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28 protocols using ft ir 6600

1

Structural and Compositional Characterization

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TEM micrographs were obtained with a field-emission TEM instrument (Hf-2000, Hitachi) equipped with an EDX detector (Kevex) operated at 200 kV. STEM images, elemental mapping, and line analysis were obtained using a JEOL-ARM 200F instrument equipped with a Kevex EDX detector (JED 2300T) operated at 200 kV. H2-TPR was conducted using a BEL-CAT (BEL Japan, Inc.) instrument by heating 50 mg samples at 5 °C/min from 50 °C to 600 °C under a 5.0% H2/Ar flow. These analyses were performed using as-deposited samples before H2 reduction. A TPD study using adsorbed CO was performed with a JASCO FT/IR-6600 instrument. In addition, in situ XAFS spectra and XRD patterns were acquired at the 01B1 beamline station in conjunction with a Si (111) monochromator at SPring-8, JASRI, Harima, Japan (proposal numbers 2019A1048 and 2019B1091). In a typical experiment, spectra were acquired, whereas a pellet sample was held in a batch-type in situ XAFS cell. XAFS data were processed using the REX2000 software program (Rigaku).
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2

Comprehensive Characterization of Materials

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SEM images were taken using an S-4800SE microscope at an acceleration voltage of 15 kV. FT-IR spectra were recorded using a Jasco FT/IR-6600. X-ray diffraction (XRD) patterns were collected using a Bruker D2 phaser (Germany) diffractometer with Cu Kα radiation. Nitrogen adsorption/desorption isotherms were obtained at 77 K on an ASAP 2010 apparatus. TEM analysis was performed using a Tecnai G2, (FEI, Netherland) microscope at an accelerating voltage of 200 kV, equipped with an EDS. X-ray photoelectron spectroscopy measurements were obtained using a Thermo Scientific, K–Alpha electron spectrometer with an Al X–ray source. Raman spectra were determined using a 532 nm laser Raman microscope (UniRAM, UniNanoTech., Korea). TGA was performed using a Tarsus® TG 209 F3 from room temperature to 1000 °C at a heating rate of 10 °C/min under nitrogen atmosphere.
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3

Characterization of ZnFe2O4 Nanoparticles

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The X-ray diffraction (XRD, Bruker, D8 Advanced, Madison, Wisconsin, USA) analysis at the scan rate of 1.2°/min and the 2θ range of 20°–80° was carried out. Cu Kα (λ = 1.54056 Å) was used as a radiation source and generated at 40 kV and 40 Ma. The crystallite size was measured using the Debye Scherrer formula [31 (link), 32 ]. Fourier transform infrared spectroscopy (FTIR) was performed to determine the stretching and bending vibrations of various bonds or functional groups in organic or inorganic materials. FTIR spectra in a range of 400–4000 cm− 1 were recorded using the FTIR spectrometer (JASCO FTIR-6600). Field emission scanning electron microscopy (FE-SEM, TESCAN, MIRA3, Institute of Space Technology, ISB) equipped with energy-dispersive X-ray spectroscopy (EDX), was conducted to assess the surface morphology and elemental compositions of ZnFe2O4 NPs. For this purpose, dried powder of ZnFe2O4 NPs was sprinkled on double-sided carbon-coated tape, followed by gold sputtering, to improve conductivity during imaging. FE-SEM images were captured under an acceleration voltage of 20 kV.
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4

Optical Characterization of Materials

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Fourier Transform Infrared spectroscopy (FTIR) measurements were performed using a JASCO FT/IR 6600 equipment in two different operation modes: (a) with a specular reflectance standard module RF-81S, scan range 1–1.7 μm with 1 cm−1 resolution using a TGS detector and aperture of 3.5 mm and (b) with an integrated sphere using an InGaAs detector, scan range 0.9–1.7 μm with 4 cm−1 resolution.
Reflection measurements at different incidence angles were performed using a variable angle spectroscopic ellipsometer (Woollam V-VASE). The Rs and Rp data, corresponding to s- and p-polarized incidence waves, were acquired from 0.3 to 1.35 μm with a 0.01 μm step, at three different angles: 35°, 60° and 75°.
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5

In-situ IR Analysis of Catalysts

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Operando IR analysis
was performed by means of the transmission method and an FT-IR spectrometer
(FT/IR-6600, JASCO) equipped with a mercury–cadmium–telluride
detector. A 20 mg sample of catalyst powder was pressed into a disk
(φ = 10 mm) and placed in a flow-type silica glass cell equipped
with CaF2 windows. The sample disk was then reduced at
500 °C for 1 h and cooled to 110 °C under He flow. IR spectra
were obtained at 1 min intervals for 30 min under a flow of the gas
mixture used in the operando XAFS experiment with or without the addition
of NH3.
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6

Comprehensive Materials Characterization Protocol

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X-ray diffraction (XRD) was conducted on a D2 PHASER (Bruker, Germany) and patterns were obtained using CuKα radiation. Fourier transform infrared (FTIR) spectroscopy was conducted by using a Jasco FT/IR-6600. The Brunauer-Emmett-Teller (BET) surface area analysis was conducted on a TriStar II (Micromeritics, GA, USA) was obtained from the N2 adsorption/desorption isotherm using a fully automatic physisorption analyzer. Scanning electron microscopy (SEM) was conducted on a Nova NanoSEM 450 (FEI, OR, USA) at an acceleration voltage of 5 kV. SEM-energy dispersive spectroscopy (EDS) mapping was performed using a QuantaX200 (Bruker). X-ray photoelectron spectroscopy (XPS, Thermo Scientific, K-Alpha) was conducted using an Al X-ray source. The UV-vis analysis was performed on a V770 spectrophotometer (JASCO). The pH of the solution was measured by using a JENWAY 3510 pH Meter.
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7

Electrochemical CO2 Reduction on BDD

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A thin 0.1% BDD film was deposited
on a Si attenuated total reflectance infrared (ATR-IR) prism using
MPCVD with the same method as mentioned before. The quality of the
BDD film was verified by Raman spectrum (Figure S3). A one chamber PTFE cell was used to perform the electrolysis
in which BDD, glassy carbon rod, and Ag/AgCl (KCl sat’d) were
set as the working electrode, counter electrode, and reference electrode,
respectively. Supporting electrolytes as 0.1 M H2SO4 and 0.1 M NaClO4 were used for the pretreatment,
while 0.5 M KCl for CO2RR. The ATR-IR spectra were measured
through a FT/IR-6600 (JASCO Corp.) with a liquid-nitrogen-cooled mercury-cadmium-telluride
detector. All of the spectra were collected at a resolution of 4 cm–1 and had 256 scans. The baseline spectrum and pretreated
comparison spectrum were measured in N2-saturated DI water.
After the electrolysis, the BDD electrode was washed by DI water for
three times, and then the ATR-IR spectrum was measured again in N2-saturated DI water.
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8

Coumarin-Initiated Photopolymerization of (Meth)Acrylates

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In this research, the ability of coumarins to initiate the photopolymerization of (meth)acrylate functions (FRP) was studied using two and three-component photoinitiating systems based on Coum/Iod salt (or NPG) (0.1%/1% w/w) and Coum/Iod/NPG (0.1%/1%/1% w/w/w). The percentage of the different chemical compounds is calculated according to the monomer weight. Kinetic study, as well as the reactive function conversion, were monitored by the evolution of the double bond vs. time. In fact, the polymerization experiments were performed in both thick (1.4 mm) and thin (25 µm) samples, they were obtained by deposition of the formulation into the mold (1.4 mm) or between two propylene films in order to reduce O2 inhibition, respectively. In addition, excellent solubility of all coumarin derivatives (excluding the CoumE) were observed. For the thick and thin samples, the evolution of the (meth)acrylate functions for TMPTA or Mix-MA were followed by RT-FTIR spectroscopy (JASCO FTIR 6600) at about 6150 cm−1 and 1630 cm−1, respectively. The procedure used to monitor the photopolymerization profile was described in detail in [30 (link),31 (link)].
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9

Advanced Materials Characterization Techniques

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Field-emission transmission electron microscopy (TEM; JEM-2100F; JEOL, Tokyo, Japan) was performed at an accelerating voltage of 300 kV. Ultraviolet (UV)-visible spectra were recorded on a Jasco V-770. Fourier-transform infrared (FT-IR) spectra were recorded using a Jasco FT/IR-6600. X-ray diffraction (XRD; D/Max-2500; Rigaku, Tokyo, Japan) patterns were collected using CuKα radiation. X-ray photoelectron spectroscopy (K-Alpha; Thermo Fisher Scientific, Waltham, MA, USA) was performed using an Al X-ray source. Thin-layer chromatography (TLC) was performed on silica-gel 60 F254 glass plates purchased from Merck Millipore (Billerica, MA, USA). PET images were taken using micro-PET (Genesys4; Sofie Biosciences, Culver City, CA, USA).
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10

Comprehensive Characterization of Functionalized Nanoparticles

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UV/vis absorption and fluorescence emission measurements were performed using a filter-based multimode microplate reader (Infinite F500; TECAN, Ltd, Männedorf, Switzerland). Transmission electron microscopy (TEM) analysis was carried out using a TEM (JEM-2100F; JEOL, Ltd., Tokyo, Japan) operated at 100 kV. Zeta potential and hydrodynamic particle size were measured by dynamic light scattering (DLS) using a Zetasizer Nano series (Malvern Inst. Ltd., Malvern, UK). Powder X-ray diffraction (PXRD) measurement was carried out using a RINT ULTIMA XRD (Rigaku Co., Tokyo, Japan) with a Ni filter and Cu-Kα source. Data were collected over 2theta = 5–60° at a scan rate of 0.01°/step and 10 s/point. Conjugation of the Ab to the NPs was confirmed via an ELISA and read through a plate reader from Bio-Rad (model 680, Hercules, USA). Fourier transform infrared spectroscopy was achieved using the FT/IR-6600 (JASCO, Tokyo, Japan).
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