The hydrodynamic size measurements of the prepared NPs were characterized by dynamic light scattering (DLS), and zeta potential was determined by a Zetasizer Nano instrument (Malvern NanoZS 90, Malvern, UK). An electron microscope (Hitachi H-800, Tokyo, Japan) was used to characterize the transmission electron microscope (TEM) images at an accelerating voltage of 200 kV. Fourier transform infrared spectra (FTIR) was performed on an FTIR spectrophotometer (Bruker Vertex 70, Karlsruhe, Germany) using KBr pellets. The UV-Visible absorption spectra were measured by a Jasco V-650 spectrophotometer (Jasco V-650, Tokyo, Japan). Nitrogen adsorption-desorption isotherms were recorded on a Micromeritics Tristar 3000 analyzer (Micromeritics Tristar 3000, Norcross, GA, USA) at 77 K. The pore-size distributions and the pore volume was calculated by the Barret-Joyner-Halenda (BJH) method, and the specific surface area was calculated by the Brunauer-Emmett-Teller (BET) method. The adsorption isotherm branches were used in calculating the pore-size distributions.
Tristar 3000
Manufactured by Micromeritics
Sourced in United States
The TriStar 3000 is a surface area and porosity analyzer that uses gas adsorption techniques to measure the surface area, pore volume, and pore size distribution of solid materials. The instrument is capable of analyzing a wide range of materials, including powders, granules, pellets, and monoliths. The TriStar 3000 provides accurate and reliable data to support research, development, and quality control applications.
Automatically generated - may contain errors
Lab products found in correlation
Jem 2100f, by JEOL (5 mentions)
Mastersizer 2000, by Malvern Panalytical (4 mentions)
S 4800, by Hitachi (4 mentions)
Jem 2010, by JEOL (4 mentions)
D2 phaser, by Bruker (4 mentions)
Escalab 250xi, by Thermo Fisher Scientific (4 mentions)
Ultra 55, by Zeiss (3 mentions)
Rtp 300 rc, by Rigaku (3 mentions)
Jem arm200f, by JEOL (3 mentions)
Nicolet 6700, by Thermo Fisher Scientific (3 mentions)
Escalab 250, by Thermo Fisher Scientific (3 mentions)
Autochem 2, by Micromeritics (2 mentions)
Dtg 60h, by Shimadzu (2 mentions)
Vacprep 061, by Micromeritics (2 mentions)
Jsm 6700f, by JEOL (2 mentions)
X pert pro, by Philips (2 mentions)
Smartprep degasser, by Micromeritics (2 mentions)
Smart prep degassing unit, by Micromeritics (2 mentions)
D8 focus diffractometer, by Bruker (2 mentions)
Fls 980 apparatus, by Edinburgh Instruments (2 mentions)
120 protocols using tristar 3000
1
Comprehensive Characterization of Nanoparticles
2
Characterization of Industrial Quartz
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The industrial quartz Q1, used in a sanitary ware composition, was selected as model quartz for the coating trials. Crystalline silica content (100% w/w) was determined by X-ray diffraction (Philips 1820/00 diffractometer, The Netherlands), particle size distribution (d10 = 1.9, d50 = 12.1, and d90 = 37.2 µm) by laser diffraction (Malvern Mastersizer 2000, UK), and surface area (0.87 m2 g−1) by the Brunauer–Emmett–Teller method (TriStar 3000, Micromeritics, USA).
3
Porous Texture Characterization by Adsorption
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Textural characterization of the samples was carried out by means of physical adsorption of N2 at −196 °C in a Micromeritics ASAP 2010 and adsorption of CO2 at 0 °C in a Micromeritics TriStar 3000. Helium density was measured in an Accupyc 1330 at 35 °C. The samples were outgassed at 100 °C under vacuum overnight prior to adsorption measurements.
The use of both adsorbates, N2 and CO2, provides complementary information about the porous texture of the samples: the adsorption of CO2 at 0 °C and up to 1 bar is restricted to pores narrower than 1 nm, whereas N2 adsorption at −196 °C covers wider pore sizes but presents diffusion limitations in the narrower pores. The total pore volume (Vp) was calculated from the amount of N2 adsorbed at a relative pressure of 0.99, and the BET surface area from the Brunauer-Emmett-Teller equation [29 (link)]. The micropore volume (W0) and the micropore surface area (SDR) were determined from the Dubinin-Radushkevich (DR) [30 (link)] and Dubinin-Astakhov (DA) [31 (link)] equations assuming a density of the adsorbed phase of 0.808 cm3·g−1 for N2 and 1.023 cm3·g−1 for CO2, a cross sectional area of 0.162 nm2 for N2 and 0.187 nm2 for CO2 and finally an affinity coefficient of 0.34 for N2 and 0.36 for CO2. The average micropore width (L0) was calculated through the Stoeckli-Ballerini equation [32 (link)].
The use of both adsorbates, N2 and CO2, provides complementary information about the porous texture of the samples: the adsorption of CO2 at 0 °C and up to 1 bar is restricted to pores narrower than 1 nm, whereas N2 adsorption at −196 °C covers wider pore sizes but presents diffusion limitations in the narrower pores. The total pore volume (Vp) was calculated from the amount of N2 adsorbed at a relative pressure of 0.99, and the BET surface area from the Brunauer-Emmett-Teller equation [29 (link)]. The micropore volume (W0) and the micropore surface area (SDR) were determined from the Dubinin-Radushkevich (DR) [30 (link)] and Dubinin-Astakhov (DA) [31 (link)] equations assuming a density of the adsorbed phase of 0.808 cm3·g−1 for N2 and 1.023 cm3·g−1 for CO2, a cross sectional area of 0.162 nm2 for N2 and 0.187 nm2 for CO2 and finally an affinity coefficient of 0.34 for N2 and 0.36 for CO2. The average micropore width (L0) was calculated through the Stoeckli-Ballerini equation [32 (link)].
4
Adsorption Isotherms of CO2, N2, H2O
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Adsorption isotherms of CO2, N2, and H2O were collected. Water vapor adsorption isotherms were determined from 30 to 70 °C in a volumetric apparatus Quantachrome Hydrosorb 1000 HT where temperature was controlled by a Julabo thermostatic bath. Single component N2 and CO2 equilibrium adsorption isotherms were collected at 30 °C in a volumetric device, TriStar 3000 from Micromeritics where temperature was controlled by a Thermo Haake thermostatic bath. Before each measurement, samples were outgassed at 100 °C under vacuum overnight.
5
Characterization of Bicomponent Textile Filaments
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Several characterization techniques were used:
- Scanning electron microscopy (SEM, Hitachi S-2360, Japan) was used to determine the morphology of the bicomponent (PET/PTT) filaments.
- Differential scanning calorimetry (DSC, Mettler Instrument with STARe SW 9.20 thermal analysis software) was carried out. The sample (10 mg) was heated from 0 °C to 300 °C with a heating rate of 10 °C min−1. Each test was carried out at least three times.
- The characterization of the bicomponent (PET/PTT) filaments and conventional PET filaments were carried out by N2 physical adsorption at −196 °C (Micromeritics, TriStar 3000, Norcross, GA, USA). Before measurement, the samples underwent degassing for 2 h at 100 °C to remove any contaminants which may have been adsorbed onto the surface or pores of the samples. The Brunauer–Emmett–Teller (BET) equation was used to estimate the apparent surface area, using the N2 adsorption isotherms at −196 °C. This equation was valid in the range of the relative pressure P/P0 between 0.18 to 0.28 m2 g−1 and 0.16 to 0.23 m2 g−1 for the bicomponent (PET/PTT) filaments and conventional (PET) filaments, respectively.
All the analysis conditions were reported in more detail in our previous studies.3,19,20 (link)
- Scanning electron microscopy (SEM, Hitachi S-2360, Japan) was used to determine the morphology of the bicomponent (PET/PTT) filaments.
- Differential scanning calorimetry (DSC, Mettler Instrument with STARe SW 9.20 thermal analysis software) was carried out. The sample (10 mg) was heated from 0 °C to 300 °C with a heating rate of 10 °C min−1. Each test was carried out at least three times.
- The characterization of the bicomponent (PET/PTT) filaments and conventional PET filaments were carried out by N2 physical adsorption at −196 °C (Micromeritics, TriStar 3000, Norcross, GA, USA). Before measurement, the samples underwent degassing for 2 h at 100 °C to remove any contaminants which may have been adsorbed onto the surface or pores of the samples. The Brunauer–Emmett–Teller (BET) equation was used to estimate the apparent surface area, using the N2 adsorption isotherms at −196 °C. This equation was valid in the range of the relative pressure P/P0 between 0.18 to 0.28 m2 g−1 and 0.16 to 0.23 m2 g−1 for the bicomponent (PET/PTT) filaments and conventional (PET) filaments, respectively.
All the analysis conditions were reported in more detail in our previous studies.3,19,20 (link)
6
Measuring Porous Silicon Characteristics
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The gravimetric porosity was calculated using the weight of the porous silicon, along with the density of bulk silicon and the total weight loss due to anodisation. Nitrogen gas adsorption/desorption [36] was carried out using a Micromeritics Tristar 3000. The samples were degassed under flowing nitrogen at 90 °C for 1 h before analysis. Computational analysis of the isotherms yielded absolute values for surface area (based on the Brunauer-Emmett-Teller (BET) method), pore volume (based on the Barrett-Joyner-Halenda (BJH) adsorption method, with P/P o chosen to represent the maximum available pore volume) and average pore diameter (from single-point adsorption). From the pore volume, the average porosity was calculated and compared with the gravimetric value.
Thermoporometry, was also used to confirm the pore volume and pore diameter of aerocrystals. The technique determines pore size based on the melting or crystallization point depression of a liquid confined within pores. 3-5 mg of sample was hermetically sealed into aluminium pans for the differential scanning calorimeter (DSC) analysis. The temperature shifts was measured using DSC for cyclohexane exothermic freezing and endothermic melting within the temperature range of -45°C to 10 °C, at a heating rate of 0.5 °C/min under N 2 gas purge of 60 mL/min.
Thermoporometry, was also used to confirm the pore volume and pore diameter of aerocrystals. The technique determines pore size based on the melting or crystallization point depression of a liquid confined within pores. 3-5 mg of sample was hermetically sealed into aluminium pans for the differential scanning calorimeter (DSC) analysis. The temperature shifts was measured using DSC for cyclohexane exothermic freezing and endothermic melting within the temperature range of -45°C to 10 °C, at a heating rate of 0.5 °C/min under N 2 gas purge of 60 mL/min.
7
Characterization of Superhydrophobic Graphene Flakes
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The morphology of sch–FLG was characterized by using high-resolution transmission electron microscopy (HRTEM, JEOL). The crystal structure of sch–FLG was characterized by using X-ray diffraction (XRD, Thermo Fisher XTRA) at a scanning rate of 10° min−1 in the 2θ range of 10–70° with Cu-Kα radiation (λ = 1.5406 Å) at room temperature. The surface elements of sch–FLG were characterized by using an X-ray photoelectron spectroscopy (XPS, Thermo Scientific ESCALAB 250Xi) system with Al Kα radiation (Energy 1486.6 eV) and a laser Raman spectrometer (HR Evolution, HORIBA FRANCE SAS) in a spectrum scanning range of 100–4000 cm−1 using a solid-state semiconductor laser with λ = 532 nm. The Brunauer–Emmett–Teller specific surface area and Barret–Joyner–Halenda pore volume of sch–FLG was measured by using a N2 adsorption–desorption method (Tristar 3000, Micromeritics). The chemical structure of sch–FLG was characterized by using Fourier transform infrared (FTIR, Thermo Nicolet 6700), and the samples were prepared with the powder pressing method in a potassium bromide pellet at room temperature.
8
Characterization of TiO2 Nanostructures
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The chemical feature was investigated by X-ray photoelectron spectroscopy (XPS, Thermo Fisher K-Alpha) with standard Al Kα (1486.7 eV) X-ray source. The binding energies were calibrated with respect to the signal from the adventitious carbon (binding energy = 284.6 eV). Raman spectra of TiO2 were collected by a confocal Raman microscope (LabRAM HR Evolution, Horiba) with excitation laser wavelength of 632.8 nm. An objective lens is employed to focus the excitation laser on the substrate and collect the Raman signal. The microstructure and morphology were examined by filed effect scanning electron microscopy (FESEM, Ultra55, ZEISS) and high-resolution transmission electron microscopy (HRTEM, Tecnai F20 S-Twin, FEI). Crystallinity and phase structures of powders were analyzed by a Rigaku-D/MAX 2000X-ray diffraction (XRD) system with Cu Kα radiation. The Brunauer-Emmett-Teller (BET) surface area was estimated by a surface area apparatus (TriStar-3000, Micromeritics). UV-visible absorption spectra were recorded by a UV-vis-NIR spectrophotometer (UV-3600, Shimadzu).
9
Particle Size and Surface Area Analysis
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Example 6
The specific surface area (SSA) and particle size distribution (PSD) were determined for two batches (A and B) of crystalline rounded particles of compound (I) prepared according to the present invention. The particles of the two batches were then milled followed by the determination of SSA and PSD. The results are shown in Tables 1 and 2. The results show that the specific surface area (SSA) of the particles did not significantly change even if the particles were milled to reduced particle size.
The specific surface area was measured using the three-point nitrogen adsorption technique based on the Brunauer, Emmett and Teller (BET) theory using TriStar 3000 automated gas adsorption analyzer (Micromeritics, Inc.). The samples were vacuum dried for 20 hours in 40° C. The volumetric method was applied at the relative pressure range 0.1-0.3 P/P0.
10
Characterization of Adsorbent Materials
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The specific surface area (SSA) and micro/meso-pore structure were obtained using a sorption meter (Tristar 3000, Micromeritics Instrument Corp., Norcross, GA, USA). The samples were subjected to degasification at 180 °C for 3 h in a nitrogen atmosphere. The SSA was calculated using the Brunauer–Emmett–Teller (BET) method.
The adsorbents’ surface morphology was examined by scanning electron microscopy (SEM) (55-VP, Supra, Zeiss, Jena, Germany), using an acceleration voltage of 20 kV. In addition, the Raman spectra of the adsorbents were obtained using a Bruker Bravo spectrometer (Bruker, Ettlingen, Germany).
The amorphous and crystalline nature of adsorbents were evaluated through X-ray diffraction, using an X-ray diffractometer (Bruker D8 Advance, Ettlingen, Germany), operating at 45 kV and 40 mA, using Cu-Kα monochromatic radiation (λ = 1.54 Å), 2θ angle interval of 10–70 and a scan rate of 0.4°/min.
The adsorbents’ surface morphology was examined by scanning electron microscopy (SEM) (55-VP, Supra, Zeiss, Jena, Germany), using an acceleration voltage of 20 kV. In addition, the Raman spectra of the adsorbents were obtained using a Bruker Bravo spectrometer (Bruker, Ettlingen, Germany).
The amorphous and crystalline nature of adsorbents were evaluated through X-ray diffraction, using an X-ray diffractometer (Bruker D8 Advance, Ettlingen, Germany), operating at 45 kV and 40 mA, using Cu-Kα monochromatic radiation (λ = 1.54 Å), 2θ angle interval of 10–70 and a scan rate of 0.4°/min.
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