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22 protocols using tristar 3000

1

Engineered Nanomaterial Characterization Protocol

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SiO2, Fe2O3, CeO2, and the composite Ag/SiO2 ENM, consisting of 10 percent silver supported on SiO2 particles, were produced by flame spray pyrolysis using the Harvard Versatile Engineered Nanomaterial Generation System (VENGES) as previously described [41 (link),42 (link),47 (link)]. TiO2 and ZnO ENM powders were purchased from EVONIK (Essen, Germany), and Alfa Aesar (Ward Hill, MA, USA), respectively. ENMs were tested for endotoxin with a Limulus Amebocyte Lysate (LAL) chromogenic quantitation kit from ThermoFisher (Waltham, MA, USA) using 10 μg ml−1 suspensions of ENMs in water and following manufacturers instructions. Specific surface area, SSA, was determined by the nitrogen adsorption/Brunauer-Emmett-Teller (BET) method using a Micrometrics Tristar 3000 (Micrometrics, Inc., Norcross, GA, USA). Equivalent primary particle diameter, dBET, was calculated, assuming spherical particles, as
dBET=6SSA×ρp, where ρp is the particle density, which was obtained for each particle from the densities of component materials, at 20°C, reported in the CRC handbook of Chemistry and Physics [48 ]. Particle crystal size and diameter was also determined by X-ray diffraction using a Scintag XDS2000 powder diffractometer (Scintag Inc., Cupertino, CA, USA), reported here as dXRD.
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2

Measuring Reinforcing BC Nanofiber Surface Area

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Nitrogen adsorption/desorption analysis was conducted using a surface
area analyzer (TriStar 3000, Micrometrics Ltd., Dunstable, UK) to
determine the specific surface area of different reinforcing BC nanofiber
networks architecture. Before the measurements, purified BC pellicles
were pressed to thicknesses of 3 and 1.5 mm, respectively, to mimic
the reinforcing architecture within composites I and II. The compressed BC pellicles were flash frozen in Petri-dishes
by immersion in liquid nitrogen, followed by freeze-drying (Christ
Alpha 1–2 LDplus, Newtown, UK). The reinforcing BC nanofiber
network architecture for composite III was produced as
previously described. All samples were purged with nitrogen at 120
°C overnight to remove any adsorbed water molecules before the
measurement. The specific surface was calculated by the Brunauer–Emmett–Teller
equation. A sample mass of approximately 70 mg was used in this measurement.
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3

Nitrogen Sorption Measurement and BET Analysis

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Samples were degassed for 24 h using the vacuum mode of the VacPrep 061 (Micrometrics, Norcross, USA) and then purged with nitrogen for one hour. Subsequently, samples were subjected to nitrogen sorption measurements at -196 • C (TriStar 3000, Micrometrics). The specific surface area (SSA) of the samples was calculated making use of the Brunauer Emmett and Teller (BET) theory (Brunauer et al., 1938) (link).
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4

Nanoparticle Surface Area Characterization

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Surface area was determined via the BET (Brunauer, Emmett and Teller) Theory using a TriStar 3000, Micrometrics Gemini 2375 V 5.01, Norcross, GA connected to a computer running Star Driver (version 2.03). The surface area for the NanoClusters was measured for all powders by nitrogen adsorption and compared to that of the micronized stock drug and nanoparticle suspension. Prior to surface area measurement, a known mass of the sample powder (120 ± 30 mg) was placed in a sample tube. Another reference tube filled with 3 mm spherical glass beads was used as a reference. Liquid nitrogen was used to maintain the sample and reference tube at low temperature to yield an accurate determination of surface area17 (link).
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5

Characterization of Zeolitic Imidazolate Framework-8

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XRD powder
patterns were acquired on a D-Max 2500 Rigaku X-ray diffractometer
with a copper anode and a graphite monochromator using Cu Kα
radiation (λ = 1.540 Å), taking data from 2θ = 2.5°
to 40° at a scan rate of 0.03°/s and operating parameters
of 40 kV and 80 mA. Phase identification was conducted by comparison
to simulated powder patterns.
The N2 adsorption–desorption
isotherms were obtained using a Micrometrics Tristar 3000 at 77 K.
Before these measurements, ZIF-8 samples were degassed for 8 h under
a vacuum at 200 °C using a heating rate of 10 °C/min. The
surface area was calculated using the Brunauer–Emmett–Teller
(BET) equation.
Thermal behavior was determined by thermogravimetric
analysis (TGA)
which was carried out using a Mettler Toledo TGA/STDA 851e. Samples
(10 mg) placed in 70 μL alumina pans were heated under airflow
of 40 mL/min between 35 and 900 °C with a heating rate of 10
°C/min.
Nanocrystal morphology and size were determined
by scanning electron
microscopy (SEM). The images were obtained using an Inspect F50 model
scanning electron microscope (FEI) operating at 20 kV. The average
particle size was determined using ImageJ 1.49b software, where at
least 50 particles were counted for each sample.
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6

Characterization of Coated and Uncoated ZnO Nanoparticles

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The morphology of these NPs was examined by electron microscopy. Uncoated and SiO2-coated ZnO NPs were dispersed in ethanol at a concentration of 1 mg/ml in 50 ml polyethylene conical tubes and sonicated at 246 J/ml (Branson Sonifier S-450A, Swedesboro, NJ, USA). The samples were deposited onto lacey carbon TEM grids. All grids were imaged with a JEOL 2100. The primary particle size was determined by X-ray diffraction (XRD). XRD patterns for uncoated ZnO and SiO2-coated ZnO NPs were obtained using a Scintag XDS2000 powder diffractometer (Cu Kα, λ = 0.154 nm, 40 kV, 40 mA, stepsize = 0.02°). One hundred mg of each sample was placed onto the diffractometer stage and analyzed from a range of 2θ = 20-70°. Major diffraction peaks were identified using the Inorganic Crystal Structure Database (ICSD) for wurtzite (ZnO) crystals. The crystal size was determined by applying the Debye-Scherrer Shape Equation to the Gaussian fit of the major diffraction peak. The specific surface area was obtained using the Brunauer-Emmet-Teller (BET) method. The samples were degassed in N2 for at least 1 hour at 150°C before obtaining five-point N2 adsorption at 77 K (Micrometrics Tristar 3000, Norcross, GA, USA).
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7

Physicochemical Characterization of Engineered Nanomaterials

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ENMs investigated are listed in Table 1. All materials were generated by the Administration and Research Coordination Core (ERCC) as part of the NHIR consortium efforts. Fast settling ENMs included composite material Ag15%/SiO2 (dBET: 6nm and 7nm for Ag and SiO2, respectively), CeO2 (dBET:5.3 nm), and Ag (dBET: 18 nm). Representative slow-settling material Fe2O3 (dBET: 10nm) was also investigated for comparison. All ENM powders were generated in-house by flame spray pyrolysis using the Harvard Versatile Engineered Nanomaterial Generation System (VENGES) as previously described [47 –49 ].
Specific surface area (SSA) was determined by the nitrogen adsorption/Brunauer-Emmett-Teller (BET) method using a Micrometrics Tristar 3000 (Micrometrics, Inc., Norcross, GA, USA). Equivalent primary particle diameter, dBET was calculated, assuming spherical particles, as
dBET=6SSA×ρp where ρp is the particle density, which was obtained for each ENM in powder form using a pycnometer (Quantachrome Instruments, ULTRAPYC 1200e) through N2 volume displacement and the volume-to-pressure relationship known as Boyle’s Law.
Details on the synthesis and characterization of ENMs used in this study are presented by the authors elsewhere [25 (link)].
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8

Characterization of Porous Materials

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FTIR spectra were collected in ATR mode on a Spectrum II spectrometer (Perkin-Elmer). The powder XRD patterns were collected with a PANalytical X’Pert Pro MPD diffractometer (Cu Kα1 = 0.1540598 nm). The SEM images were obtained with a Hitachi S-4800 electron microscope. EDX was done on an Oxford Instruments X-MaxN SDD instrument. Nitrogen adsorption and desorption isotherms were measured at 77 K with a Micrometrics TriStar 3000 apparatus; the specific surface area was determined by the BET method in the 0.05–0.25 P/P0 range. The mesopore volume and pore size distribution were obtained by the Barrett–Joyner–Halenda (BJH) method from the desorption branch.
Solid-state 31P magic angle spinning (MAS) NMR experiments were performed on a Varian VNMRS 400 MHz (9.4 T) spectrometer using a 3.2 mm Varian T3 HXY MAS probe. Single pulse experiments were carried out with a spinning rate of 20 kHz, a 90° excitation pulse of 3 μs, a recycle delay of 30 s and 100 kHz spinal-64 1H decoupling. 200 transients were recorded. The 31P chemical shift was determined using an external reference, hydroxyapatite Ca10(PO4)6(OH)2, at 2.8 ppm (with respect to H3PO4, 85 wt % in water).
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9

Nitrogen Adsorption for Surface Area

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Surface area (BET method) was determined using from nitrogen adsorption isotherms obtained with a Tri-Star 3000 (Micrometrics) in the same manner as previously published8 (link). One of the three sample measurement ports of the Tri-Star was equipped with an empty sample tube with which the saturation vapor pressure (P0) of N2 was measured concurrently with each measurement of the equilibrium vapor pressure (P) over the sample.
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10

Characterization of Zinc Oxide Nanoparticles

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SEM was used to examine the morphology of the ZnO-NPs (SEM, Vega Tescan TS5136MM). Using KBr pellets, the FTIR spectra were recorded with a Nicolet 6700 FTIR spectrometric analyzer. Furthermore, the BET technique was used to compute the specific surface area in the relative pressure range of 0.05–0.3. The Barrett–Joyner–Halenda (BJH) method was used to compute the mesopore size and distribution from the desorption curves, whereas the t-plot approach was used to calculate the micropore area values. The porosity (using the DFT approach) and surface area were measured using a N2 adsorption–desorption isotherm analysis (Tristar 3000 apparatus, Micrometrics Instrument Corp., Norcross, GA, USA) (BET method). A UV-vis spectrophotometer was used to obtain the spectrophotometric readings (UV 4000, MRI, Stuttgart, Germany).
An XRD (D/Max 2550PC, Rigaku, Japan) diffractometer was used for X-ray diffractometry. The reflection-scanning mode was used to record the radical scan while changing 2 θ from 0° to 100°. A pH meter was used to determine the pH of the solution (Metrohm Herisau Digital E 532, Herisau, Switzerland).
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