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Biospin nmr spectrometer

Manufactured by Bruker
Sourced in Germany

The BioSpin NMR spectrometer is a laboratory instrument designed for nuclear magnetic resonance (NMR) spectroscopy. It is capable of analyzing the chemical and structural properties of materials, including biological samples, through the detection and measurement of nuclear magnetic resonances.

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5 protocols using biospin nmr spectrometer

1

Characterization of Grafted PCL in MCC-g-PCL Copolymers

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The contents of grafted PCL in MCC-g-PCL copolymers were characterized by 1H nuclear magnetic resonance (NMR) spectroscopy. 1H NMR spectra were recorded at 400 MHz using a Bruker BioSpin NMR spectrometer (Bruker Company, Germany) in dimethyl sulfoxide-d6 (DMSO-d6) solvent. The chemical shifts were calibrated against the internal standard signals of tetramethysilane (TMS). 13C NMR spectra were acquired on a Bruker BioSpin NMR apparatus at 100 MHz, at ambient temperature, using TMS as the internal standard and DMSO-d6 as solvent.
Raman spectroscopy was conducted on a Renishaw InVia Reflex Raman system. The Raman scattering was excited using a diode laser at a wavelength of 785 nm. The laser beam was focused on the sample with a 100 an0.85 microscope objective. The laser power at the sample was 320 mW. The exposure was 10 s and two accumulations of Raman measurements were carried out. In addition, an optical microscope was coupled to the system.
The molecular weight and molecular weight distribution of prepared MCC-g-PCL were measured on a Waters 5510 gel permeation chromatograph (U.S.A.). DMSO was used as eluent at a flow rate of 0.5 mL min−1 at 50 °C. The SEC system was calibrated with linear polystyrene standards.
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2

Purification and Characterization of Organic Compounds

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All chemicals used were purchased pure from commercially available sources such as Sigma Aldrich, VWR, Fisher or other chemical vendors. 1H NMR (300 MHz) spectra were recorded on a Bruker Biospin NMR spectrometer. Thin layer chromatography was performed using Whatman silica gel 60 Å plates with florescent indicator and visualized using a UV lamp (254 nm) or KMnO4 stain. Flash chromatography was performed on Grace with GraceResolve Normal Phase disposable silica columns. High performance liquid chromatography (HPLC) was performed on a Gilson 322 HPLC pump with a Gilson UV/VIS-155 detector and a Phenomenex Gemini C18 column (10 µm, 250 mm × 10 mm). Liquid chromatography electrospray ionization mass spectroscopy (LC–MS/ESI–MS) were acquired on an Agilent LC/MSD-SL with an 1100 HPLC and G1956B mass spectrometer with a Phenomenex Gemini 5 μm C18 110 Å 50 × 3 mm column.
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3

NMR Spectroscopy Characterization Protocol

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NMR spectra were
recorded on a BRUKER BIOSPINNMR spectrometer (400 MHz). Chemical shifts
are reported in parts per million (ppm) relative to internal standard
residual solvent peaks (DMSO-d6 = 2.5
ppm, methanol-d4 = 3.31 ppm, chloroform-d = 7.27 ppm).1H NMR coupling constants (J) are reported in hertz (Hz), and multiplicity is indicated
as follows: s (singlet), d(doublet), t (triplet), and m (multiplet).
HRMS were obtained on an instrument named Aglient 7250& JEOL-JMS-T100LP
AccuTOF. Purities of the tested compounds determined by HPLC. Preparative
HPLC was carried out on 250 × 10 mm C-18 column using gradient
conditions (50–100% B, flow rate = 1.0 mL/min, 10 min, detection
at 245 nm). The eluents were as follows: solvent A (H2O)
and solvent B (CH3OH).
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4

Synthesis and Characterization of (E)-2-(Prop-2-yn-1-yloxy)benzaldehyde O-Methyl Oxime

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All commercial reagents were ACS grade reagents and used without further purification from freshly opened containers. All solvents were distilled prior to use. Melting points were determined in an open capillary tube with Buchi M-580 melting point apparatus. Infrared spectra were recorded as ATR on a P Agilent Cary 630 FT-IR spectrophotometer. NMR spectra were recorded on a Bruker BioSpin NMR spectrometer at 400 or 600 MHz ((1H NMR), 101 or 150 MHz (13C NMR), 376 MHz (19F NMR)). Chemical shifts are reported in parts per million (ppm). High-resolution mass spectrometry measurements were performed using a Shimadzu LCMS-9030 Q-TOF mass spectrometer, coupled with LC-30 UHPLC system. X-ray crystal analysis was performed by Rigaku XtaLAB Synergy, single source at home/near, HyPix using CuKα radiation (λ = 1.54184 Å) at 105 K. Please see the supporting information or the cif file for more detailed crystallography information. The (E)-2-(Prop-2-yn-1-yloxy)benzaldehyde O-methyl oxime 5 was prepared according to the reported procedure [74 (link)].
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5

Compound Purification and Structural Analysis

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Reverse-phase HPLC-PDA analyses was performed at 280 nm UV absorbance using a C 18 column packed with YMC-Pack ODS-AQ; 4.6 mm internal diameter, 150 mm long and 5 μm particle size long, connected to photo diode array (PDA) on binary condition consisting of solvent A (0.05% trifluoroacetic acid buffer-TFA), water, and 100% acetonitrile maintained at a flow rate of 1 ml/min for a 25-min program. The acetonitrile was set throughout as 0-40% (0-15 min), 40-75% (15-20 min), 75-0% (20-25 min). The purification of compounds was carried out by preparative HPLC with a C 18 column (YMC-PACK ODS-AQ; 150-250 mm long, 20 mm internal diameter, 10 μm particle size) connected to a UV detector using a 36-min binary program. The flow was 10 ml/min throughout the program as acetonitrile flowed for 0-20 min (40%), 20-30 min (75%), 30-36 min (0%).
The high resolution quadruple-time of flight electrospray ionization-mass spectrometry (HRQTOF-ESI/MS) was performed in positive-ion mode using Acquity mass spectrometer (with UPLC; Waters, USA) coupled with a Synapt G2-S system (Waters). The purified compounds were structurally determined by Avance II 300 Bruker (Germany) BioSpin NMR spectrometer equipped with a TCI CryoProbe (5 mm). All the samples were exchanged with D 2 O and dissolved in methanol-d 4 for 1 H NMR (proton), 13 C NMR (carbon).
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