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35 protocols using eca 600 spectrometer

1

Spectroscopic Characterization of Materials

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FTIR spectra were obtained by using a Nicolet iS5 Thermo Fisher Scientific FTIR spectrophotometer (81 Wyman Street, Waltham, MA, USA). The samples were directly measured by ATR device using 60 scans to reduce the signal/noise ratio with a 2 cm−1 of resolution.
Solid state 13C-NMR spectra were acquired using a 14 Tesla Jeol ECA 600 spectrometer (Tokyo, Japan) operated at room temperature, with a rotor spinning speed set to 10 kHz. Samples were packed into a 4 mm I.D. Si3N4 rotor and measured in a two channels (H, X) solid state DOTY probe. 13C CPMAS NMR experiments were used at an operation frequency of 150.9 MHz and a 90° pulse width of about 3.08 µs. The CP contact time was 3 ms with a 10 s of acquisition delay.
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2

Synthesis and Characterization of Catalytic Compounds

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All solvents
used for the synthesis of the ligand and catalytic reaction (THF,
toluene, CH2Cl2, and MeCN) were purified over
a Glass Contour Solvent Dispending System under an Ar atmosphere.
Other reagents of the highest grade that were commercially available
were used without further purification. Atomic absorption analysis
was performed on a Shimadzu AA-6200. Elemental analysis was performed
on a Perkin-Elmer CHNS/O Analyzer 2400II. GC analysis was performed
on a Shimadzu GC2010 gas chromatograph with an Rtx-5 column (Restek,
length = 30 m, i.d. = 0.25 mm, and thickness = 0.25 μm). IR
spectra were recorded on a JASCO FT/IR 4200 spectrometer. NMR spectra
were recorded on a JEOL ECA-600 spectrometer. UV–vis spectra
of solution samples were recorded on a JASCO V650 spectrometer, and
solid reflectance spectra were recorded on the same instrument with
a PIN-757 integrating sphere attachment for solid. Nitrogen sorption
studies were performed at liquid nitrogen temperature (77 K) using
Micromeritics TriStar 3000. Before the adsorption experiments, the
samples were outgassed under reduced pressure for 3 h at 333 K.
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3

Multimodal Characterization of Novel Materials

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1H NMR spectra were recorded
on a JEOL ECA600 spectrometer. XRD measurements were performed using
a PANalytical X’Pert Pro MPD diffractometer with Ni-filtered
Cu Kα radiation (λ = 0.15418 nm). UV–vis measurements
were conducted using a Jasco V-650Q1 spectrometer. GPC analysis was
performed by using a pump NPL-5000 (Nihon Seimitsu Kagaku, Co. Ltd.)
and a TOSOH RI detector RI-8020 under the following conditions: a
Shodex GPC LF-804 column with DMSO as the eluent at a flow rate of
0.3 mL/min at room temperature. Pullulan samples were used as standards.
Dynamic viscoelastic measurements were conducted on a rheometer (Rheosol-G1000,
UBM). SEM images were obtained using a Hitachi S-4100H electron microscope.
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4

NMR Characterization of Polymers

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The spectra were acquired at ambient temperature on an ECA-600 spectrometer (JEOL Ltd, Tokyo, Japan) operating at 600 MHz (1H) or 150 MHz (13C). The polymers were dissolved in CDCl3 at a concentration of 2% (1H) or 15% (13C) (w/v). Tetramethylsilane (TMS) was used as an internal chemical shift reference. The 1H NMR spectra were obtained with a digital resolution of 0.36 Hz/point with 32 K data points together with a 45° flip angle and a 4 s pulse delay. For 1H homonuclear decoupling, the irradiation position was set to 1.57 ppm and the power was optimized to achieve the best results. The 13C NMR spectra were obtained with 1H broadband decoupling and a digital resolution of 1.44 Hz/point with 32 K data points together with a 45° flip angle and a 2 s pulse delay.
An analysis of the NMR intensities via different statistical models was conducted with a custom-written QuickBASIC program called MIXCO.PLA. The parameters were varied via a simplex algorithm by minimizing the mean deviation between the observed and calculated intensities. The flow chart and logic of the program were similar to the NMR tacticity and sequence analysis programs reported earlier [32 ,33 (link)]. Interested readers may write to the corresponding authors for a copy of the program.
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5

Analytical Methods for Chemical Characterization

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The optical rotations were recorded on a Rudolph Research Analytical Autopol III automatic polarimeter. UV spectrophotometric data was acquired on a Shimadzu PharmaSpec UV–visible spectrophotometer. NMR data were collected on a JEOL ECA-600 spectrometer operating at 600.17 MHz for 1H and 150.9 MHz for 13C. The edited-HSQC experiment was optimized for JCH = 140 Hz and the HMBC spectrum was optimized for 2/3JCH = 8 Hz. 1H NMR chemical shifts (referenced to residual CHCl3 observed at δH 7.25) were assigned using a combination of data from 2D DQF COSY and multiplicity-edited HSQC experiments. Similarly, 13C NMR chemical shifts (referenced to CDCl3 observed at δC 77.0) were assigned on the basis of multiplicity-edited HSQC experiments. The HRMS data were obtained using an Agilent 6210 LC-TOF mass spectrometer equipped with an APCI/ESI multimode ion source detector at the Mass Spectrometer Facility at the University of California, Riverside, California. Silica gel 60 (EMD Chemicals, Inc. 230–400 mesh) was used for column chromatography. All solvents used were of HPLC grade (Fisher Scientific).
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6

Analytical Characterization of Compounds

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Optical rotations were determined using a Jasco DIP–370 automatic polarimeter. The Fourier Transform Infrared spectra were measured using a Jasco Report–100 infrared spectrometer. The nuclear magnetic resonance spectra were recorded using a JEOL ECA 600 spectrometer (1H, 600 MHz; 13C, 150 MHz). Electrospray ionization mass spectrometry was recorded using an Agilent 1200 LC MSD trap spectrometer. Column chromatography was performed using a silica gel (Kieselgel 60, 70–230, and 230–400 mesh, Merck, Darmstadt, Germany), YMC RP-18 resins, and thin layer chromatography was performed using precoated silica-gel 60 F254 and RP-18 F254S plates (both 0.25 mm, Merck, Darmstadt, Germany); the spots were detected under ultraviolet light and using 10% H2SO4.
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7

Comprehensive Characterization of Powder Samples

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Powder XRD patterns were recorded on a RINT-Ultima III (Rigaku) using a Cu Kα X-ray source (40 kV, 40 mA). XPS spectra were taken by using a ULVAC-PHI ESCA 1700R (Al Kα radiation). Binding energy was calibrated with respect to C 1 s peak of a carbon tape at 284.8 eV. Field-emission scanning electron microscopic images of the powder samples were obtained on a Hitachi SU9000 microscope operated at 1 kV. TEM images of the powder samples were obtained on a JEOL JEM-2010F. 27Al MAS NMR spectra were obtained on a JEOL ECA-600 spectrometer. Elemental analyses of the samples were performed on an inductively coupled plasma-atomic emission spectrometer (ICP-AES, Shimadzu ICPE-9000).
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8

NMR Spectral Characterization of Desulphated Sample

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The NMR spectra were obtained from the sample (10 mg) after desulphation that was dissolved in D2O (0.5 mL). The 1H, and 13C NMR spectra of the sample were recorded on a JEOL ECA-600 spectrometer (JEOL, Akishima, Japan) at 70 °C at a base frequency of 150 MHz for 13C, and 600 MHz for 1H. Two-dimensional COSY, and HMQC experiments were processed using the pulse programs.
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9

Spectroscopic Analysis of Organic Compound

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Optical rotations were measured on a Perkin-Elmer 343 digital polarimeter. UV spectra were collected on a Hitachi U-3010 spectrophotometer. IR spectra were collected on a Thermo Nicolet IR100 Spectrometer with potassium bromide discs. NMR data was collected on a JEOL ECA-600 spectrometer operating at 600 MHz for 1H and 150.9 for 13C (g-HSQC; g-HMBC, 2D-g-DQF-COSY; 2D-NOESY, 1D-DPFGSE-NOE). Chemical shifts were recorded using an internal deuterium lock for 13C and residual 1H in CD2Cl2H 5.32, δC 54.0) or methanol-d4H 3.31, δC 48.0. The edited-g-HSQC spectrum was optimized for 140 Hz, and the g-HMBC spectrum was optimized for 8 Hz. High resolution mass spectrometry was performed using a JEOL AccuTOF DART mass spectrometer.
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10

Analytical Characterization of Compounds

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Unless otherwise noted, the following instruments and conditions were used. The 1H-NMR, 13C-NMR, and 2D-NMR spectra were recorded using an ECA-800 or ECA-600 spectrometer (JEOL), and chemical shifts were expressed in δ (ppm) with tetramethylsilane (TMS) as the reference standard. The LC/Orbitrap MS analysis was performed using an LC-20A UFLC system (Shimadzu) equipped with the LTQ Orbitrap XL mass spectrometer (Thermo Fisher Scientific). The UPLC/MS analysis was performed using a Xevo TQD UPLC/MS system (Waters). The LC/MS analysis was performed using an LC-20A UFLC system equipped with an LCMS-2020 mass spectrometer (Shimadzu).
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