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13 protocols using spectrum 100 series

1

Synthesis of Organometallic Catalyst Precursors

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Unless otherwise noted, all operations were
performed without taking precautions to exclude air and moisture.
The glass equipment was heated under vacuum to remove oxygen and moisture,
and then they were filled with argon. Starting compounds and reagents
were obtained from Merck, Fluka, Alfa Aesar, and Acros Organics; Ruthenium(III)
chloride hydrate, iridium(III) chloride hydrate, and α-terpinene
were obtained from Alfa Aesar, and dichloromethane, diethyl ether,
and toluene were obtained from Merck and Ridel de Haen. [IrCl2Cp*]2 was synthesized according to the published
procedures by a reaction of iridium(III) chloride and pentamethylcyclopentadiene.33 [RuCl2(p-cymene)]2 was prepared according to the method reported by Bennett
and Smith through the reaction of ruthenium(III) chloride with α-terpinene.34 (link) Catalytic reactions were carried out under the
inert atmosphere on Carousel 12 Plus Reaction Station system. 1H and 13C NMR spectra were recorded on a Varian
AS 400 Mercury instrument. Melting points were measured on Gallenkamp
electrothermal melting point apparatus without correction. FT-IR spectra
were recorded on a PerkinElmer Spectrum 100 series.
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2

Synthesis of Air-Sensitive Organometallic Complexes

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Reactions that
involved air-sensitive components were performed using a Schlenk-type
flask under argon atmosphere and high-vacuum line techniques. The
glass equipment was heated under vacuum to remove oxygen and moisture,
after which it was filled with argon. Ir(III) chloride hydrate, thioglycolic
acid, toluene, potassium carbonate, and 1,2,3,4,5-pentamethylcyclopentadiene
were obtained from Merck; Ru(III) chloride hydrate was obtained from
abcr; α-terpinene was obtained from Sigma; aniline was obtained
from Alfa Aesar; acetonitrile and dimethyl sulfoxide were obtained
from Carlo Erba. 1H, 13C, 2D 1H–1H gHSQC, and 2D 1H–13C gCOSY
NMR spectra were recorded on a Varian 400 MHz spectrometer. XRD analysis
was performed on a D8-QUEST diffractometer equipped with graphite-monochromatic
Mo–Kα radiation or a STOE IPDS-II diffractometer using
graphite-monochromated Mo–Kα radiation via the ω-scan
method. FT-IR spectra were recorded on a PerkinElmer Spectrum 100
series instrument. Melting points (m.p. values) were measured on an
Electrothermal IA9100 melting point apparatus. RuCl2(p-cymene)]2 was prepared according to the method
reported by Bennett and Smith through the reaction of Ru(III) chloride
with α-terpinene.44 (link) [IrCl2Cp*]2 was synthesized according to the published procedures
via a reaction between Ir(III) chloride and pentamethylcyclopentadiene.45
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3

FTIR Analysis of Pharmaceutical Formulations

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A Fourier transform infrared (FTIR) spectrophotometer (Perkin Elmer Spectrum 100 Series, Beaconsfield, UK) equipped with the Spectrum V 6.2.0 software was used to capture the spectra of the model drugs, excipients, placebo, and the optimized formulation in the transmission mode. Changes in the chemical backbone structure of each sample was recorded as spectra at a vibrational frequency range of 550–4000 cm−1. Each spectrum was generated as an average of 32 scans to achieve an acceptable signal-to-noise ratio and spectra resolution was maintained at 16 cm−1 [49 (link)].
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4

Green Synthesis and Characterization of AuNps

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A change in the color of the mixture (Chloroauric acid solution and plant extract) was observed soon after mixing. The mixture was incubated in a water bath for 24hrs at 40°C. The color of the mixture started changing from light reddish to dark reddish brown color which indicated the synthesis of AuNps. The characterization of green synthesized AuNps was carried out using UV-visible Spectrophotometer (Shimadzu 1600). The absorbance was measured at 200 nm, 400 nm, 600 nm, and 800nm. The structural characterization of green synthesized AuNps was identified through a scanning electron microscope (SEM: Jeol JSM-6510LV). FTIR spectrometric analysis (Perkin Elmer Spectrum 100 series) was also performed for synthesized BE-AuNps only because there was no characteristic peak observed for the IE-AuNps.
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5

FTIR Analysis of Solid Samples

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Samples were homogenized with potassium bromide (KBr) and ground into a powder. The mixture was transferred into a mold and pressed using a hydraulic press to form a KBr disc. FTIR spectra were recorded using a Perkin Elmer Spectrum 100 series in the range of 4000 to 450 cm−1 with a total accumulation of 16 scans.
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6

FTIR Characterization of PZA Formulations

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A Fourier transform infrared (FTIR) spectrophotometer (Perkin Elmer Spectrum 100 Series, Beaconsfield, UK) equipped with the Spectrum V 6.2.0 software was utilized for the characterization of PZA, all excipients, optimized drug loaded and placebo formulation samples. The FTIR spectra of each sample were recorded in the transmission mode at a frequency range of 550–4000 cm−1. Each spectrum was an average of 32 scans combined in order to achieve a satisfactory signal-to-noise ratio. In all cases, spectra resolution was maintained at 8 cm−1 and the gauge force at 150. The compatibility of the samples was checked and FTIR spectra documented for further analysis.
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7

Structural and Photocatalytic Analysis of CaCrO4

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X-ray diffraction
(XRD) using a DMAX-3A, instrument with Cu Kα radiation at a
wavelength of 1.54 Å was employed to investigate the structural
and phase analysis of the CaCrO4 chromite. The XRD spectrum
was scanned in a 2θ range of 10–80° with a step
size of 0.05°. The morphology of the sample was examined using
field emission scanning electron microscopy (FESEM, Zeiss Merlin),
and the elemental composition was determined by the energy-dispersive
X-ray (EDX) study. X-ray photoelectron spectroscopy (XPS) was conducted
using a ULVAC-PHI Quantera II instrument with Al K source having an
energy of 1486.6 eV to explore the chemical states of the elements
in the sample. The high-resolution spectra were fitted using the CasaXPS
software (Ver. 2.3.22PR1.0). The Shirley-type background with a Gaussian–Lorentzian
spectral line shape (30% Lorentzian component) was used in the curve-fitting
method. The binding energy of the “neutral” C peak,
including the C–C and C–H components, was used to calibrate
XPS spectra at 285.0 eV. FT-IR spectroscopy (Perkin Elmer Spectrum
100 series) was utilized to examine the chemical bonds and functional
groups in the sample. The photocatalytic performance of the CaCrO4 catalyst against rhodamine B dye was evaluated using a UV–Vis
spectrometer (Data Stream 3000 series) with different time intervals
ranging from 20 to 140 min with a time difference of 20 min.
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8

ATR-FTIR Analysis of Silane-Coated Steel Corrosion

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ATR-FTIR spectra were collected
using a PerkinElmer Spectrum 100 series FTIR spectrometer in the mid-IR
range from 4000 to 400 cm–1. The spectra were collected
for the intact silane deposited on the steel surface, the residue
of the biotic medium, and the corrosion product film that developed
on the silane-coated specimen pre-exposed to the anaerobic chloride
solution with SRB (biotic). For each test, 64 scans were performed
with a spectral resolution of 4 cm–1. Prior to the
collection of FTIR spectra, background scans were performed to be
subtracted from the collected FTIR spectra.
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9

FTIR Analysis of Film Samples

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A Fourier Transform Infrared (FTIR) spectrometer (Spectrum 100 series, PerkinElmer, Beaconsfield, UK) was used to obtain infrared spectra of the film samples. The analysis was conducted at wavelength range of 4000 to 380 cm−1 at spectra resolution of 4 cm−1 in the infrared region.
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10

Suzuki–Miyaura Cross-Coupling Reactions

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Unless otherwise noted, all operations were performed without taking precautions to exclude air and moisture. The glass equipment was heated under vacuum in order to remove oxygen and moisture and then they were filled with argon. Starting compounds and reagents were obtained from Merck, Fluka, Alfa Aesar and Acros Organics; pyridine, PdCl2 were obtained from Alfa Aesar and dichloromethane, acetonitrile, ethanol, diethyl ether, toluene, pyridine were obtained from Merck and Ridel de Haen. Catalytic reactions for Suzuki–Miyaura cross-coupling reactions were carried out under argon gas on Carousel 12 Plus Reaction Station system. 1H and 13C NMR spectra were recorded on a Varian AS 400 Mercury instrument. FTIR spectra were recorded on a PerkinElmer Spectrum 100 series. Scanning Electron Microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and metal mapping analyses were collected on a Thermo Scientific Apreo S.
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