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400 ultrashield spectrometer

Manufactured by Bruker
Sourced in Germany, United States

The 400 Ultrashield spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for analytical applications. It features a superconducting magnet that provides a stable and homogeneous magnetic field for precise spectral analysis. The spectrometer is capable of detecting and analyzing a variety of nuclei, including 1H, 13C, and other commonly used NMR-active isotopes. The instrument's core function is to facilitate the acquisition and processing of high-quality NMR data for chemical identification, structural elucidation, and other analytical purposes.

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16 protocols using 400 ultrashield spectrometer

1

Synthesis and Characterization of PCL-PEG Block Copolymers

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Block copolymers composed of PCL and PEG were synthesized. First, CL was polymerized by ring-opening polymerization (ROP) using mPEG as the initiator and Sn(Oct)2 as the catalyst. In a typical synthesis, mPEG (0.75 mmol) and Sn(Oct)2 (0.62 mmol) were dissolved in dried toluene under an argon atmosphere, followed by CL (32 mmol) addition. The reaction mixture was then stirred at 110 °C for 24 h. The reaction was stopped by the addition of cold diethyl ether to precipitate the polymer. The solid product was recovered via filtration and dried under reduced pressure at room temperature. In 1H-NMR (400 MHz, CDCl3, δ, ppm), the distinctive signals of PCL were as follows: 4.08 (t, J = 6.6), 2.33 (t, J = 6.6 Hz, 73H), 1.72–1.62 (m, 146H), 1.40 (m, 73H), and mPEG:3.66 (s, 494H).
The copolymers were characterized by 1H-NMR and GPC. The spectrum of copolymers was recorded on a 400 Ultrashield spectrometer operated at 400 MHz (Bruker, Mannheim, Germany) using CDCl3 as the solvent. The molecular weight distribution and polydispersity index (PDI) were determined by GPC using a high-performance liquid chromatography (HPLC) system (Thermoscitific, Ultimate 3000) equipped with a differential refractive index detector. Analyses were performed in THF at 0.8 mL/min flow rate in an HR 4E column. The calibration curve was constructed using polystyrene standards (2.5–50 kDa).
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2

NMR and SEC Characterization of Polymers

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The 1H NMR spectra were recorded on a Bruker 400 Ultra Shield spectrometer (Billerica, MA, USA). Size exclusion chromatography (SEC) was conducted on a Viscotek TDAmax (Malvern Instruments, Worcestershire, UK) consisting of a GPCmax integrated solvent sample delivery module, a TDA 302 Triple Detector Array (Malvern Instruments, Worcestershire, UK), and OmniSEC software (Version 10, Malvern Panalytical, Egham, UK). Further, 2 × PLgel 5 µm Mixed-C (200–2,000,000) columns were applied for separation. THF was used as the eluent at 1.0 mL/min and 30 °C, ad molecular weights were determined against polystyrene standards.
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3

Proton NMR Analysis using Bruker Spectrometer

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Proton nuclear magnetic
resonance measurements were performed on a Bruker 400 Ultrashield
spectrometer equipped with a Bruker SampleCase autosampler, using
CDCl3 as a solvent and TMS as an internal standard.
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4

Multimodal Characterization of Zeolite Materials

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Powder X-ray diffraction patterns were collected using a PANalytical X'Pert PRO MPD diffractometer equipped with a Cu Ka source at room temperature. TEM images were obtained with a Tecnai F30 microscope operated at 300 kV. HAADF-STEM and EDX measurements were carried out with a Hitachi HD-2700CS microscope or a Talos F200X both operated at 200 kV. Regarding the focus ion beam (FIB) milling, the zeolite sample was supported on a silicon wafer. Before milling, the sample was coated again with B1 mm carbon to protect the sample. The milling was done with a sequence decreasing milling current to avoid amorphization of the sample. The FIB-SEM investigation of the sample was done in the NVision 40 Station. The Si/Al ratio of the liquid was determined using a Varian SpectrAA 220FS atomic absorption spectrometer (AAS). Solid-state 27 Al MAS NMR was performed on a Bruker 400 UltraShield spectrometer operating at a resonance frequency of 104.29 MHz. The rotor was spun at 10 kHz and the spectra were recorded with a 4 mm MAS probe, with 3000 scans averaged for each spectrum. The chemical shifts were referenced to (NH 4 )Al(SO 4 ) 2 Á12H 2 O for aluminum. Solid-state 29 Si MAS NMR measurements were performed at a resonance frequency of 79.51 MHz. The rotor was spun at 10 kHz, with 3000 scans averaged for each spectrum.
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5

Synthesis of N-(2-Aminoethyl)-3-Octadecylaminopropionamide

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N-(2-amino-ethyl) -3-{ [2-(2-amino-ethylcarbamoyl) -ethyl] -octadecyl-amino} -propioamide (C18AA) was syn-thesized according to a previously published procedure. First, 10.22 g (0.12 mol) of methyl acrylate was added to 2.0 g (7.12 mmol) of octadecylamine in 15 mL of methanol. The solution was stirred at 40℃ for 3 days, and then the solvent and excess methyl acrylate were removed from the solution by rotary evaporation. 3-[ (2-Methoxycarbonyl-ethyl) -octadecyl-amino] -propionic acid methyl ester (C18ME) was obtained as a viscous liquid. Yield: 95%. Next, 3.2 g of C18ME and 17.8 g (0.30 mol) of ethylenediamine were dissolved in 15 mL of methanol and the mixture was stirred for 1 week at room temperature. Upon removal of the solvent and ethylenediamine by evaporation and freeze-drying, C18AA was obtained as a light yellow solid. The final product was recrystallized from the crude solid using a mixed solvent of toluene and methanol. Yield: 90%.
1 H-NMR (CDCl 3 ) : δ 0.88
. HRMS: calcd for C18AA (M+H + ) 498.47, found 498.48.
NMR spectra were recorded in CDCl 3 on a Bruker 400 Ultrashield spectrometer operating at 400 MHz.
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6

Synthesis and Characterization of BNIPP Derivatives

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BNIPPiProp, BNIPPiEth and trans,trans-BNIPDaCHM were synthesised according to the methods (with some modifications) previously described by Kong Thoo Lin and Pavlov. 10 The chemical structure, purity and stability of the derivatives were confirmed by TLC, NMR, MS and melting point determination. All reagents were purchased from Fisher Scientific or Sigma-Aldrich, unless otherwise stated. TLC was performed on silica gel 60 F254 aluminium plates (EMD/Merck) in chloroform/methanol (95 : 5). NMR was recorded on a Bruker 400 Ultrashield spectrometer operating at 400.1 MHz for 1 H and 100.6 MHz for 13 C. Accurate mass spectra were obtained by were obtained on Thermo Scientific LTQ Orbitrap XL or Waters Xevo G2-S analytical instruments (EPSRC National Mass Spectrometry Service Centre at Swansea University, Swansea).
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7

Structural Characterization of Coordination Polymers

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Single crystal X-ray diffraction data for the group 2, manganese and zinc coordination polymers were collected on an Agilent SuperNova Dual Atlas four-circle diffractometer with either a Cu source (SrL and BaL) or a Mo source (MgL, CaL, MnL and ZnL) and CCD detector. For Cu3L2, data were collected on a Bruker Apex II with a Mo source and CCD detector. Data integration and reduction was performed by the CrysAlisPro system software. All structures were solved by direct methods using Olex2 [30 ], with the ShelXT and ShelXS structure solution program [31 ,32 (link)], refined with the ShelXL refinement package using least-squares minimization [33 ]. The H atoms on water molecules could not be located, but are included in the formula sums. PXRD was collected at room temperature on an X'Pert PRO PANalytical Chiller 59 diffractometer using CuKα radiation. The samples were loaded onto zero-background silicon wafers directly from the reaction solution. TGA was performed using a PerkinElmer Pyris 1 thermogravimetric analyser. The samples were heated from 25°C to 600°C under a flow of air (20 ml min−1), using a heating rate of 5°C min−1. A SHIMADZU IRAffinitt-1S spectrometer was used to obtain IR data. 1H and 13C nuclear magnetic resonance spectra were recorded on a Bruker 400 UltraShieldTM spectrometer and referenced to the residual solvent peak.
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8

NMR, IR, and Mass Spectrometry Analysis

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The NMR spectra (1H and 13C) were recorded on a Bruker 400 UltrashieldTM spectrometer (Rheinstetten, Germany) and are provided in the supplementary material. The samples were solved in CDCl3 and TMS was used as an internal standard. IR spectra were obtained on a Thermo Nicolet FT-IR Nexus spectrophotometer (Thermo Nicolet, Madison, WI, USA) using KBr pellets for solids or NaCl plates for oil compounds. The HRMS spectra were recorded on a Thermo Scientific Q Exactive Focus mass spectrometer (Thermo Scientific™, Waltham, MA, USA) by direct infusion. For TLC assays, Alugram SIL G7UV254 sheets (Macherey-Nagel; Düren, Germany) were used. Column chromatography was performed with silica gel 60 (E. Merck KGaA, Darmstadt, Germany). Chemicals were purchased from E. Merck KGaA (Darmstadt, Germany), Panreac Química S.A. (Montcada i Reixac, Barcelona, Spain), Sigma-Aldrich Quimica, S.A. (Alcobendas, Madrid, Spain), and Acros Organics (Janssen Pharmaceuticalaan, Geel, Belgium).
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9

Synthesis and Characterization of Organic Compounds

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All the reagents and organic solvents used for synthesis were purchased from Fluka (Grenoble, France) and Merck (Darmstadt, Germany). Seeds of wheat, recommended as model crops, were used for seed germination toxicity test and were supplied by a local seed supplier in Galati city, Romania.
Melting points were recorded with a Stuart SMP10 instrument (Keison Products, Essex, UK). FTIR spectra were recorded from 4000 to 650 cm−1 with a Perkin-Elmer Spectrum 100 instrument (Perkin-Elmer, Shelton, CT, USA) by ATR (Attenuated Total Reflectance) technique on a CdSe crystal. 1H-NMR and 13C-NMR spectra were recorded with a Bruker 400 Ultrashield spectrometer (Bruker Daltonics, Hamburg, Germany) (at 400 MHz for 1H-NMR and at 75 MHz for 13C-NMR) operating at room temperature (298 K), using DMSO-d6 as the solvent and TMS as the internal standard. For the NMR data analysis, MestReNova software (Thermo Scientific, Waltham, USA) was used. Elemental analyses (C, H, N) were performed with a Fisons Instruments 1108 CHNS-O elemental analyzer (Thermo Scientific, Waltham, MA, USA).
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10

Spectroscopic Analysis of Sesquiterpenes and Derivatives

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The heartwood EO, PEE and DCME and natural sesquiterpenes (1–6) were analyzed according to previously described methods (Espinoza et al., 2016 (link), 2018 (link)). The synthetic derivatives 15-copaenyl acetate (6AC) and 15-copaenal (6OX) were analyzed by ATR-FT-IR and 1H- and 13C-NMR. The FT-IR spectra were recorded on a Perkin Elmer Spectrum 65 spectrometer. Both the 1H- and 13C-NMR spectra were recorded on a Bruker 400 Ultra Shield spectrometer (Bruker-Biospin GmbH, Germany) with the 5 mm NMR tube, using CDCl3 (99.8% D, contains 0.03% (v/v) TMS, Sigma-Aldrich, United States). 1H-NMR spectra were acquired using Bruker pulse program with the following settings: flip angle of 30°; relaxation delay (d1) = 0 s, size of fid = 32768, number of scans = 32, spectral width = 14.983 ppm, acquisition time = 5.4657 s, requested probe temperature = 300.0 K. 13C-NMR spectra were acquired using Bruker pulse program with the following settings: flip angle of 30°; relaxation delay (d11) = 30 ms and (d12) = 20 μs, size of fid = 16384, number of scans = 24166, spectral width = 240.049 ppm, acquisition time = 0.6783 s, requested probe temperature = 300.0 K. All data acquisition and processing were done with MestreNova 6.0.2 (Mestrelab Research, S.L., Santiago de Compostela, Spain).
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