morphology of the POMs was obtained by scanning electron microscopy using the FEI-SEM system (FEI Helios Nanolab 600i, FEI, Hillsboro, OR, USA) at 5 kV. The surface chemistry was determined by FTIR spectroscopy using the Perkin–Elmer Spectrum GX-spectrophotometer (Thermo, Waltham, MA, USA) with a spectral resolution of 1 cm−1 and scan number of 32. The molecular structure was confirmed by the 29Si NMR technique using the Varian Inc. 400 MHz UNITY INOVA spectrometer (Varian Medical Systems, Palo Alto, CA, USA) at room temperature and magic-angle spinning, resonance frequencies, and 90° pulse length of 5 kHz, 79.5 MHz, and 6.5 µs, respectively. The morphology of the gold nanoparticles on POMs were observed using the FEI Tecnai G2F30 electron microscope (FEI) operating at 200 kV. For the nanoparticle size gauge values, the average of ≥100 particles on the TEM images were taken. The UV–Vis spectra were obtained using the Evolution 201 (Thermo) UV–vis spectrophotometer with 1 cm quartz cuvettes. TGA was conducted using the Mettler TGA/DSC 3+ (Mettler-Toledo, Zurich, Switzerland) from natural temperature to 800 °C at a heating rate of 5 °C min−1 under N2 atmosphere. EA was performed using the Vario EL Cube (Elementar, Frankfurt, Germany) EA instrument. Inductively coupled plasma (ICP) analysis was performed using the Perkin-Elmer Nexion 300 (Perkin-Elmer, Waltham, MA, USA).
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3

Extraction and Purification of Corn Fiber Esters

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Example 9

In this example, 500 g of concentrated ethanol oil containing ethyl ferulate and ethyl coumarate extracted from corn fiber was added to 1 L deionized water with 0.5 N NaOH. The oil was soluble in aqueous base. The aqueous solution was placed into a separatory funnel and washed with 330 mL hexanes. The hexanes was then removed from the separatory funnel and the aqueous solution was washed with 330 mL hexanes two additional times. In total 990 mL hexanes was used. The hexane extract was then placed in a round bottom flask and the hexanes removed with a rotary evaporator to yield liquid corn oil. Following extraction of the aqueous ethyl ferulate and ethyl coumarate solution with hexanes, the volume of the aqueous layer was 1.5 L and the ethyl ferulate and ethyl coumarate remained in the aqueous layer. HPLC analysis (Method 2) of the aqueous phase following hexane extraction confirmed that ethyl ferulate and ethyl coumarate remained in the aqueous layer as shown in FIG. 14. 1HNMR analysis of the corn oil using a Varian Unity Inova 400 MHz spectrometer was used to confirm that the corn oil is comprised of primarily the ethyl esters of oleic and linoleic acid as shown in FIG. 15.

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4

Inert Conditions Reaction Characterization

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Reactions that
required inert conditions
were performed using modified Schlenk techniques or in an MBraun Unilab
glovebox under a nitrogen atmosphere. 1H and 13C NMR spectra were recorded on a Varian Unity Inova 400 MHz spectrometer. 1H and 13C NMR chemical shifts are given relative
to the residual proton or 13C solvent resonances. NMR spectra
were recorded at room temperature (20–25 °C) unless otherwise
noted. GC/MS data were collected on an Agilent 6890 Series GC connected
to a HP 5973 mass detector. Elemental analyses were performed using
a Thermo Electron Flash EA 1112 Series analyzer. Microwave heating
was conducted using a CEM Discover SP instrument in either 10 or 35
mL snap cap pressure tubes or in an open vessel mode. The temperature
of the reactions in the microwave was monitored using the floor-mounted
IR sensor in the instrument (external surface measurement).
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5

Deuterium-labeled NMR Characterization

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Samples were prepared as ~5 mg/mL solutions in deuterium-labeled chloroform (Acros Organics, Waltham, MA, USA), dimethylsulfoxide (Cambridge Isotope Laboratories, Tewksbury, MA, USA), or methanol (CDN Isotopes, Pointe Claire, Canada). 1H-NMR spectra were measured on a Varian Unity Inova 400 MHz spectrometer. Chemical shifts were reported in parts per million (ppm). Results can be found in the supporting information section.
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6

NMR Spectroscopy of Biological Samples

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1H NMR spectra were recorded on a Varian Unity INOVA 400 MHz spectrometer equipped with a multinuclear probe and z-axial gradients. The samples of Gel, GM, and GL were prepared by dissolving 5 mg in 700 μL of D2O containing 0.1 mM of 3-(trimethyl-sily1)-1-propane sulfonic acid (DSS) as internal reference standard at 0 ppm. One-dimensional spectra were acquired in Fourier mode with quadrature detection.
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7

Analytical and Preparative HPLC Procedures

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Analytic HPLC was performed with one of three systems: a Waters Alliance 2695 separation module (Milford, MA) equipped with a Waters 2998 diode array detector and an analytical Apollo C-18 column (250 mm × 4.6 mm, 5 μm) or a Dionex Ultimate 3000 Focused separation module (Bannockburn, IL) equipped with a DAD-3000(RS) and MWD-3000(RS) diode array detector and an Acclaim 120 C-18 column (4.6 mm × 100 mm, 3 μm) or an Agilent 1200 Series Quaternary LC system and an Eclipse XDB-C18 column (150mm × 4.6 mm, 5 μm, 80Å) equipped with an Agilent 6120 Quadrupole MSD mass spectrometer (Agilent Technologies, Santa Clara, CA). Semi-preparative HPLC was performed with a Waters 600 controller and pump (Milford, MA) equipped with a 996 diode array detector, 717plus autosampler, and an Apollo C-18 column (250 mm × 10 mm, 5 μm) purchased from Grace (Deerfield, IL). LC-electrospray ionization (ESI)-mass spectroscopy (MS) was performed using an Agilent 6120 Quadrupole MSD mass spectrometer (Agilent Technologies, Santa Clara, CA) equipped with an Agilent 1200 Series Quaternary LC system and an Eclipse XDB-C18 column (150mm × 4.6 mm, 5 μm, 80Å). High resolution (HR)-MS was performed using a Bruker BioTOF II, and NMR data were collected using a Varian Unity Inova 400 MHz spectrometer (Varian, Inc., Palo Alto, CA).
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8

Spectroscopic Analysis of Chemical Samples

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All UV-visible (UV-Vis) spectrophotometry was carried out on a Varian Cary-Bio 300 UV-Vis spectrophotometer. 1 H NMR spectra were recorded on a Varian Unity Inova 400 MHz spectrometer (5 mm broad band probe) at room temperature. Mass spectra were obtained using electrospray ionization mass spectrometry (ESI-MS) and tandem mass spectrometry (ESI-MS/MS) on a Micro Mass QTOF-2 mass spectrometer (Waters Corp.), using argon as the collision gas. Inductively coupled plasma atomic emission spectroscopy (ICP-AES), measurements were taken on a Thermo iCAP 6300, and calibrated from dilutions of 1000 ppm Mn(II) or Fe(III) standard solutions (Fisher), using class A volumetric glassware. X-Band EPR spectra were obtained using a Bruker EMXplus Spectrometer with an aqueous flat cell. Prior to inoculation, 20 mL of filter-sterilized 1.0 M HEPES buffer (pH 7.4), and 4 mL of filtersterilized 1.0 M NaHCO 3 buffer were added to the medium.
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