The PHA film obtained after dissolving in chloroform was pelletized using potassium bromide (KBr). FTIR spectrum was recorded for each pelletized sample in the sample chamber of FTIR spectrophotometer and was exposed to infra-red radiation. The obtained spectrum using Shimadzu 8400 S was in the spectral range of 4000–400 cm−1. 5 mg of PHA film was used for 1H NMR and characterized in Bruker Ascend 400 NMR spectrometer at 22 °C.
Ascend 400 nmr spectrometer
Manufactured by Bruker
Sourced in United States
The Ascend 400 NMR spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for various analytical applications. It operates at a frequency of 400 MHz and is capable of providing detailed information about the structure and properties of chemical compounds.
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Lab products found in correlation
Acd labs 10 freeware, by Advanced Chemistry Development (2 mentions)
Rf 5301pc spectrometer, by Shimadzu (1 mentions)
6210 esi tof ms instrument, by Agilent Technologies (1 mentions)
Tcs sp8 confocal microscope, by Leica camera (1 mentions)
Uv 2600 uv vis spectrophotometer, by Shimadzu (1 mentions)
Dsc 60 plus, by Shimadzu (1 mentions)
Topspin 4, by Bruker (1 mentions)
Vnmrs 500, by Agilent Technologies (1 mentions)
Avance 500 nmr spectrometer, by Agilent Technologies (1 mentions)
Microtof 2 spectrometer, by Bruker (1 mentions)
13 protocols using ascend 400 nmr spectrometer
1
Structural Characterization of PHA Films
2
NMR Characterization of Compounds 2-5
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1D and 2D NMR spectra of compounds 2 , 3 , 4 and 5 were obtained with a Bruker Ascend 400 NMR spectrometer (MA, USA). Bruker TopSpin 4.1.3 software or ACD/Labs 10 Freeware (Advanced Chemistry Development Inc., Ontario, Canada) was used to analyze the NMR spectra.
3
Analytical Techniques for Chemical Characterization
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The chemical
reagents were purchased commercially. The nuclear magnetic resonance
(NMR) was carried out using a Bruker Ascend 400 NMR spectrometer.
Absorption spectra were recorded using a UV-2600 UV–vis spectrophotometer
(Shimadzu). Fluorescence experiments were performed using a RF-5301PC
spectrometer (Shimadzu). HRMS was carried out using an Agilent 6210
ESI/TOF/MS instrument. Confocal fluorescence images were collected
using a Leica TCS SP8 confocal microscope.
reagents were purchased commercially. The nuclear magnetic resonance
(NMR) was carried out using a Bruker Ascend 400 NMR spectrometer.
Absorption spectra were recorded using a UV-2600 UV–vis spectrophotometer
(Shimadzu). Fluorescence experiments were performed using a RF-5301PC
spectrometer (Shimadzu). HRMS was carried out using an Agilent 6210
ESI/TOF/MS instrument. Confocal fluorescence images were collected
using a Leica TCS SP8 confocal microscope.
4
PHA Characterization via FTIR, NMR, and DSC
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For FTIR analysis, pelletization of the obtained PHA film was done by mixing up with potassium bromide (KBr). The pellet in the sample chamber of FTIR spectrophotometer was exposed to infra-red radiation with a spectral range of 4000–400 cm−1 (Shimadzu 8400 S). For NMR spectrum, 5 mg of PHA film was dissolved in deuterated chloroform with 1H NMR spectrum (Bruker Ascend 400 NMR spectrometer). DSC analysis was performed using DSC-60 plus (Shimadzu, Japan); the nitrogen flow of the instrument was 50 ml/min, which helped in minimizing the oxidative degradation of polyhydroxybutyrate (PHB) standard. A total of 5 mg of PHB standard in powder form wrapped in aluminum foil helped in minimizing thermal conductivity.
5
NMR Analysis of LAFO Compound
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NMR spectra were measured on a Bruker Ascend 400 NMR Spectrometer functioning at 400 MHz for 1H and 100MHz for 13C nuclei using typical experiments. Thirty mg of LAFO was pooled in an NMR tube after being dissolved in 2 mL CDCl3. On the other hand 500 mg of LAFO was submitted to liquid-liquid extraction using water-chloroform as a solvent system. The water layer rich in sugar was separated, lyophilized, dissolved in 2 mL D2O and then loaded onto an NMR tube. Coupling constants (J) are denoted in Hertz and the chemical shifts (δ) in ppm [24 (link)].
6
Characterization of Copolymer Composition
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Fourier transform infrared (FTIR) spectra were recorded on NEXUS 670 spectrometer (Nicolet, USA) with a resolution of 4 cm−1 to determine chemical composition of the synthesized copolymer. 1H nuclear magnetic resonance (1H NMR) was applied to investigate the chemical structure of products on Ascend400 NMR spectrometer (Bruker, CH) using tetramethylsilane as internal standard and d6-DMSO as deuterated solvent. Elemental analysis was carried out on a Vario MACRO Cube analyzer (Elementar, Germany) to determine the monomeric ratio and the degree of protonation of the synthesized copolymers.
7
NMR Spectra Acquisition Protocol
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NMR spectra were recorded at 400 MHz 1H NMR and 101 MHz 13C NMR in a Bruker Ascend™ 400 NMR spectrometer in different deuterated solvents at 30 °C with the solvent signals as an internal reference.
8
NMR Spectroscopy Analysis of Compounds 1 and 2
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1D and 2D NMR spectra of compounds 1 and 2 were obtained with a Bruker AVII500 NMR spectrometer (Billerica, MA, USA). 1D NMR spectra of the hexane fraction of J. insularis were obtained with a Bruker Ascend 400 NMR spectrometer. ACD/Labs 10 Freeware (Advanced Chemistry Development Inc., Toronto, ON, Canada) or Bruker TopSpin 4.1.3 software was used to analyse the NMR Spectra.
9
Synthesis of Antimony Chloride Complexes
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Ph3SbCl2 and
Mes3SbCl2 were prepared according to reported
procedures.21 (link) Solvents were dried by reflux
under N2 over Na/K (pentane and THF). All other solvents
were used as received. Commercially available chemicals were purchased
and used as provided (commercial sources: Aldrich for SbCl3, Matrix Scientific for biphenyl, and TCI Chemicals for Ph3PO). Ambient-temperature NMR spectra were recorded on a Varian Unity
Inova 500 FT, a Bruker Avance 500 NMR spectrometer, or a Varian VnmrS
500 for the DOSY experiments (500 MHz for 1H and 126 MHz
for 13C). A Bruker Ascend 400 NMR spectrometer (400 MHz
for 1H and 101 MHz for 13C) was also used for
some of the spectra. 1H and 13C NMR chemical
shifts are given in ppm and are referenced against SiMe4 using residual solvent signals used as secondary standards. Elemental
analyses were performed at Atlantic Microlab (Norcross, GA).
Mes3SbCl2 were prepared according to reported
procedures.21 (link) Solvents were dried by reflux
under N2 over Na/K (pentane and THF). All other solvents
were used as received. Commercially available chemicals were purchased
and used as provided (commercial sources: Aldrich for SbCl3, Matrix Scientific for biphenyl, and TCI Chemicals for Ph3PO). Ambient-temperature NMR spectra were recorded on a Varian Unity
Inova 500 FT, a Bruker Avance 500 NMR spectrometer, or a Varian VnmrS
500 for the DOSY experiments (500 MHz for 1H and 126 MHz
for 13C). A Bruker Ascend 400 NMR spectrometer (400 MHz
for 1H and 101 MHz for 13C) was also used for
some of the spectra. 1H and 13C NMR chemical
shifts are given in ppm and are referenced against SiMe4 using residual solvent signals used as secondary standards. Elemental
analyses were performed at Atlantic Microlab (Norcross, GA).
10
Comprehensive Characterization of SiO2 Nanoparticles
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Fourier transform infrared (FT-IR) spectra of all samples were measured with KBr pellets on a FTS-3000 spectrophotometer (Digilab, America) from 4000 to 500 cm−1. The 1H NMR experiment was performed on a Bruker ASCEND-400 NMR spectrometer with D2O as solvent. The morphologies of solution samples were obtained by scanning electron microscope (SEM, SU800, Japan). The size and morphology of SiO2 nanoparticle were determined by transmission electron microscope (TEM, JEM-2100, Japan) at an accelerating voltage of 200 kV. Particle size distribution of the SiO2 nanoparticle was determined using a dynamic light scattering spectrophotometer (DLS, Qudix, Scatteroscope I system, Korea) at 25 °C. Thermal gravimetric analysis (TGA) in nitrogen atmosphere was conducted with a Diamond TG/DTA synchronal thermal analyzer (America). The samples were heated from 25 to 700 °C at a heating rate of 10 °C min−1 under a N2 flow rate of 140 cm3 m−1.
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