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9 protocols using raman station 400

1

Coupled DSC-Raman Analysis of Molecular Interactions

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A power compensation DSC (Perkin-Elmer DSC 8500) connected to a Raman spectrometer (Perkin-Elmer Raman Station 400) through a DSC-Raman interface probe was used. The laser irradiation of the samples and scattering collection from the samples were conducted through glass fibers to minimize the laser irradiation area and to avoid temperature changes. Laser irradiation was configured to 100 mW for 4 s with a heat flow amplitude of less than 8 mW or 0.03 °C [59 (link)]. The collection of Raman spectral data ranged from 3200 to 200 cm−1. DSC-Raman measurements were carried out from 25 to 190 °C at a heating rate of 2 °C min−1. The samples (4 mg) were placed in an Al pan, and a SiO2 disk was placed on the sample to minimize the effect of sample thickness on Raman intensity. MeCD was used as received.
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2

Raman Spectroscopy for Catalyst Quantification

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UV–vis absorption spectroscopy
was carried out using a ThermoSpectronic Aquamate UV–Vis spectrometer.
Online reaction monitoring with Raman spectroscopy was performed on
a PerkinElmer RamanStation 400 benchtop Raman spectrometer (350 mW
near-infrared 785 nm laser delivering 100 mW at the sample), which
was coupled with a standard Raman fiber probe at an excitation wavelength
of 785 nm. The internal response factor (IRF) in Raman of the FePcS
complex with Na2SO4 as the internal standard
(IS) was calculated using eq 3 where CIS is the
concentration of the internal standard, Na2SO4 (M), and CFePcS is the concentration
of the catalyst, FePcS (M).
The IRF was determined to be 819.9
for FePcS. The concentration of FePcS was calculated using eq 4 The conversion of FePcS was then calculated
using eq 5 The conversion of FePcS
during the initial
reaction phase was calculated using eq 6 where CFePcS,added is the concentration of the FePcS
added (M) and CFePcS,0 is the concentration
of the FePcS directly after
addition to the mixture (M).
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3

Characterization of PET Degradation Products

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To remove the water, terephthalic acid (TA), bis(2‐hydroxyethyl) terephthalate (BHET), dimethyl terephthalate (DMT) and poly(ethylene terephthalate) PET as standards were lyophilized for 24 h; 50 mg of samples was incubated with different volumes of pure triethylamine in 10 ml of chloroform for 6 h. Afterwards, chloroform was removed by evaporation at 21 °C for 24 h. The virgin material and the powders obtained from the chemical process and after the enzymatic treatment were also incubated as described above. The FT‐Raman spectra were recorded using a Perkin‐Elmer Raman station 400, coupled with a 785 nm laser. Spectra were collected at a resolution of 2 cm−1 for 25 scans and normalized in the region 2200–2400 cm−1 before any data processing. The bands were assigned as follows: 3000–2700 cm−1 ν(Et‐NH4+), 1728 cm−1 ν(C=O, bended), 1632–1604 cm−1 νas(C=O), single band 1398 cm−1 δ(C‐O), single band 1286 cm−1 coupled mode ν(C=O)+δ(COH).
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4

Raman Mapping of Lipid Mixtures

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The samples were prepared by heating the solid lipids (CP, MM) 10 °C above their melting temperatures, followed by addition of the liquid lipid (TRANS, DK) under stirring until a visually homogeneous mixture was obtained. The concentration of the liquid lipid was set to 30% (w/w) for the analyses. The samples were cooled to room temperature in an aluminum cell and an area of 1.95 × 1.95 mm2 was mapped in a Raman Station 400 (Perkin Elmer, Waltham, USA) using a laser of 785 nm as an excitation light and nominal power of 100 mW. The exposure time was set at 3 s/pixel, 2 exposures/pixel, 50 µm pixel size, in the spectral range of 3200–600 cm−1, with 4 cm−1 resolution. Each sample provided a data cube whose dimension was 40 × 40 × 651, where 40 represents the number of pixels at x and y axis, and 651 is the number of spectral variable/Raman shift.
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5

Raman Characterization of Abexinostat Tosylate

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Example 5

Form 1 of abexinostat tosylate was characterised by Raman spectroscopy. The spectra were recorded in diffuse reflectance mode (Raman Station 400, PerkinElmer) using a 785 nm laser. The signal was recorded by a CCD detector. The wavelength shift depends on the material and is characteristic of that material, which allows analysis of the chemical composition and of the molecular arrangement of the sample studied. The spectra were acquired with maximum power (100% laser capacity), a spot size of 100 μm, twenty exposures of 2 seconds and a spectral resolution of 2 cm−1. The spectral range explored ranges from 0 to 3278 cm−1.

Significant peaks were observed at the following positions: 940 cm, 1088 cm−1, 1132 cm, 1242 cm−1, 1360 cm−1, 1608 cm−1.

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6

Synthesis and Characterization of Yb2O3.CuO@rGO

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All necessary chemicals, including ascorbic acid, copper (II) nitrate, ytterbium (III) nitrate, sodium hydroxide, reduced graphene oxide, NaH2PO4, Na2HPO4, citric acid, glucose, uric acid, dopamine, sodium chloride, and calcium nitrate, were purchased from Sigma–Aldrich, and utilized exactly as they were given. All solutions were made using double-distilled water. The XPS investigation of Yb2O3.CuO@rGO was performed using a MgKα spectrometer (JEOL, JPS 9200) in the subsequent circumstances: pass energy = 50 eV (wide-scan) and 30 eV (narrow-scan), Voltage = 10 kV, Current = 20 mA. A PANalytical X-ray diffractometer was used to acquire X-ray diffraction (XRD) spectra with Cu Kα1/2, λα1 = 154.060 pm, λα2 = 154.439 pm radiation. A “Raman station 400 (Perkin Elmer)” spectrometer was used to acquire the Raman spectra. A FE-SEM (JEOL-6300F, 5 kV) was used to analyze the morphology and structural characteristics of Yb2O3.CuO@rGO. EDS (JEOL) was used to investigate the elemental composition of the Yb2O3.CuO@rGO. A JEOL JEM-2100F-UHR field emission apparatus fitted with a Gatan GIF 2001 energy filter and a 1 k-CCD camera was used to capture transmission electron microscopy (TEM) micrographs at 200 kV. Electrochemical measurements were conducted using a Zahner Zennium potentiostat.
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7

Characterization of PCL-CIP-NP Microspheres

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The PCL–CIP–NP microspheres were characterized using a Fourier transform infrared spectrometer (Spectrum 400; PerkinElmer Inc., Waltham, MA, USA) equipped with a universal attenuated total reflectance sampling accessory (PerkinElmer Inc.). The samples were also measured by dynamic light scattering (DLS) measurements. The DLS measurements were performed on a Zetasizer Nano S (Malvern Instruments, Malvern, UK) equipped with an HeNe laser at 632.8 nm and a scattering detector at 173°C using water as a dispersant (refraction index =1.33 and viscosity =0.8872) at the room temperature with cumulants analysis. Raman spectra of the synthesized NPs were obtained using a Raman spectrometer (RamanStation 400; PerkinElmer Inc.) equipped with an excitation source of 350 mW near-infrared 785 nm laser. The spectra were obtained from 100 cm−1 to 1,800 cm−1 with a peak resolution of 4 cm−1. The solutions of NPs and PCL–CIP–NPs were dropped and dried overnight on carbon-coated Formvar 200 mesh copper grids (Ted Pella, Inc., Redding, CA, USA). The grids were visualized using a Philips 400 120 keV transmission electron microscope (TEM; Philips, Hillsboro, OR, USA) with a high-tilt goniometer stage.
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8

Multifaceted Characterization of Nanomaterials

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Transmission electron microscopy (TEM) was conducted at 200 kV with a JEOL JEM-2100 F-UHR field-emission instrument (Tokyo, Japan) equipped with a Gatan GIF 2001 energy filter (Pleasanton, CA, USA) and a 1 K CCD camera in order to obtain EEL spectra. Field emission scanning electron microscope (FE-SEM) images were carried out with a FE scanning electron microanalyzer (JEOL-6300 F, 5 kV). X-ray diffraction (XRD) data were acquired on a PANalytical X’ port diffractometer using CuKα1/2, λα1 = 154.060-pm and λα2 = 154.439-pm radiation. Raman spectroscopy was carried out using a Perkin Elmer Raman Station 400 (Waltham, MA, USA). The nitrogen adsorption and desorption isotherms were measured at 77 K using a Quantachrome Autosorb 3B after the samples were vacuum-dried at 200°C overnight. The sorption data were analyzed using the Barrett-Joyner-Halenda (BJH) model with Halsey equation [26 ]. Fourier transform infrared spectroscopy (FTIR) spectra were recorded with a Bruker FRA 106 spectrometer (Ettlingen, Germany) using the standard KBr pellet method. Reflectance spectrum was taken at room temperature using UV-visible spectrophotometer (lambda 950 Perkin Elmer) fitted with universal reflectance accessory in the range of 200 to 800 nm and using BaSO4 as reference.
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9

Comprehensive Characterization of Carbonized Nanofibers

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Several characterization tools were used to characterize the CNFs. Morphologies of nanofibrous mats were investigated with JSM-7500F field emission scanning electron microscopy and the diameter distribution of each sample was obtained from 50 randomly selected nanofibers that were image-analyzed (ImageJ software). The structure of carbonized nanofibers was characterized by X-ray diffraction patterns (XRD, Philips, Netherlands) using Cu-Kα radiation (wavelength λ = 1.54 Å) and Raman spectra (Raman-Station 400, PerkinElmer, MA, USA). Chemical surface composition of carbonized samples was characterized by X-ray photoelectron spectroscopy (XPS, ESCALAB 250Xi, Thermo Fisher, USA) with a monochromated Al Kα X-ray source of 1486.6 eV. The Brunauer–Emmett–Teller (BET) specific surface areas and the density functional theory (DFT) pore size distribution of carbonized samples were determined using N2 adsorption–desorption (ASAP 2020 Plus HD88, Micromeritics, USA) at −196 °C after outgassed at 300 °C for 6 h under vacuum.
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