Optical rotations were measured on a JASCO P-1010 polarimeter with a 1 cm cell and circular dichroism spectrum was recorded on a JASCO J-1500 CD spectrometer (Jasco Corporation, Tokyo, Japan). The UV and IR spectra were acquired on a Varian Cary 50 and JASCO FT/IR 4100 spectrometers, respectively. The NMR spectra were measured on a Varian VNMRS 500 MHz spectrometer (Varian, Palo Alto, CA, USA) with a 3 mm ID probe in MeOH-d4 solvent, which was referenced by residual solvent peaks at δH 3.30 and δC 49.0). The high-resolution ESI mass spectrum was acquired by using a SCIEX X500R (Sciex Co., Framingham, MA, USA). The HPLC was performed using an Agilent 1200 system (Santa Clara, CA, USA) using Phenomenex polar C18 and YMC ODS-A columns and an ELSD detector. Quantum calculations were conducted by Dell PowerEdge R740 server (Dell, Round Rocks, TX, USA) installed Gaussian 16 (Gaussian Inc., Wallingford, CT, USA) and Spartan 20 (Wavefunction Inc., Irvine, CA, USA) software.
Vnmrs 500 mhz spectrometer
Manufactured by Agilent Technologies
Sourced in United States
The VNMRS 500 MHz spectrometer is a nuclear magnetic resonance (NMR) instrument designed for analytical chemistry and material science applications. It operates at a frequency of 500 MHz and provides high-resolution NMR spectroscopy capabilities for the characterization of chemical compounds and materials.
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Lab products found in correlation
Phenogel column, by Phenomenex (3 mentions)
1260 infinity 2, by Agilent Technologies (3 mentions)
Pmma standards, by Agilent Technologies (3 mentions)
5.0 μm guard column, by Phenomenex (3 mentions)
Cary 50, by Jasco (1 mentions)
P 1010 polarimeter, by Jasco (1 mentions)
J 1500 cd spectrometer, by Jasco (1 mentions)
Spartan 20, by Wavefunction (1 mentions)
Deuterated chloroform, by Merck Group (1 mentions)
2695 hplc, by Waters Corporation (1 mentions)
500 mhz spectrometer, by Agilent Technologies (1 mentions)
Orbitrap xl instrument, by Thermo Fisher Scientific (1 mentions)
Sure seal, by Merck Group (1 mentions)
Electrospray ion source, by Waters Corporation (1 mentions)
Sdt q600 simultaneous tga dsc, by TA Instruments (1 mentions)
Q200 differential scanning calorimeter, by TA Instruments (1 mentions)
6230 time of flight, by Agilent Technologies (1 mentions)
Mr 400 mhz instrument, by Agilent Technologies (1 mentions)
Specord s600 spectrometer, by Analytik Jena (1 mentions)
X band emx spectrometer, by Oxford Instruments (1 mentions)
14 protocols using vnmrs 500 mhz spectrometer
1
Structural Elucidation of Compounds
2
Polymer Molecular Weight Analysis by GPC
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Polymer molecular weight (Mw and Mn) and polydispersity (Đ) were measured by GPC using an Agilent 1260 Infinity II. Polymer samples were eluted through a Phenomenex 5.0 μm guard column (50 × 7.5 mm) preceded by two Phenomenex Phenogel columns (104 and 103 Å). GPC calibration was completed with Agilent PMMA standards. Polymers were prepared at 50:1 eluent/polymer ratio in DMF and filtered with a 0.45 μm PTFE filter. Polymer conversion was calculated by obtaining 1H NMR spectra using a Varian VNMRS 500 MHz spectrometer with mesitylene as an internal standard and processed using Mestrenova 11.0.4.
3
NMR Analysis of DP Oil
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NMR experiments were performed at room temperature on a Varian VNMRS 500 MHz spectrometer. Processing of the spectra was performed using the software MNova. For sample preparation, 200 µL of the DP oil was diluted in 400 µL of deuterated chloroform (Sigma-Aldrich 99.8%).
4
Polymer Molecular Weight Analysis by GPC
5
Multidimensional NMR and UV Analysis
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1H, 13C, APT, HMBC, and HSQC NMR data were acquired in deuterated dimethyl sulfoxide (DMSO-d6) and chloroform-d (CDCl3) at 25 °C (Varian VNMRS 500 MHz spectrometer). UV-1240 ultraviolet spectrometer (Shimadzu, Japan) uses MeOH and anhydrous sodium acetate (NaOAc) P.A. as displacement reagent.
6
Synthetic Procedures for Organic Compounds
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All commercial reagents were purchased from Sigma-Aldrich, Alfa Aesar, Apollo Scientific, or Fluorochem and of the highest available purity. Anhydrous solvents were purchased from Acros (AcroSeal) or Sigma-Aldrich (SureSeal) and were stored under nitrogen. Proton nuclear magnetic resonance spectra were recorded at 500 MHz on a Varian VNMRS 500 MHz spectrometer, at 30°C. Carbon Nuclear Magnetic Resonance spectra were recorded at 125 MHz on a Varian 500 MHz spectrometer. LCMS data were recorded on a Waters 2695 HPLC using a Waters 2487 UV detector and a Thermo LCQ ESI-MS. Samples were eluted through a Phenomenex Lunar 3μ C18 50 mm × 4.6 mm column, using water and acetonitrile acidified with 0.1% formic acid at 1 ml/min and detected at 254 nm. The gradient employed was a 10 min. method of 5-95% MeCN. Mass Spectra (HRMS) were recorded at the University of Sussex Mass Spectrometry Centre on a high-resolution Orbitrap-XL instrument (Thermofisher). All experiments were carried out under an inert atmosphere of N2 unless otherwise stated.
7
Comprehensive Analysis of Novel Compounds
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1H and 13C NMR spectra were obtained on a Varian VNMRS 500 MHz spectrometer. The molecular mass values of the compounds were analyzed by a Synapt G2 HDMS quadrupole time-of-flight (TOF) mass spectrometer equipped with an electrospray ion source (Waters, Milford, MA, USA) in positive ion mode. DSC results were obtained on a TA Instrument Q200 differential scanning calorimeter with a scan rate of 10 K min−1 under N2. TGA results were obtained on a TA Instrument SDT Q600 Simultaneous TGA/DSC with a heating rate of 10 K min−1 under N2. Melting points were observed on an Electrothermal 9300 melting point apparatus with a 1 K min−1 heating rate. Ionic conductivity was measured on a Novocontrol GmbH Concept 40 broad band dielectric spectrometer. Samples for dielectric relaxation spectroscopic measurements were placed on a 30 mm-diameter polished brass electrode and dried in vacuo at 100 °C for 24 h, after which a second polished brass electrode with 15 mm diameter was placed on top of the sample. Also, 50 μm silica-rod spacers were used to control the sample thickness. Data were collected in isothermal frequency sweeps every 5 K from 220 to 0 °C under a dry N2 flow. Frequency sweeps were performed isothermally from 10 MHz to 0.01 Hz for every measurement.
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1H and 13C NMR spectra were obtained on a Varian VNMRS 500 MHz spectrometer. The molecular mass values of the compounds were analyzed by a Synapt G2 HDMS quadrupole time-of-flight (TOF) mass spectrometer equipped with an electrospray ion source (Waters, Milford, MA, USA) in positive ion mode. DSC results were obtained on a TA Instrument Q200 differential scanning calorimeter with a scan rate of 10 K min−1 under N2. TGA results were obtained on a TA Instrument SDT Q600 Simultaneous TGA/DSC with a heating rate of 10 K min−1 under N2. Melting points were observed on an Electrothermal 9300 melting point apparatus with a 1 K min−1 heating rate. Ionic conductivity was measured on a Novocontrol GmbH Concept 40 broad band dielectric spectrometer. Samples for dielectric relaxation spectroscopic measurements were placed on a 30 mm-diameter polished brass electrode and dried in vacuo at 100 °C for 24 h, after which a second polished brass electrode with 15 mm diameter was placed on top of the sample. Also, 50 μm silica-rod spacers were used to control the sample thickness. Data were collected in isothermal frequency sweeps every 5 K from 220 to 0 °C under a dry N2 flow. Frequency sweeps were performed isothermally from 10 MHz to 0.01 Hz for every measurement.
8
NMR Characterization of Material Samples
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The NMR experiments were performed with the sample placed inside a 4 mm Zirconia rotor. The control experiments were performed on a silicone greased Si substrate with the empty rotor as well (i.e., inspecting probe and rotor background). 1H spectra and spin–spin relaxation times (T2) were measured using the spin-echo pulse sequence (π/2 − τ − π − τ − acquisition) conducted in a Varian VNMRS 500 MHz spectrometer operating at the resonance frequency of 499.8 MHz, with temperature at 25 °C. The inter-pulse delay (τ) of the spin-echo pulse sequence was varied from 67 to 4288 μs and 2048 transients were collected. T2 was calculated from the single exponential decay fit of the intensity of the deconvoluted and background-subtracted peaks as a function of 2τ. The acquisition parameters were π/2 pulse length of 2.5 μs and relaxation delay of 5 s. Chemical shifts are reported relative to tetramethylsilane at 0 ppm. The signal was deconvoluted as sum of Lorentz/Gaussian line-shapes. More details are described in the ESI.†
9
Spectroscopic Characterization of Molecular Compounds
10
Synthesis and Characterization of PVC-based Ion-Selective Membranes
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Chemical reagents and solvents for the synthesis were commercially purchased and purified according to the standard methods, if necessary. All inorganic salts were of analytical grade and were purchased from Fluka. The solutions of inorganic salts (0.01 M) were prepared with deionised water. High-molecular-weight poly(vinyl chloride) (PVC), o-nitrophenyl octyl ether (o-NPOE), and potassium tetrakis[3,5-bis(trifluoromethyl)phenyl]borate (KTFPB) were obtained from Fluka (Selectophore). Freshly distilled tetrahydrofuran (THF, Fluka) was used as a solvent for membrane components.
Thin layer chromatography (TLC) and preparative thin layer chromatography (PTLC) were performed using Merck Silica gel 60 F254 plates.
NMR experiments were carried out using a Varian VNMRS 500 MHz spectrometer ( 1 H at 500 MHz, { 1 H} 13 C NMR at
Thin layer chromatography (TLC) and preparative thin layer chromatography (PTLC) were performed using Merck Silica gel 60 F254 plates.
NMR experiments were carried out using a Varian VNMRS 500 MHz spectrometer ( 1 H at 500 MHz, { 1 H} 13 C NMR at
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