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29 protocols using sdt 650

1

Thermal Characterization of Materials by DSC and TGA

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Differential scanning calorimetry measurements (DSC) were performed on a DSC 25 from TA Instruments under a constant nitrogen flow (50 mL min–1). Before the measurement, the samples were ground and placed in a hermitically sealed aluminium crucible and a hole was pinched into the lid of the sealed crucible. Simultaneous thermogravimetric analysis/differential scanning calorimetry (TGA/DSC) measurements were conducted on an STA 504 instrument or SDT 650 from TA Instruments under a constant argon flow (4 L h–1) for STA 504 or a nitrogen flow (100 mL min–1) for SDT 650 on powdered samples. Data were processed and evaluated using the TRIOS (v5.1.0.46403) software from TA instruments. The melting temperatures (Tm) are determined as the peak offset, the glass transition temperatures (Tg) as the peak onset, whereas all other derived temperatures are defined as the peak temperature. The enthalpies are determined from the integral of the corresponding signal.
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2

Thermal Analysis of Metal-Organic Frameworks

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Thermogravimetric analysis was performed with a TA Instruments SDT-650 instrument using alumina cups and a 10 °C min−1 heating rate up to 600 °C in nitrogen atmosphere (N2 flow of ~100 mL/min). In the case of Mg2(dobpdc) and ii-2-Mg2(dobpdc) a heating rate of 3 °C min−1 was used with an upper temperature bound of 500 °C.
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3

CO2 Capture Capacity of NiRuK/CeAl Sorbent

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The CO2 capture capacity of the DFM was measured during a thermogravimetric analysis (TGA) experiment. The apparatus used was an SDT650 from TA Instruments. The NiRuK/CeAl sample was reduced ex situ at 800 °C for 1 h with 10% H2/N2 and a 50 mL min−1 total flow rate. In each run, approximately 15 mg of sample was used. The temperature was increased to 150 °C and maintained for 20 min to desorb any weakly adsorbed molecules. Then, the temperature was increased to 950 °C at a rate of 10 °C min−1. In the first experiment, 100 mL min−1 of Ar flow was used during the ramp stage, and in the second experiment, 20 mL min−1 of CO2 and 100 mL min−1 of Ar were used.
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4

Comprehensive Material Characterization

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The molecular arrangement was analyzed by Fourier transform infrared (FTIR) spectroscopy (Jasco 4700 Spectrophotometer, Jasco, Oklahoma City, OK, USA) using the attenuated total reflection (ATR) accessory and determining the main peaks in the 2000–800 cm−1 region. Thermogravimetric analysis (TGA, SDT 650, TA instruments, New Castle, DE, USA) was performed under oxygen flow (50 mL min−1) up to a temperature of 800 K increased in steps of 5 K min−1. Morphological features were examined using scanning electron microscopy (SEM, Quanta FEI 650FEG), also used to observe the atomic distribution of components by energy dispersive spectroscopy (EDS). The BET (Brunauer–Emmet–Teller) surface area (Sa), the BJH (Barrett–Joyner–Halenda), and cumulative adsorption pore volume between 1.7–300 nm (Vp) were determined by collecting N2 adsorption/desorption isotherms at 77 K (ASAP 2020, Micromeritics Inc., Norcross, GA, USA), after degassing the samples at 393 K for 20 h. The zeta potential values of the different bare components and nanocomposite were measured in aqueous suspensions (10 mg L−1) in the 2–8 pH range, adjusted with HNO3, using Malvern Zetasizer Nano ZS equipment (Malvern, UK).
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5

Biochar Characterization by Thermogravimetry

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All the investigated carbons were analyzed by thermogravimetric analysis in the range 30–850 °C, in air flow, and with a heating rate of 10 °C/min (SDT 650, TA Instruments, New Castle, DE, USA). The produced biochars (namely SPBCP and SPBCG) were also characterized in terms of textural properties. In this regard, the specific surface area (SSA) of the produced samples were obtained by adopting the Brunauer–Emmett–Teller model (B.E.T.) to nitrogen adsorption isotherms performed at 77 K with an ASAP 2020 Micromeritics instrument. In particular, the B.E.T. was applied in the P/P° range 0.01–0.1 in order to obtain a positive C-value, which is exponentially related to the adsorption energy of the monolayer [33 (link)]. Total pore volume was calculated at P/P° = 0.99. Pore size distribution was determined by Non-Local Density Functional Theory (NLDFT) by using MicroActive Version 4.06 software (Micromeritics, Norcross, GA, USA) and by adopting an available model for carbon slit-shape pores. Before the analysis, the investigated samples were degassed, by heating at 300 °C, at a rate of 5 °C min−1, under a high vacuum (<10−8 mbar) for 12 h. Scanning electron microscope (SEM) images of the investigated samples were collected by a scanning electron microscope (FEI model Inspect, ThermoFisher Scientific, Hillsboro, OR, USA).
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6

Comprehensive Material Characterization Protocol

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A ThermoFisher Scientific (Waltham, MA, USA) Nicolet iS 10 FTIR spectrometer was used for FTIR characterizations. 1D 1H and 13C NMR were performed using a Bruker (Billerica, MA, USA) Avance 300 MHz NMR spectrometer, while 2D 1H-1H COSY and 1H-13C HMBC NMR were performed on a Bruker (Billerica, MA, USA) Avance 600 MHz NMR. All NMR spectra were collected in D2O. Thermogravimetric analysis was performed using a TA Instruments (New Castle, DE, USA) simultaneous thermal analyser (SDT 650) under nitrogen atmosphere. Data were collected from 30 to 800°C at a heating rate of 10°C min−1 after water was removed through equilibration at 110°C for 4 min. Scanning electron microscopy (SEM) images were obtained in backscatter mode using a Phenom ProX SEM (Phenom-World B.V., Eindhoven, Netherlands).
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7

Comprehensive Material Characterization Protocol

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X-ray powder diffraction
(XRD) measurements were taken using a PAN analytical X-ray diffractometer
(Cu Kα source, λ = 1.54178 Å). X-ray Rietveld refinement
was performed with the FullProf Software package. The scanning electron
microscopy images were obtained via a Carl Zeiss Ultrafield-emission
scanning electron microscopy (FESEM) unit equipped with energy-dispersive
spectroscopy (EDS). The materials’ morphology and microstructure
were examined further using transmission electron microscopy (TEM;
JEOL-JEM-2100F). Fourier transform infrared spectroscopy (FTIR) was
performed with a PerkinElmer (Spectrum 2) spectrophotometer at a resolution
of 4 cm–1 in the scanning range of 400–4000
cm–1. The thermal stabilities of the samples were
determined using the TA Instruments SDT650 thermogravimetric analysis
(TGA) method. N2 adsorption–desorption studies were
performed using the Brunauer–Emmett–Teller (BET) method
via a Quantachrome Nova 2000e BET analyzer. The Co/Ni ratio in the
CoNi-MOF was analyzed by inductively coupled plasma-atomic emission
spectrometry (ICP-AES) using IRIS Intrepid II XSP (Thermo Fisher Scientific).
X-ray photoelectron spectroscopy (XPS) spectra were obtained using
a Thermo Fisher Scientific ESCALAB250Xi spectrometer. 1H NMR and 13C NMR spectra were provided via a Bruker spectrometer
(MSL 400).
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8

Thermal Stability and CO2 Desorption of IL-Loaded SAPO-34

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The
thermal stability, the mass fraction
of IL in the loaded sample, and the values of CO2 desorption
heat for [Bmim][Ac], SAPO-34, and SAPO-34-IL were determined using
TGA and DSC (TA, SDT650). The samples were heated from room temperature
to 373 K at 10 K min–1 under 50 mL min–1 nitrogen (N2) atmosphere until no significant weight
loss was observed and then heated to 673 K at 10 K min–1. The decomposition temperatures of pure and loaded IL, as well as
the loading of IL were calculated using thermogravimetric (TG) curves
and derivative TG curves. Additionally, the CO2 desorption
heat was obtained from the DSC heat flow curve of the CO2 sorption.
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9

FTIR and Thermogravimetric Analysis of Modified Nanoparticles

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The FTIR spectra of the modified nanoparticles and films were recorded using an Agilent Cary 660 instrument. The analysis was carried out using an Attenuated Total Reflectance (ATR) mode in 4000 to 400 cm−1. The thermogravimetric analysis was carried out with the help of differential scanning calorimeter equipment from TA instruments, model SDT 650, with a simultaneous thermogravimetric analyzer. The analysis was conducted with a 10 °C/min ramp in a temperature range of 25–600 °C under a nitrogen atmosphere.
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10

Thermogravimetric Analysis of Sample

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The thermogravimetric analysis of the sample was
carried out with an SDT 650 instrument (TA Instruments, New Castle,
DE, USA) A sample (5.52 mg) was placed in an alumina pan. Measurement
was performed in the temperature range 19–700 °C with
a heating rate of 10 °C/min, using nitrogen as the purge gas.
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