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20 protocols using miniflex 2 diffractometer

1

Powder X-Ray Diffraction Analysis

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A Miniflex II Rigaku Diffractometer (Rigaku, Japan) with Ni-filtered
Cu Kα radiation (1.54 Å) was used for the PXRD analysis.
The tube voltage and tube current were 30 kV and 15 mA, respectively.
Powder was evened out on a zero-background silicon sample holder.
The diffractogram was collected between 5 and 40° 2 theta (2θ).
For qualitative purposes (n = 2), a step size of
0.05° and a stepping time of 1 s were used. For quantitative
phase analysis (QPA) by Rietveld refinement, a step size of 0.02°
and a stepping time of 1 s were used.
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2

Powder X-ray Diffraction Analysis

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Powder X-ray analysis was performed using a Miniflex II Rigaku diffractometer (The Woodlands, TX, USA) with Ni-filtered Cu Kα radiation (1.54 Å). The tube voltage and tube current used were 30 kV and 15 mA, respectively. The PXRD patterns were recorded (n=3) for 2 theta ranging from 5° to 40° at a step scan rate of 0.05° per second. Rigaku Peak Integral software was used to determine peak intensity for each sample using the Sonneveld-Visser background edit procedure.
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3

Powder X-ray Analysis of Mini-Tablets and Filaments

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Powder X-ray analysis was performed using a Miniflex II Rigaku diffractometer with Nie current used were 30 kV and 25 mA, respectively. The PXRD patterns were recorded (n=3) from 5° to 40° on the 2 theta scale at a step scan rate of 0.05° per second (Serrano et al., 2016) . Full mini-tablets and filaments were loaded in an open holder to avoid altering the PXRD signal by grinding (n=3). The NFD PXRD peak used was at 16.6 2 degrees, which was selected due to the lack of interference with other peaks in the diffractogram. Rigaku Peak Integral software was used for the determination of the peak intensity for each sample using the Sonnefelt-Visser background edit procedure.
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4

Powder X-Ray Diffraction Characterization

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Powder X-Ray Diffraction Powder X-ray analysis was performed using a Miniflex II Rigaku diffractometer with Nibe current used were 30 kV and 15 mA, respectively. The PXRD patterns were recorded (n=3) for 2 theta ranging from 5° to 40° at a step scan rate of 0.05° per second. Rigaku Peak Integral software was used to determine peak intensity for each sample using the Sonneveld-Visser background edit procedure.
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5

Advanced Materials Characterization

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Powder XRD data
of synthesized specimens were obtained using a Rigaku MiniFlex II
diffractometer (Cu Kα, λ = 1.5419 Å) working in the
Bragg–Brentano (θ/2θ) geometry. The data were obtained
within the 10–60° 2θ angle range with a speed of
1°/min. Fourier transform infrared spectra (FTIR) were recorded
in the range of 4000–400 cm–1 with a Bruker
ALPHA-FTIR spectrometer. Raman spectra were recorded using a combined
Raman and scanning near-field optical microscope WiTec Alpha 300 R
equipped with a 532 nm excitation laser source. Elemental composition
of synthesized compounds was determined using inductively coupled
plasma optical emission spectrometry (ICP–OES) with a PerkinElmer
Optima 7000 DV spectrometer. The morphology of synthesized powders
and elemental distribution were analyzed by scanning electron microscopy
(SEM) using a Hitachi SU-9000 microscope equipped with an energy-dispersive
X-ray spectrometer. Transmission electron microscopy (TEM) analysis
was performed on a JEOL JEM-2100F FEG TEM instrument.
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6

Synthesis and Characterization of Fe-Exchanged Y-Zeolite

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Na ion-exchanged Y-type zeolite (Na-Y) with SiO2/Al2O3 = 5.5 was supplied by Tosoh Co. The following chemicals were used as received: FeSO4∙7H2O (Wako, > 99%), sodium nitrate (Wako, 99.0%), ethylenediaminetetraacetate acid (TCI, 98.0%), ethylenediaminetetraacetate acid disodium salt (Wako, 99.5%), sodium hydroxide (Wako, 93%), 2,2′;6′,2″-terpyridine (TCI, 98.0%), methanol (Wako, 99.8%), 30% aqueous hydrogen peroxide (Wako, 30–35.5%), benzene (Wako, 99.5%), phenol (Wako, 99.0%), catechol (Wako, 99.0%), hydroquinone (Wako, 99.0%), o-dichlorobenzene (Wako, 98.0%), and acetonitrile (Wako, 99.5%).
ICP-AES and CHN elemental analyses of all catalysts were carried out after the sample was dissolved into a HF solution. The powder XRD patterns of the catalysts were collected on a Rigaku MiniFlex II diffractometer using CuKα radiation. The Brunauer–Emmet–Teller (BET) surface area measurements were conducted to determine the specific surface areas and pore diameters of the samples by performing N2 adsorption experiments at 77 K using a BEL Japan Bellsorp-max instrument. The UV-vis spectra were recorded on a Hitachi U-4000 spectrometer for solid samples. Gas chromatography (GC, Shimadzu GC-2014) was performed using a flame ionization detector equipped with a DB-1MS capillary column (internal diameter = 0.25 mm and length = 30 m) at the nature of the non-polar liquid phase.
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7

Multi-Technique Characterization of Materials

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Scanning electron microscope (SEM)
images were taken at an acceleration voltage of 5 keV and a working
distance of 15 mm using a JEOL JSM-7500F instrument. Transmission
electron microscopy (TEM) analysis was conducted using an FEI Tecnai
G2 F20 Super-Twin FE-TEM instrument operating at 120 kV. TEM samples
were prepared using a Tescan LYRA-3 Model GMH dual-beam FIB instrument.
X-ray diffraction (XRD) patterns were collected using a Miniflex II
diffractometer (Rigaku) with Cu Kα radiation (λ = 1.5406
Å) in the 2θ range of 5–40°. A Nicolet iS5
spectrophotometer equipped with iD7 ATR (Thermo Scientific) was used
to obtain attenuated total reflectance Fourier transform infrared
(ATR-FTIR) spectra at a resolution of 5 cm–1 with
16 scans in the span of 4000–400 cm–1. Thermogravimetric
analysis (TGA) was performed using a Q50 apparatus (TA Instruments)
in the temperature range of 25–800 °C at the heating rate
of 10 °C min–1 under an air flow of 60 cm3 min–1. N2 adsorption isotherms
were taken using an ASAP 2020 plus instrument (Micromeritics) at 77
K.
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8

Characterization of Barium-Borosilicate Glass Bioactivity

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The surface area, pore size,
and diameter of the BaBG were analyzed by the Brunauer–Emmett–Teller
(BET) and Barrett–Joyner–Halenda (BJH) methods during
nitrogen adsorption–desorption measurements (Quantachrome Instruments
NOVA 1000).24 (link) The mean diameter of synthesized
BaBG was determined using a particle size analyzer as previously reported.22 (link) Further, BaBG after incubation with SBF for
7 days was filtered followed by washing with deionized water and oven-dried
at 60 °C for 5 h. The formation of an HA layer was affirmed by
Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction
(XRD), and SEM–EDX. The phase analysis of BaBG before and after
treatment with SBF was determined by XRD (RIGAKU-Miniflex II diffractometer)
at 2θ, varying from 20 to 80° with a step size of 0.02°,
and the interpretation of peak was validated by utilizing the standard
JCPDS-International Centre for Diffraction Data Cards. Similarly,
the functional group present in BaBG and the newly formed HCA post
SBF treatment were characterized by FTIR (FTIR-8400S, SHIMADZU). The
surface morphology and changes in the elemental composition were evaluated
by SEM–EDX (EVO/18 Research, ZEISS).
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9

Characterization of Fe(III)-carboxylate Complexes

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All reagents and solvents were of the reagent grade purchased from ACROS or Aldrich. NMR spectra were recorded on Agilent 400MR spectrometer. Routine electrospray mass-spectra were obtained on a Thermo Finnigan TSQ Ultra instrument. High-resolution mass spectra were obtained on Thermo Q-Exactive LC/MS/MS System and on Agilent Technologies 6530 Accurate Mass QTofLC/MS (at the University of Texas at Austin mass-spectrometry facility). Dynamic light scattering (DLS) experiments were performed with a Malvern Zetasizer Nano ZS instrument combined with a MPT-2 automatic titrator. The initial concentrations were: FeIII: 1.5 mmolL‒1; 2: 2.25 mmolL‒1; salicylic and 5-hydroxyisophthalic acids: 4.5 mmolL‒1, NaOH (titrant): 0.25 M. In the experiments with Fe2O3 nanoparticles and 1 and 5, the initial [FeIII] was 5×10‒3M, [L] was 5.5×10‒4M, and titrations were done with 0.01M NaOH and HCl. The elemental analyses were performed by Galbraith, Inc. Powder X-ray diffractogram was obtained using Rigaku MiniFlex II diffractometer. TEM images were obtained on JEOL JEM 2010 transmission electron microscope. FT-IR spectra were obtained on Thermo Nicolet 380 spectrometer.
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10

Synthesis of Magnetic Gold Nanoparticles

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Firstly, 5 mg of dried magnetic nanoparticles were sonicated in 5 mL of water until fully dispersed. Then, 10 mL of 0.27 mol L−1 EDTA solution prepared in 1 mol L−1 NaOH was added, and MNPs were re-suspended by using an ultrasonic bath. Particles were collected with a magnet and dispersed in a 10 mL mixture of 0.1 mol L−1 CTAB and 0.01 mol L−1 HAuCl4 solution. Subsequently, the 150 mg hydroxylamine hydrochloride was added to the vigorously stirred solution in order to reduce AuCl4 ions to Au(0) on the surface of MNPs. The color of the solution changed from brown to dark red, indicating the formation of nanoparticles with gold shells (MNPs-Au). These particles were characterized by UV-vis spectrophotometer Lambda 25 (Perkin Elmer, Shelton, WA, USA) and transmission electron microscope (TEM) Tecnai F20 X-TWIN (Eindhoven, The Nederland). X-ray diffraction (XRD) measurements were performed using a MiniFlex II diffractometer (Rigaku, Japan). The diffractograms were recorded in the 2θ range from 25° to 80° using CuKα λ = 1.5406 Å radiation.
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