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16 protocols using asap 2020 instrument

1

Characterization of Sulfur Samples

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The content of sulfur was analysed using a thermogravimetric analyser (Diamond PE) under an Ar atmosphere at a heating rate of 10°C min−1 from room temperature to 600°C, with a gas flow-rate of 40 ml min−1. Scanning electron microscope (SEM) observation was carried out on a FEI Quanta 650 SEM operated at 20 kV. Scanning transmission electron microscopy (STEM) was conducted with a Hitachi S-5500 SEM, and energy-dispersive X-ray spectroscopy was applied for collecting elemental signals and mapping. Transmission electron microscopy (TEM) and high-resolution TEM images were recorded with a JEOL-2100 instrument. Powder X-ray diffraction (XRD) was conducted on a Bruker D8 Advance X-ray diffractometer using Cu Kα radiation at a scanning rate of 4° min−1 in the 2θ range from 10° to 70°. Specific surface area, pore volume and pore-size distribution were determined by the Brunauer–Emmett–Teller (BET) method on a Micromeritics ASAP 2020 instrument.
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2

Characterization of Microcapsule Morphology

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The surface morphology of the microcapsules was investigated via scanning electron microscopy (SEM) using a Hitachi S4800 microscope (Tokyo, Japan). The powders were previously fixed on a brass stub using double-sided adhesive tape, and then were made electrically conductive by coating under a vacuum with a thin layer of platinum (approximately 3–5 nm) for 3 min at 30 W. Images were taken in decelerating mode at a voltage of 0.5 kV. Elemental mapping was carried out via energy dispersive X-ray analysis (EDX) to provide the spatial distribution and composition of the palladium in the samples.
Nitrogen adsorption–desorption isotherms were recorded using an automated Micromeritics ASAP2020 instrument (Norcross, GA, USA). Prior to the adsorption measurements, the samples were outgassed in situ under a vacuum (10–6 Torr) at 120 °C for 15 h to remove adsorbed gases.
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3

Characterization of Strontium-Substituted Hydroxyapatite Nanofibers

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The structure of the mSrHANFs was observed using scanning electron microscopy (SEM, ZEISS SIGMA, Dresden, Germany) and transmission electron microscopy (TEM, JEOL JEM-2100, Tokyo, Japan). The average diameter of the mSrHANFs was analyzed using SEM images with image analysis software (Image-Pro Express Version 6.0, Media Cybernetics, Rockville, MD, USA). The phase composition of the mSrHANFs was characterized by X-ray diffraction (XRD, Bruker D2-Phaser, Madison, WI, USA), SEM-energy dispersive spectrometry (SEM-EDS), and Fourier transform infrared spectroscopy (FTIR, Bruker tensor II, Madison, WI, USA). The nitrogen adsorption–desorption experiment was performed to obtain the Brunauer-Emmett-Teller (BET) specific surface area and pore size (Micromeritics ASAP 2020 instrument, Norcross, GA, USA). The chemical compositions of the mSrHANFs were analyzed by inductively coupled plasma–optical emission spectrometry (ICP-OES, Agilent Technologies, Santa Clara, CA, USA).
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4

Characterization of Vaterite Microspheres

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The morphologies of the microsphere samples were characterized with scanning electron microscopy (SEM, S-4800, Hitachi, Tokyo, Japan). The samples were sputter coated with platinum and then measured with SEM at 3 kV. The polymorph of the vaterite samples was assessed with X-ray diffraction (XRD). The XRD measurement was conducted with an X-ray diffractometer (X’Pert-Pro MPD, PANalytical, Almelo, Holland) with Cu Kα radiation at 40 kV and 30 mA and scanning rate of 0.6 °/min. Fourier transform infrared spectroscopy (FTIR) was carried out with a Nicolet FTIR 5700 spectrometer (Thermo Scientific, Florida, USA) in the range 4000-400 cm−1 to determine the presence of silk in the vaterite microspheres. N2 gas sorption isotherms were obtained using an ASAP 2020 instrument (Micromeritics, GA, USA). Specific surface areas and pore size distributions were derived from the isotherms using BET calculations.
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5

Comprehensive Physicochemical Characterization of SiNPs

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The size, surface area, functional groups, metal content, polydispersity/aggregation and zeta potential of the SiNP nanoforms in the dry state were analysed as previously described. 23 (link) Briefly, transmission electron microscopy (TEM) images for size distribution of the SiNPs were performed by a JEOL 2010 TEM (with LaB6 electron gun). Brunauer-Emmett-Teller (BET) surface area analysis was done by nitrogen absorption using the ASAP 2020 instrument (Micromeritics, Norcross, GA, USA). Fourier transform infrared (FT-IR) spectroscopic analyses and thermogravimetric analysis (TGA) were performed for functional group analysis using a Thermo Nicolet Magna 750 IR spectrometer and a Mettler Toledo Star TGA/DSC system, respectively. Quantitative nuclear magnetic resonance (NMR) spectroscopy was done in solution state using a Bruker Avance 400 MHz spectrometer to determine the surface functional groups. The metal contents of pristine SiNP samples were analyzed using inductively coupled plasma-mass spectrometry/ atomic emission spectroscopy (ICP-MS/AES, Varian Vista-PRO, Mulgrave, Australia). Dynamic light scattering (DLS) and zeta potential measurements were done using the Zetasizer Nano ZS (Malvern Instruments, UK).
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6

Comprehensive Characterization of Material Samples

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Diffuse reflectance spectroscopy (DRS) was conducted using a Hitachi U-3010 36 dual-beam UV-Vis spectrometer equipped with an integrating sphere for sample composition analysis. A German NETZSCH thermogravimetric analyzer was employed to analyze the organic matter, such as pyrazole and carbon deposits, in the sample. The IR experiment was carried out on a Vertex 33-IR infrared spectrometer produced by Bruker, Germany. The Py-IR experiment was performed on a Bruker Tensor-27 FT-IR spectrometer with a resolution of 4 cm−1. A nitrogen adsorption–desorption isotherm was obtained at-196 °C using a Micromeritics ASAP2020 instrument. The Brunauer–Emmett–Teller (BET) model was used to estimate the surface area of the sample. The pore volume of the sample was calculated by the Barrett–Joyner–Halenda (BJH) method. The powder XRD pattern was recorded on a D8 ADVANCE X-ray diffractometer with Cu-Kα radiation (λ = 0.15418 nm) at 40 kV and 40 mA.
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7

Calcium Hydroxyapatite-Alginate Microspheres

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CHA powders with or without MINO were gently dispersed in a 10 mg/mL aqueous solution of sodium alginate (Fluka Biochemika, Buchs, Switzerland) to achieve a 1:15 alginate-CHA ratio. The alginate/CHA mixture was extruded drop-wise into a 0.35 M CaCl2 solution at room temperature using a needle with a diameter of 0.70 mm (BD Precision Glide, Sao Paulo, SP, Brazil). Spherical particles instantaneously formed and were allowed to mature in the CaCl2 solution for 15 mins, for gelation to occur. The CHA-alginate microspheres were dried using the freeze-lyophilization method for 24 hrs and sterilized by gamma rays (15 kGy). Additionally, the microspheres were characterized by X-ray diffraction (X’Pert Pro X-Ray diffractometer) and Fourier transform infrared spectroscopy (IR Prestige Series 21), respectively. The specific surface area of the microspheres was determined by the BET method using the ASAP 2020 instrument (Micromeritics Instrument Corp., Norcross, USA). The morphology of the implants was investigated using scanning electron microscopy (SEM; JEOL JSM 5310).
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8

Comprehensive Materials Characterization Protocol

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FESEM images were obtained
by a Hitachi S-4160 at an accelerating voltage of 20 kV. SEM analysis
was performed with a TESKAN-Vega 3. XRD patterns were obtained by
using a D8 ADVANCE type (BRUKER-Germany) with Cu-Kα radiation
(λ = 0.1542 nm). The XRD patterns were taken with an angular
step of 0.02°, with a sampling time of 1 s per step in the range
of 2Θ [5–50°]. The absorbance measurements were
performed using a Shimadzu 1601 PC UV–vis spectrophotometer.
FTIR spectra were obtained by tensor II (BRUKER-Germany). TGA was
performed by a TGA/DSC 1–Thermogravimetric Analyzer that was
made by Mettler-Toledo International Inc. under a nitrogen atmosphere
from room temperature to 800 °C with a heating rate of 5 °C
min–1. BET analysis was performed using a Micromeritics
(USA), ASAP 2020 instrument. Absorbance of the solution for MTT assay
was recorded by plate reader Polar Star Omega, BMG LABTECH, Germany
instrument.
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9

Analytical Characterization of Materials

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Nuclear magnetic
resonance (NMR) spectra
were recorded on a Varian 500 spectrometer. Powder X-ray diffraction
(PXRD) data of solid samples were recorded on a Bruker AXS D8 Advance
A25 powder X-ray diffractometer (40 kV, 40 mA) with Cu Kα (λ
= 1.5406 Å) radiation. Fourier transform infrared spectroscopy
(FTIR) was performed with a PerkinElmer Spectrum Two FT-IR spectrometer.
Vibrational circular dichroism (VCD) spectra were obtained using a
Bruker Optics PMA 50 FTIR spectrometer. Transmission electron microscopy
images and energy dispersive spectrometry (EDS) were attained using
an FEI Tecnai F30 microscope. X-ray photoelectron spectra (XPS) were
conducted on a PHI 5000 Versaprobe Scanning XPS Microprobe instrument
with UPS. High-performance liquid chromatography (HPLC) was recorded
with an Agilent 1220 Infinity II LC System. Thermogravimetric analysis
(TGA) was measured by a TA Instruments Q50 Thermogravimetric Analyzer.
N2 sorption isotherm measurements were performed at 77
K on a Micromeritics ASAP 2020 instrument. The elemental data were
collected on a Thermo Flash Smart elemental analyzer.
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10

Structural Characterization of Mesoporous Silica Nanoparticles

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TEM images were taken using a FEI Tecnai T12 Spirit microscope operated at an acceleration voltage of 120 kV. FFT analysis was performed using ImageJ software. Each TEM sample was prepared after CTAB removal by evaporating 10 µL of suspension on TEM grid in dry air. Cryo-TEM images were collected under low-dose conditions using a customized FEI Titan Themis 300 operating at 300 kV equipped with a cryo-box and FEI Ceta 16 M camera. More details can be found in the Supplementary Methods.
SAXS patterns were obtained at the G1 station at the Cornell High Energy Synchrotron Source (CHESS) using a 10 keV beam and a sample-to-detector distance of 40 cm. All samples were powders prepared by vacuum drying MSN suspensions after CTAB removal and were imaged soon after drying.
Nitrogen sorption measurements were performed using a Micromeritics ASAP2020 instrument. For each measurement, approximately 10 mg of freshly vacuum-dried powder sample was degassed at room temperature under vacuum overnight prior to the analysis.
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