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Avance dmx 500 spectrometer

Manufactured by Bruker
Sourced in Germany

The AVANCE DMX 500 is a nuclear magnetic resonance (NMR) spectrometer manufactured by Bruker. It is designed to operate at a frequency of 500 MHz and is capable of performing a range of NMR experiments to analyze the structure and properties of chemical compounds.

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8 protocols using avance dmx 500 spectrometer

1

Characterization of Organometallic Compounds

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NMR spectra were measured on a Bruker Avance 500 DMX spectrometer. 1H
NMR spectra are reported in ppm relative to SiMe4 (δ = 0) and were
referenced internally with respect to the protio solvent impurity (δ 7.26 for
CDCl3 and 2.50 for
Me2SO-d5).32 (link)13C NMR spectra are reported in ppm relative to SiMe4 (δ =
0) and were referenced internally with respect to the solvent (δ 77.16 for
CDCl3).32 (link) Coupling
constants are given in hertz. IR spectra were recorded in diffuse reflectance (DR) mode on
a Thermo Nicolet 6700 spectrometer (ThermoScientific) equipped with a smart collector
accessory, and the data are reported in reciprocal centimeters. Samples were finely ground
with KBr and a similarly prepared sample of KBr was used to obtain a background spectrum.
All chemicals were purchased from Sigma-Aldrich. [TmMeBenz]K was prepared by
the literature method.19b (link)
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2

NMR and IR Spectroscopic Characterization

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NMR spectra were measured on
a Bruker Avance 500 DMX spectrometer. 1H NMR spectra are
reported in ppm relative to SiMe4 (δ = 0) and were
referenced internally with respect to the protio solvent impurity
(δ 7.16 for C6D5H and 2.50 for DMSO-d5).72 (link)13C NMR spectra are reported in ppm relative to SiMe4
= 0) and were referenced internally with respect to the solvent (δ 128.06
for C6D6 and 39.52 for DMSO-d6).72 (link)77Se NMR spectra
are reported in ppm relative to neat Me2Se (δ = 0)
and were referenced using a solution of Ph2Se2 in C6D6 (δ = 460) as an external standard.73 199Hg NMR spectra are reported in
ppm relative to neat Me2Hg (δ = 0) and were
referenced using a 1.0 M solution of HgI2 in DMSO-d6 (δ = −3106) as an external
standard.74 Coupling constants are given
in hertz. IR spectra were recorded as KBr pellets on a Nicolet iS10
FT-IR spectrometer (ThermoScientific), and the data are reported in
reciprocal centimeters. 1-methyl-1,3-dihydro-2H-benzimidazole-2-selone
was obtained by a literature method,31a and all other chemicals were purchased from Sigma-Aldrich.
CAUTION! All mercury compounds are toxic, and
appropriate safety precautions must be taken in handling these compounds
.
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3

Enzymatic Ring-Opening Polymerization of ε-Caprolactone

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Standard enzymatic ring-opening polymerization of ε-caprolactone was conducted as follows: 200 μL ε-caprolactone, 600 μL organic solvent (with no addition of organic solvents in the solvent-free system), 50 μL of butyl acetate (internal standard) and different amounts of immobilized enzyme EC-EP-AFEST were mixed together in a screw-capped vial. During the reactions (stirring at 180 rpm), an aliquot of reaction mixture (10 μL) was taken via a syringe at regular intervals, diluted with dichloromethane (100 μL) and then analyzed by gas chromatography (GC) to determine the monomer conversion. After the reactions, dichloromethane was added to the systems, and enzymes were removed via filtration and washed with dichloromethane three times. The filtrate was collected and evaporated under reduced pressure to remove the dichloromethane. Following this, the viscous sample was precipitated in methanol at −20 °C, and the white precipitate was collected by the centrifugation at 8000 rpm for 15 min, which was then dried in a vacuum oven and identified by 1H-NMR in chloroform-d at 500 MHz on an AVANCE DMX 500 spectrometer (Bruker, Rheinstetten, Germany).
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4

Polymer Characterization by NMR and GPC

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1H NMR and 13C NMR spectra were recorded on a Bruker Avance DMX500 spectrometer in CDCl3 or (CD3)2SO with tetramethylsilane as the internal standard. The molecular weight and molecular weight distribution of these polymers were all determined by gel permeation chromatography (GPC), which was recorded on a Wyatt GPC/SEC-MALS using DMF as the mobile phase with a flow rate of 1.0 mL min−1. The solution concentration was 10 mg mL−1 and filtered before analysis. The FT-IR spectra were measured by a Nicolet iS 10.
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5

Characterization of Nanomaterials

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All chemical reagents were commercially available and used as received. Dichloromethane was dried and redistilled with CaH2. Other solvents were employed as purchased. NMR spectra were collected on a Bruker AVANCE DMX-500 spectrometer at room temperature. Chemical shifts (δ) are given in ppm and referenced to the standard TMS or residual solvent peaks. Mass spectra were recorded on an Agilent Technologies 6530 Q-TOF mass spectrometer with ESI resource. Dynamic light scattering (DLS) were recorded on a Malvern Nanosizer S instrument at room temperature. Transmission electron microscope (TEM) was performed at 120 kV using JEM-2010 or JEM-1010. Scanning electron microscope (SEM) was done with a JSM-6390LV or TM-1000 using second electron images. High-resolution transmission electron microscope (HRTEM) was carried out on a JEM-2100F at room temperature. Atomic force microscope (AFM) was carried out on a Bruker ICON3-sys. UV-vis spectra were measured with a Hitachi UH-5300 at room temperature. Fluorescence spectra were recorded on a Perkin Elmer LS55 at room temperature. Fourier transform infrared (FTIR) spectroscopy was carried out on a Thermo Scientific Nicolet iS50 at room temperature and only noteworthy absorptions (in cm–1) are listed.
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6

Identification of SBM compounds by MS and NMR

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The purified compounds from SBM were identified by electrospray ionization-mass spectrometry (ESI-MS), 1H NMR and 13C NMR spectrometry. The ESI-MS was carried out in a LCQ-Fleet mass spectrometer (Thermo Fisher Scientific, Waltham, MA), with an electrospray ionization source using a negative mode (m/z 50–800). 1H NMR spectra and 13C NMR spectra were recorded on a Bruker Avance DMX-500 spectrometer (Bruker Biospin GmbH, Germany), operating at 500 and 125 MHz for 1H and 13C, respectively, using D2O or deuterated dimethyl sulfoxide (DMSO-d6). In D2O, tetramethylsilane (TMS) was used as the internal standard. In DMSO-d6, the residual solvent was used as the internal standard. Chemical shifts were expressed in δ (ppm) downfield from TMS as an internal standard, and coupling constants were reported in hertz.
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7

NMR Spectroscopy and SEC Analysis

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1H-NMR spectra were recorded on a Bruker Avance DMX 500 spectrometer using CDCl3 as solvent and tetramethylsilane as internal reference. The molecular weight and molecular weight distribution were determined by size exclusion chromatographic (SEC). The SEC system consisted of a Waters degasser, a Waters 1525 HPLC pump with 717 plus autosampler, Waters 2410 RI detector and columns: Styragel, HT 3; HT 4. The calibration was performed with commercial polystyrene standards. Tetrahydrofuran (THF) was used as the mobile phase at a flow rate of 1.0 mL/min at 40℃.
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8

Characterization of PFS Samples

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1H NMR measurements were performed on an AVANCE DMX 500 spectrometer (Bruker, Karlsruhe, Germany). The solvent was dimethyl sulfoxide-d6 (DMSO)-d6 and the internal reference was tetramethylsilane.
FTIR measurements were recorded on a FTIR 8400s spectrometer (Shimadu, Kyoto, Japan) in KBr discs.
CD spectra were measured at 185–250 nm of wavelength, 100 nm min−1 rate, on a J-815 spectropolarimeter (Jasco, Tokyo, Japan). PFS samples were dissolved in phosphate-buffered saline (PBS; 50 mM, pH 7.4) and 50% (v/v) aqueous solution of TFE.
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