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770 protocols using asap 2020

1

N2 Sorption Analysis of Porous Materials

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N2 sorption analysis was carried out at −196 °C using an ASAP 2020 from Micromeritics on unloaded and loaded samples. The samples were degassed at a vacuum lower than 10 μm Hg at 130 °C for 6 h. The specific surface area (SSA) was calculated using the multipoint BET method [25 (link)], while the pore size distribution was calculated based on the density functional theory (DFT) method using the model for N2 at −196 °C for slit-shaped pores. The total pore volume was obtained from single-point adsorption at a relative pressure P/P0 ≈ 1. These calculations were all performed using ASAP 2020 (Micromeritics) software.
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2

Characterization of Porous Carbons

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Nitrogen adsorption and desorption isotherms were measured at 77 K on a Micromeritics ASAP 2020 volumetric adsorption system. The total surface area and micropore volume were determined using the BET equation and the method of Dubinin-Radushkevich, respectively. The total volume Vpor total N2 was calculated by the single point method at a relative pressure of 0.97 from the nitrogen adsorption isotherms. The pore size distribution was obtained from the adsorption branch of the nitrogen isotherm using the density functional theory (DFT, slit pores).
Carbon dioxide adsorption isotherms were measured at 273 K on a Micromeritics ASAP 2020 volumetric adsorption system in the pressure range up to 0.1 MPa, (corresponding to a relative pressure of p/p0 = 0.03).
The total volume Vpor total H2O was obtained by a complete infiltration of the carbons with water in a vacuum (about 15 min) and subsequent weighing.
The macropore system of the carbons was investigated via mercury intrusion in the device Poremaster from Quantachrome. These measurements were done at the Institute for Technical Chemistry of the Leipzig University by the working group of D. Enke.
SEM photographs were taken on a FEI Nova Nanolab 200 (Portland, OR, USA) (accelerating voltage 10 kV) using a secondary electron detector. These measurements were done by the working group of Dirk Enke at Leipzig University.
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Comprehensive Characterization of Porous Carbon

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Micromeritics ASAP2020 (US) adsorption analyzers was employed to measure the N2 adsorption–desorption isotherms at 77 K. Before performing the adsorption–desorption analyses, samples were degassed under dynamic vacuum conditions to constant weight at a temperature of 393 K for 2 h. Raman spectroscopy was conducted on a Takram micro-Raman spectrometer (Teksan™, Iran). FTIR spectroscopy was accomplished on a PerkinElmer Spectrometer in the range of 500–4000 cm−1 with KBr pallets. X-ray photoelectron spectroscopy (XPS) measurements were carried out on an Al Kα source (XPS Spectrometer Kratos AXIS Supra). Transmission electron microscope (TEM) using Philips EM208S 100 kV. Thermogravimetric analyses (TG) in argon and air atmosphere were conducted on a Q600 (US) TA. Field emission scanning electron microscopy (FESEM) was observed on a Nanosem-450 microscope. Low-pressure CO2 adsorption isotherms of the synthesized porous carbon were measured at 273 K on an ASAP 2020 (US) Micromeritics at 0–1 bar.
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4

Physisorption Characterization of Porous Materials

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The system is connected to a vacuum station that can generate a vacuum up to 10−7 Pa. N2 and H2 physisorptions at 77 K were performed on a Micromeritics ASAP 2020 with liquid nitrogen as a coolant. CO2 physisorption at 273 K and 195 K were performed on a Micromeritics ASAP 2020 with ice water and dry ice/isopropanol as coolants, respectively. Olefins and paraffin physisorption at different temperatures (273, 286, and 298 K) were determined using a Micromeritics 3Flex and ice water or a recycle water bath was used to control the temperature. Before the measurements, about 100 mg of the samples were degassed under a vacuum at 150 °C for at least 6 h.
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5

Comprehensive Characterization of Synthesized Products

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The morphology of synthesized products was observed by field emission scanning electron microscopy (SEM, S-4800, Hitachi, Tokyo, Japan) and high-resolution transmission electron microscopy transmission electron microscope (HRTEM) with an accelerating voltage of 200 kV (JEM-2100, JEOL, Tokyo, Japan). The component element and content of the products were measured by energy disperse X-ray spectroscopy (EDS) on EDAXTLS attachment with an operating voltage of 30 kV (S-4800, Hitachi, Tokyo, Japan). X-ray photoelectron spectroscopy (XPS) spectra were recorded (ESCALAB 250 Xi, Thermo Fisher Scientific, Waltham, MA, USA). The XRD patterns were collected using a Bruker D8 diffraction instrument with Cu Kα radiation (40 kV, 40 mA) (D8, Bruker, Bremen Germany). Surface area quantification was achieved using the Brunauer–Emmett–Teller (BET) method on a Micromeritics ASAP 2020 instrument using nitrogen gas, and pore size distribution was obtained according to the Barrett–Joyner–Halenda (BJH) algorithm (ASAP 2020, Micromeritics, Norcross, GA, USA).
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6

Characterization of Cu@APS-TDU-PMO Nanosphere

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All chemicals were purchased from Merck or Aldrich and used as received, except for benzaldehyde which was distilled before its using. Characterization of the new Cu@APS-TDU-PMO (1) was performed by FESEM (TESCAN-MIRA3), TEM (Philips EM 208S), FTIR (Shimadzu 8400S), BET (ASAP™ 2020 Micromeritics), and TGA Bahr Company STA 504). XRD patterns of the mesoporous silica nanosphere were obtained using TW 1800 diffractometer with CuKα radiation (λ = 1.54050 Å). 1H NMR and spectra (500 MHz, Bruker DRX-500 Avance spectrometer) were recorded in DMSO-d6 at ambient temperature. Spectral data were compared with those obtained from authentic samples or reported in the literature. Distilled water was used in all experiments.
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7

Felt BET Surface Area Measurement

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For the BET surface area test, a total of 10 g felt was cut into pieces to form the sample. ASAP2020 micromeritics® (Micromeritics Instrument Corp., Norcross, GA, USA) was used as the measuring tool. The process of isothermal absorption line condition started from the degas process, followed by a measuring process set from relative pressure 0.1 to 1 under 77 K. The desorption process operated under reverse, at room temperature. The results were transferred to surface area data using the Brunauer-Emmett-Teller (BET) calculation model.
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8

BET Surface Area Analysis of Metal Debris

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The specific surface area analysis was carried out using ASAP 2020 equipment (Micromeritics, Norcross, GA, USA). Nitrogen was used as an adsorbate. The metal debris obtained was degassed at 100 °C under vacuum conditions (10 µm Hg). The specific surface area was analyzed by applying mathematical calculations described by the BET (Brunauer–Emmett–Teller) theory [22 (link)]. An analysis of the specific surface area was carried out in triplicate.
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9

Morphological and Surface Analysis of Chitosan-based Adsorbents

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The morphology of the materials
was examined using a scanning electron microscope (Phenon Pro X),
operated at an electron-accelerating voltage of 10 kV. Prior to scanning,
the samples were kept onto a carbon adhesive tape on an aluminum stub
under high vacuum conditions. The surface area and porosity of the
chitosan-adsorbent samples were analyzed by nitrogen sorption isotherms,
obtained at −196 °C, on the Micromeritics ASAP 2020 equipment.
The surface area was determined using the BET method applied to the
adsorption data with the relative pressure (P/Po) ranging from 0.06 to 0.3. The materials were
outgassed at 120 °C for 24 h prior to the analyses.
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10

Comprehensive Material Characterization

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The crystallographic properties of the samples were obtained from X-ray diffraction (XRD) measurements using an X-ray diffractometer (Bruker D8 Discover) equipped with Ni-filtered Cu Kα radiation (λ = 0.15406 nm). The scan rate was 0.02° s−1, the accelerating voltage was 50 kV, and the current was 40 mA. The optical absorption spectra of the samples were acquired via an ultraviolet-visible (U.V.-Vis) spectrometer (Agilent Cary 100), and BaSO4 was used as a reflectance standard. The optical band gap of the samples was further acquired from a Tauc plot, [hv.F(R)]1/n vs. hv, where n = ½ for the indirect band gap. The surface microstructure was acquired from a field emission scanning electron microscope (FESEM) (Hitachi SU8010). The surface area of the samples was measured using the Micromeritics ASAP 2020.
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