The morphology of the materials was characterised on a SEM Quanta 650. PXRD analysis was performed on Rigaku Model D/MAX2500 diffractometer using Cu-Kα radiation at a scan speed of 2o/min. Infrared spectra were collected on an iD5 ATR (Attenuated Total Reflection) instrument, and TGA was measured under N2 at a flow rate of 10 mL·min−1. EPR spectra at X-band and Q-band were recorded using Bruker Micro spectrometers, and the intensity of the EPR signal of different samples was normalised to the sample quantity. The BET surface areas were obtained from N2 adsorption/desorption isotherms recorded on a Micromeritics 3-Flex instrument at 77 K. CO2 adsorption isotherms were obtained using Micromeritics 3-Flex at 273 K, 283 K and 298 K, and the value for Qst for CO2 adsorption was estimated by fitting these isotherms to the Van t’ Hoff equation. X-ray photoelectron spectroscopy (XPS) was performed on a Kratos Axis Ultra DLD spectrometer with a monochromated Al-Kα X-ray source (E = 1486.6 eV, 10 mA emission). Fluorescence micrographs were recorded on an Olympus Fluoview FV-1000 instrument to measure the fluorescence generated by the oligomerisation of 1 mL furfuryl alcohol catalysed by 10 mg of MOF at 60 °C over 2 h.
3flex
Manufactured by Micromeritics
Sourced in United States
The 3Flex is a surface area and porosity analyzer that can accurately determine the surface area, pore size, and pore volume of a wide range of materials. It uses gas adsorption techniques to provide comprehensive characterization of porous solids.
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Lab products found in correlation
Escalab 250xi, by Thermo Fisher Scientific (6 mentions)
Nicolet is50, by Thermo Fisher Scientific (6 mentions)
D8 advance, by Bruker (4 mentions)
Smartlab, by Rigaku (4 mentions)
Asap 2020, by Micromeritics (4 mentions)
K alpha, by Thermo Fisher Scientific (4 mentions)
Sigma 300, by Zeiss (4 mentions)
Sigma probe, by Thermo Fisher Scientific (4 mentions)
Jsm 7610f, by JEOL (3 mentions)
Nexsa, by Thermo Fisher Scientific (3 mentions)
S 4800, by Hitachi (3 mentions)
X pert pro, by Malvern Panalytical (3 mentions)
Multilab 2000, by Thermo Fisher Scientific (3 mentions)
Libra 120, by Zeiss (2 mentions)
Jsm 6701f, by JEOL (2 mentions)
Jem 2100f, by JEOL (2 mentions)
Quanta 250 feg, by Thermo Fisher Scientific (2 mentions)
V 670 uv vis spectrophotometer, by Jasco (2 mentions)
Miniflex 600, by Rigaku (2 mentions)
S8 tiger, by Bruker (2 mentions)
102 protocols using 3flex
1
Comprehensive Material Characterization
2
Characterization of Zeolite Catalyst
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The structure of the prepared catalyst was determined via XRD (Ultima IV, Rigaku Co. Ltd.) using a Cu Kα radiation source. The specific surface area, pore volume, and pore size distribution were determined by N2 adsorption–desorption at −196 °C (3-flex: Micromeritics Instrument Co. Ltd.). Scanning electron microscopy (SEM) was performed on an electron microscope (JSM-IT700HR/LA, JEOL Co. Ltd.) operated at 15.0 kV to identify the morphology of the as-prepared zeolite catalyst.
3
Comprehensive Analysis of Material Composition
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Morphology and composition of samples were evaluated by eld emission scanning electron microscopy (FESEM), performed on a JEOL JSM6701F and transmission electron microscopy (TEM) (LIBRA 120, Carl Zeiss NTS GmbH) equipped with an energy dispersive X-ray spectrometer (EDX). The crystalline and phase compositions were analyzed by X-ray diffraction (XRD, Shimadzu XRD-6000) with Cu Kα radiation λ = 0.154 nm. Fourier transform infrared (FT-IR) spectra (400-4000 cm - 1 ) of samples were recorded on a Nicolet IS10 at room temperature. UV-vis diffuse re ectance spectra (DRS) were performed through Perkin Elmer, Lambda 950. Time-resolved photoluminescence (TRPL) was performed on an Edinburgh FLS-920 with excitation wavelength at 376.4 nm and emission wavelength at 450 nm to obtain the recombination time. Speci c surface area of the samples was evaluated using Brunauer, Emmett and Teller (BET) theory on a Micromeritics 3Flex using nitrogen adsorption at 77 K. Sample was degassed at 120°C for 180 min with a ramping rate of 10°C/min before undergoing adsorption analysis. X-ray photoelectron spectroscopy (XPS) was performed using Shimadzu, AXIS ULTRA DLD. The sample surface was excited using aluminium monochromatic X-ray source (Al Kα).
4
Characterization and Emulsifying Properties of Modified Mesoporous Silica Nanocarriers
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Scanning electron microscopy (SEM) was performed using a Hitachi S-3400 II (Japan) at an accelerating voltage of 3 kV. A surface area and pore size analyzer (Micromeritics 3Flex, USA) was employed to measure the surface areas and pore sizes of the different samples. The chemical functional groups were analyzed using a Nicolet IS5 FTIR spectrophotometer (USA). Thermogravimetric analysis (TGA) was performed using a TA Q500 (USA) in a nitrogen environment at a heating rate of 10 °C min−1 over the temperature range of 25–800 °C. The emulsifying properties of NaDC, MSNC and PLD@MSNC samples were measured using the volume of the aqueous phase, emulsion phase, and organic phase. All samples contained aqueous solutions comprising different concentrations of samples and equal volumes of lauric acid methyl ester; solutions were oscillated for 60 min to mix evenly, and then kept still for 60 min. The volume fractions of the aqueous phase, emulsion phase, and organic phase were determined for each sample.
5
Characterization of Hydrogels and Aerogels
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The volumetric change of the hydrogels and organogels was determined from their diameter and height measured by caliper. The apparent density of the aerogel samples was calculated from its diameter, height and weight. Nitrogen sorption isotherms were acquired at 77 K with a gas-adsorption instrument (Micromeritics, 3flex) after 20 h of degassing at 50 °C and 0.06 mbar. The specific surface area was calculated from the isotherms from the low pressure range (P/P0 between 0.07 and 0.30) using Brunauer-Emmett-Teller (BET) method. The pore properties were evaluated from the adsorption part of the isotherm using Barrett-Joyner-Halenda (BJH) analysis. The microstructure of the samples was observed with a fieldemission scanning electron microscope (SEM, FEI, Nova NanoSEM 230) after application of a thin coating of conductive Pt.
6
Comprehensive Material Characterization
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Sample morphology was observed by field emission scanning electron microscopy (FE-SEM, Gemini SEM 300, Germany). The microstructural morphology of the samples was studied by transmission electron microscopy (TEM, JEM2010, Japan). Raman spectroscopy was performed with an inVia Raman spectrometer (Renishaw) with 532 nm laser excitation. N2 adsorption–desorption isotherms were measured at 77 K (Micromeritics 3Flex, USA). The samples were analyzed using an X-ray diffractometer (XRD, D8 ADVANCE, Germany) and Cu Kα radiation. The surface chemical composition was determined by X-ray photoelectron spectroscopy (XPS, ESCALAB Xi, USA).
7
Characterization of Submicrometer Calcite Grains
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Individual calcite grains were determined to be submicrometer size based on scanning electron microscopy (SEM) and energy dispersive spectrometry (EDS) analysis. The SEM and EDS analyses were performed on a Quanta 650 with an 150 mm Oxford Instruments X-Max detector at 10–15 kV, spot 2.5–4. Triplicate BET analyses were performed on the calcite powders using Micromeritics 3Flex surface characterization and nitrogen gas. The calcite powder has a N2 Brunauer-Emmett-Teller (BET) surface area of 8.72 ± 0.04 m2 g−1.
8
Nitrogen Adsorption Analysis of GF Powders
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The surface area and pore size analysis of GF powders was performed by means of N 2 adsorption/desorption measurements at 77 K on a volumetric gas adsorption analyzer (3Flex, Micromeritics, USA) up to 0.965 P/P 0 . Prior to the analysis, the samples were degassed under high vacuum (10 -4 Pa) at 130 °C for 12 hours while high purity (99.999%) N 2 and He gases were used for the measurements. The Brunauer-Emmett-Teller area (BET) was determined with respect to Rouquerol criteria for BET determination 68 assuming a molecular cross-sectional area of 16.2 Å 2 for N 2 (77 K). Pore size distribution was analyzed by the N 2 -DFT slit pore kernel.
9
Pore Analysis of Materials via Nitrogen Sorption
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Nitrogen sorption isotherms were
recorded at 77.4 K (3Flex, Micromeritics). Before each measurement,
samples were degassed at 105 °C for 20 h at a pressure of 1.3
× 10–2 mbar. Accessible pore volumes and surface
areas were measured using both classical analytical models (respectively
Barrett–Joyner–Halenda50 (link) between
2 and 50 nm and Brunauer–Emmett–Teller51 (link) with the modified Rouquerol equation) and state-of-the-art
nonlocal density functional theory (NLDFT) kernels, as recommended
by the ISO-15901-3 standard.52 For NLDFT
calculations, a cylindrical geometry was assumed for mesopores, based
on Tarazona’s work.53 (link),54 (link)
recorded at 77.4 K (3Flex, Micromeritics). Before each measurement,
samples were degassed at 105 °C for 20 h at a pressure of 1.3
× 10–2 mbar. Accessible pore volumes and surface
areas were measured using both classical analytical models (respectively
Barrett–Joyner–Halenda50 (link) between
2 and 50 nm and Brunauer–Emmett–Teller51 (link) with the modified Rouquerol equation) and state-of-the-art
nonlocal density functional theory (NLDFT) kernels, as recommended
by the ISO-15901-3 standard.52 For NLDFT
calculations, a cylindrical geometry was assumed for mesopores, based
on Tarazona’s work.53 (link),54 (link)
10
Brunauer-Emmett-Teller (BET) Film Analysis
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Example 7
Characterization: Brunauer-Emmett-Teller (BET) Analysis
Brunauer-Emmett-Teller (BET) analysis was conducted to examine the surface area, total pore volume, and average pore size of film samples using a Micromeritics 3Flex equipment. Before analysis, each film sample was degassed for 20 min at 60° C. with nitrogen purging under vacuum condition of 50 kilopascal (kPa).
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