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11 protocols using nova 4200e

1

Adsorbent Preparation and Characterization

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Lignin (Lig) was purchased from Tokyo Chemical Industry Co., Ltd. (Tokyo, Japan). Calcined Lig at 200, 400, 600, 800, and 1000 °C was prepared by keeping it in a muffle furnace for 2 h (denoted as Lig200, Lig400, Lig600, Lig800, and Lig1000, respectively). Cadmium chloride was purchased from FUJIFILM Wako Pure Chemical Co. (Osaka, Japan).
The morphologies of each adsorbent were measured by scanning electron microscopy SU1510 (SEM, Hitachi High-Technologies Co., Tokyo, Japan). The specific surface area and pore volumes were analyzed using a specific surface analyzer NOVA4200e (Quantachrome Instruments Japan G.K., Kanagawa, Japan). The surface functional groups were analyzed by the Fourier-transform infrared (FT-IR) spectroscopy system 460Plus (JASCO Co., Tokyo, Japan). The binding energy and elemental distribution of the adsorbent surface were measured by the X-ray photoelectron spectroscopy system AXIS-NOVA (Shimadzu Co., Ltd., Kyoto, Japan) and electron microanalyzer JXA-8530F (JEOL, Tokyo, Japan), respectively.
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2

Nanopaper Characterization by FE-SEM and Porosimetry

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The surfaces and cross-sections of the nanopapers were observed using FE-SEM (SU-8020, Hitachi High-Tech Science Corp., Tokyo, Japan) at an accelerating voltage of 2 kV. Prior to FE-SEM observation, platinum sputter coating of the nanopapers was conducted using an E-1045 Ion Sputter (Hitachi High-Tech Science Corp., Tokyo, Japan) at a current of 20 mA for 10 s. Pore size distribution curves were obtained based on the Brunauer–Emmett–Teller and Barrett–Joyner–Halenda models using a pore size analyzer (NOVA 4200e, Quantachrome Instruments, Kanagawa, Japan). The porosity of each nanopaper was calculated using the following equation:30 (link)where ρb denotes the bulk density of the nanopapers, and ρt denotes the true density of the TEMPO-oxidized cellulose nanofibers with carboxylate content of 1.37 mmol gcellulose−1, which is 1.68 g m−3 according to a previous study.48 (link)
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3

Characterization of Chitin and Cellulose Nanopapers

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Surface structures of the original and carbonized chitin and cellulose nanopapers were observed using field-emission scanning electron microscopy (FE-SEM) (SU-8020, Hitachi High-Tech Science Corp., Tokyo, Japan) at an accelerating voltage of 2 kV. Prior to FE-SEM, platinum sputtering of the samples was conducted using an E-1045 Ion Sputter (Hitachi High-Tech Science Corp., Tokyo, Japan) at a current of 20 mA for 10 s. Pore size distribution curves were obtained using nitrogen adsorption analysis at −196 °C based on the Brunauer−Emmett−Teller and density functional theory models (NOVA 4200e, Quantachrome Instruments, Kanagawa, Japan).
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4

Comprehensive Structural Characterization of Materials

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Crystallographic phases of all the products were investigated by powder X-ray diffraction (XRD, Rigaku D/max2500) with Cu Kα (λ = 1.5406 Å) radiation. The morphologies of the samples were examined by field-emission scanning electron microscopy (SEM, FEI Nova NanoSEM 230) and transmission electron microscopy (TEM; JEOL-JEM-2100F transmission electron microscope). A combined Differential Scanning Calorimetry (DSC)/Thermogravimetric Analysis (TGA) instrument (Netzsch STA449C, Germany) was used to study the reactions during the annealing process and measure the carbon content in CW-LVP. Raman spectra were obtained using a Renishaw INVIA micro-Raman spectroscopy system. Nitrogen adsorption-desorption measurements were conducted at 77K (NOVA 4200e, Quantachrome Instruments).
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5

Characterization of BT-An@Zetag Composites

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BT-An@Zetag composite samples were analyzed using an X-ray diffractometer (Shimadzu XRD-7000, Tokyo, Japan with an X-ray wavelength Cu detector). Scanning electron microscopy was used to analyze the morphological topographies of BT-An@Zetag composites (SEM, JEOL JSM-6610 LV, Tokyo, Japan). Thermal gravimetric analysis (TGA-51 Shimadzu, Tokyo, Japan) and DSC were used to assess thermal changes across a temperature range of 25–600 °C (Shimadzu DSC-60 Plus, Tokyo, Japan). Raman spectrometer (Shimadzu IR–Tracer 100 Fourier Transform Infrared Spectrophotometer, Tokyo, Japan) was used to determine the Raman spectra of the BT-An@Zetag composite (HOUND UNCHAINED LABS spectrometer, Berlin, Germany). A NOVA 4200e was used to evaluate the nitrogen adsorption–desorption isotherms at 77 K (Quantachrome Instruments, Boynton Beach, FL, USA). The Brunauer–Emmett–Teller (BET) equation and the specific surface area were used to further investigate surface area and pore size.Also, Pore size distributions were also calculated using the Barrett–Joyner–Halenda (BJH) methods. Initial and final concentrations of arsenate were analyzed using Triple Quadrupole Inductively Coupled Plasma Mass Spectrometry (TQ-ICP-MS), Thermo Fishers scientific (Waltham, MA, USA).
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6

Comprehensive Characterization of Activated Carbon from Pumpkin Seed Shells

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The Fourier Transform-Infrared Spectroscopy (FT-IR, Bruker Vertex 70v, Billerica, MA, USA) analysis was performed to demonstrate that the activated carbon obtained from the pumpkin seed shell was functionalized with KOH. Scanning Electron Microscopy (SEM, Zeiss EVO 10, Oberkochen, Germany) analysis was used to examine the morphological structure of the adsorbent in detail. The elemental analysis technique (CHNS-932, Leco, Corporation, St. Joseph, MI, USA) was applied to determine the adsorbent’s elemental composition. Further, the adsorbent’s net load was determined using Zeta analysis (Malvern/Zetasizer Nano ZSP, United Kingdom). Additionally, X-ray Photoelectron Spectroscopy (XPS, PHI 5000 VersaProbe, Chanhassen, MN, USA) was utilized to measure the elemental composition of the material’s surface of the material and the binding states of the elements. Brunauer–Emmett–Teller (BET, Nova 4200e Quantachrome Instruments, Boynton Beach, FL, USA) analysis was performed to determine the adsorbent’s surface area of the adsorbent.
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7

Nitrogen Adsorption Analysis of Deproteinized Bovine Femur

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Deproteinized bovine (mineral only) femur was granulated by pestle and mortar. N2 adsorption/desorption isotherms were measured at 77 K in the range 1.00 × 10–2P/P0 ≤ 1.00 on a NOVA 4200e instrument by Quantachrome Instruments (Boynton Beach, Florida USA), running version 11.03 of the NovaWin software package. Ultrahigh purity N2 (99.999%) was purchased from Cryogenic Gasses and used as received. BET surface area was calculated using the BET assistant and pore size distributions were calculated using the Nonlocal Density Functional Theory (NLDFT) N2 silica adsorption branch kernel at 77 K based on a cylindrical/spherical pore model as implemented in NovaWin 11.03.
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8

Comprehensive Characterization of Nanomaterials

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For
recording FTIR readings, a Shimadzu IR Tracer-100 FTIR spectrophotometer
has been applied. Powder XRD profiles have been recorded using the
X-ray diffractometer Maxima—X (D/Max2500VB2+/Pc, Shimadzu Company,
Japan) with an X-ray wavelength Cu detector. Raman spectroscopic analysis
was conducted. The developed materials’ morphological features
were examined applying FESEM (Zeiss FESEM Ultra 60). A NOVA 4200e
(Quantachrome Instruments) surface area and pore size analyzer collected
the nitrogen adsorption–desorption isotherms at 77 K. FESEM
investigation using Zeiss FESEM Ultra 60 was conducted to investigate
the morphology of the nanocomposite. CO2 desorption (CO2-TPD) assessment was performed on a Quantachrom Nova Sorbimetric
system.
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9

Comprehensive Characterization of ZMAC Material

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ZMAC was
characterized by X-ray diffraction model Philips APD-3720 diffractometry,
DSC (TA Instruments Q2000 DSC), Raman spectra (Bruker, Senterra II,
Germany), TGA (Q500 equipment thermo gravimetric analyzer), scanning
electron microscopy (JSM-6700F, JEOL, Japan), and SBET. The nitrogen
adsorption-desorption isotherms at 77 K were measured using a NOVA
4200e (Quantachrome Instruments, USA). The specific surface area and
pore size were then analyzed using the Brunauer-Emmett-Teller (BET)
equation. Additionally, the pore size distributions were estimated
using the Barrett-Joyner-Halenda (BJH) technique based on the isothermic
adsorption branch.
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10

Characterization of Cellulose/TiO2 Monoliths

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The microstructure of cellulose/TiO2 monoliths was observed with a Scanning Electron Microscope (SEM, S-3000N, Hitachi Ltd., Tokyo, Japan) at 15 kV. Before observation, the samples were cut with a scalpel and coated with a thin layer of gold by an ion sputter apparatus (E-1010 Ion Sputter, Hitachi Ltd., Tokyo, Japan). The specific surface area of the cellulose monolith was measured by a nitrogen adsorption apparatus using the Brunauer-Emmett-Teller (BET) method (NOVA 4200e, Quantachrome Instruments, Boynton Beach, FL, USA). Energy Dispersive Spectroscopy (EDS, Quantax 400, Bruker, Germany) was adopted to investigate the chemical composition of the composite monolith surface. The chemical structure of the composite monolith was analyzed using a Nicolet Is 5 Fourier transform infrared spectrophotometer. The UV-Vis adsorption spectra were carried out using a Shimadzu UV-2550 spectrophotometer. XRD patterns were run on an X-ray diffractometer (Rigaku D/max-2550 VB/PC, RICOH Company, Ltd., Tokyo, Japan) at a scanning rate of 4.0°/min from 5° to 60° (2θ). The measurement was performed under conditions of 40 kV and 30 mA using Cu-Kα radiation (λ = 1.5418 Å). The surface chemical composition of the samples was analyzed by X-ray photoelectron spectroscopy (XPS, AXIS ULTRA DLD, Kratos Analytical Ltd., Manchester, UK) with an Al Kα radiation source.
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