Variable-temperature powder X-ray diffraction measurements were carried out with an ARL X’TRA diffractometer (Thermo Fisher Scientific, Waltham, MA, USA) and HTK2000 (Anton Paar GmbH, Graz, Austria) using Cu-Kα radiation (λ = 1.54 Å) operated at 40 mA and 45 kV. A tungsten block acted as a sample holder. The thickness layer measured ca. 50 μm. Patterns were collected in the 2θ range of 10–35° with a step size of 0.05° and 4.0 s counting per step. The copper block with the sample was heated at the rate of 300 °C/min. Temperature control was performed by Eurotherm 2604 (Eurotherm Ltd., Worthing, UK) with BP5\20 thermal element. Data recollection lasted 7 min. Diffraction data were collected at 25, 130, and 170 °C so that changes in structure during heating could be observed. The samples were vacuumed, the residual pressure ranged from 5 × 10−5 to 5 × 10−4 Pa.
Arl x tra diffractometer
Manufactured by Thermo Fisher Scientific
Sourced in United States, Switzerland
The ARL X'TRA diffractometer is a laboratory instrument designed for X-ray diffraction analysis. It is used to identify and quantify the crystalline phases and structures present in solid materials. The ARL X'TRA provides high-resolution measurements and data analysis capabilities for a wide range of applications.
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Lab products found in correlation
Originpro software, by OriginLab (1 mentions)
Pulverisette 9, by Fritsch (1 mentions)
Toc 5050 ssm 5000 a, by Shimadzu (1 mentions)
Flash 2000, by Thermo Fisher Scientific (1 mentions)
4300 handheld ftir, by Agilent Technologies (1 mentions)
Merlin field emission scanning electron microscope fe sem, by Zeiss (1 mentions)
Aas 3, by Zeiss (1 mentions)
Alpha ftir spectrometer, by Bruker (1 mentions)
Vario micro cube, by Elementar (1 mentions)
8 protocols using arl x tra diffractometer
1
Variable-Temperature Powder X-Ray Diffraction of Samples
2
Characterization of Porous Materials
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The values of specific surface area (SSA) were determined by the Brunauer–Emmett–Teller (BET) method. The data were obtained by low-temperature argon adsorption using an ASAP-2400 analyzer (Micromeritics Instrument Corp., Norcross, GA, USA).
X-ray powder diffraction (XRD) analysis was made on an ARL X’tra diffractometer (ThermoFisher Scientific, Waltham, MA, USA) with a Cu–Kα radiation source (λ = 1.5418 Å). The diffraction patterns were registered in a 2θ range of 15–85° with a step of 0.05° and a signal accumulation time of three s per step. Rietveld profile refinement of the XRD patterns was calculated using a GSAS–II program [49 (link)].
The Electron Paramagnetic Resonance (EPR) spectra were recorded at room temperature using a Varian E-109 spectrometer (Varian Instruments, Palo Alto, CA, USA) operating in the X–band. The g-factors were obtained with reference to a standard 2.2-diphenylpicrylhydrazyl (DPPH) resonance at g = 2.0036. The weighted portion of copper (II) sulfate pentahydrate (CuSO4·5H2O) was used to evaluate the concentration of paramagnetic species. The intensities of EPR spectra were determined by numerical double integration with baseline compensation using standard OriginPro software (v. 9.1.0; OriginLab Corp., Northampton, MA, USA).
X-ray powder diffraction (XRD) analysis was made on an ARL X’tra diffractometer (ThermoFisher Scientific, Waltham, MA, USA) with a Cu–Kα radiation source (λ = 1.5418 Å). The diffraction patterns were registered in a 2θ range of 15–85° with a step of 0.05° and a signal accumulation time of three s per step. Rietveld profile refinement of the XRD patterns was calculated using a GSAS–II program [49 (link)].
The Electron Paramagnetic Resonance (EPR) spectra were recorded at room temperature using a Varian E-109 spectrometer (Varian Instruments, Palo Alto, CA, USA) operating in the X–band. The g-factors were obtained with reference to a standard 2.2-diphenylpicrylhydrazyl (DPPH) resonance at g = 2.0036. The weighted portion of copper (II) sulfate pentahydrate (CuSO4·5H2O) was used to evaluate the concentration of paramagnetic species. The intensities of EPR spectra were determined by numerical double integration with baseline compensation using standard OriginPro software (v. 9.1.0; OriginLab Corp., Northampton, MA, USA).
3
Soil pH and Mineralogy Determination
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We measured soil pH H2O with a MetrohmTM pH-meter, using 10 g of 2 mm sieved soil mixed with 25 mL of deionized water and agitated for 16 h [22 (link)]. Litter was crushed and powdered (5–10 µm) using a Pulverisette 9 (Fritsch, Welden, Germany). Then we determined its mineralogical content using an ARL Xtra diffractometer (Thermo, Waltham, MA, USA). We analyzed the diffractograms using the MacDiff software and converted peak intensities of major minerals into relative abundances [33 ].
4
Comprehensive Characterization of Organic-Clay Interactions
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The concentration of organic carbon in solution was measured using an elemental analyzer (Shimadzu TOC 5050 /SSM 5000-A). Moreover, elemental analyses (Carbon, Nitrogen) on powder form samples were performed by using a Thermo Scientific Flash 2000 organic analyzer.
Fourier transform infrared (FTIR) measurements in the range 650-4000 cm -1 , were recorded using a Thermo Nicolet 6700 FT spectrometer equipped with a Deuterated Triglycine Sulfate (DTGS) detector and a Nicolet Continum microscope. The powder samples were spread over a NaCl window of the microscope. The analyzed sample area was a square of side 100 m chosen under the microscope 15X Infinity Reflechromat objective. The analyses were performed in transmission mode and each spectrum was the average of 256 scans collected at 2 cm -1 resolution.
The d 001 spacing's of the starting Mt clay mineral and after being in contact with organic pollutants were determined by the first 00l reflection from the X-rays patterns which were recorded in a conventional θ-θ Bragg-Brentano configuration by using a Thermo Electron ARL'XTRA diffractometer equipped with a Cu anode (CuK α1,2 = 1.5418 Å) coupled with a Si(Li) solid detector. The diffractograms on dry samples (100°C for 24 hours) were performed between 2 and 64° (2θ) with an angular and time steps of 0.04° and 10s respectively.
Fourier transform infrared (FTIR) measurements in the range 650-4000 cm -1 , were recorded using a Thermo Nicolet 6700 FT spectrometer equipped with a Deuterated Triglycine Sulfate (DTGS) detector and a Nicolet Continum microscope. The powder samples were spread over a NaCl window of the microscope. The analyzed sample area was a square of side 100 m chosen under the microscope 15X Infinity Reflechromat objective. The analyses were performed in transmission mode and each spectrum was the average of 256 scans collected at 2 cm -1 resolution.
The d 001 spacing's of the starting Mt clay mineral and after being in contact with organic pollutants were determined by the first 00l reflection from the X-rays patterns which were recorded in a conventional θ-θ Bragg-Brentano configuration by using a Thermo Electron ARL'XTRA diffractometer equipped with a Cu anode (CuK α1,2 = 1.5418 Å) coupled with a Si(Li) solid detector. The diffractograms on dry samples (100°C for 24 hours) were performed between 2 and 64° (2θ) with an angular and time steps of 0.04° and 10s respectively.
5
Characterization of MOF Degradation
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PXRD data of MOF samples at different degradation stages were collected in the 3–70° range by the ARL X’TRA diffractometer (Thermo Electron Corporation, Ecublens, Switzerland) using CuKα radiation source at a 0.02° step size and a 5°/min scanning rate.
6
Structural Characterization of Compounds
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The structures of the compounds were determined using a Fourier-transform infrared spectroscopy Nicolet 6700 spectrometer (Thermo Electron Scientific Instruments Corporation, Madison, WI, USA) equipped with a model 300 photoacoustic cell (FTIR-PAS) (MTEC Photoacoustics, Inc., Oakland, California, USA) and an attenuated total reflection Fourier-transform infrared spectroscopy (ATR-FTIR) instrument (4300 Handheld FTIR, Agilent Technologies, USA). The surface morphologies were obtained using a MERLIN field emission-scanning electron microscope (FE-SEM) (Carl Zeiss Microscopy GmbH, Jena, Germany), and the surface elemental compositions and distribution were analyzed using a Thermo Fisher 250Xi X-ray photoelectron spectrometer (XPS) and an energy-dispersive spectroscopy (EDS) detector attached to the SEM. The powder X-ray diffraction (PXRD) data were collected in the 5–80° range using an ARL X'TRA diffractometer (Thermo Electron Corporation, Switzerland). The elemental compositions were measured by laser-induced breakdown spectroscopy (LIBS) with a MobiLIBS system (IVEA, France), an iCAP 7000 inductively-coupled plasma optical emission spectrometer (ICP-OES, Thermo Fisher Scientific, USA), and a CHN-O-Rapid elemental analyzer (Heraeus, Germany).
7
Powder X-Ray Diffraction Characterization
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PXRD data were collected in the 3–70° range by the ARL X’TRA diffractometer (Thermo Electron Corporation, Ecublens, Switzerland) using CuKα radiation source at 0.02° step size and 5°/min scanning rate, and the powder XRD data of MOF was compared to the International Centre for Diffraction Data (ICDD) for phase identification.
8
Multi-Technique Characterization of Copolymers
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The content of C, H, N was determined on an element analyzer “Vario Micro cube” (Elementar GmbH, Hanau, Germany). The content of metals (Cu, Zn) was found using an atomic absorption spectrometer “AAS-3” (Zeiss, Jena, Germany). DSC and TGA curves and mass spectra of gaseous products were recorded using an STA 409 C Luxx (NETZSCH, Selb, Germany) conjugated with quadrupole mass spectrometer QMS 403C Aeolos and METZSCH STA 409 PC/PG. The samples were heated in an argon atmosphere at a heating rate of 10 K min−1 in the temperature range 30–500 °C. Attenuated total reflection infrared (ATR-FTIR) spectra of the polymers were recorded on an ALPHA FTIR spectrometer (Bruker, Shelton, CT, USA). A monolithic diamond crystal with an aperture angle of 45° was used as an element of internal reflection. The wavenumber was varied from 4000 to 1000 cm−1; number of scans—16; resolution is 4 cm−1. UV-vis-NIR-spectra were recorded using a SPECS-SSP-705-1 spectrometer (JSC “Spectroscopic Systems”, Moscow, Russia). The obtained copolymers were analyzed for phase identification and crystallinity by X-ray powder diffraction (XRD) on an ARLX’TRA diffractometer (Thermo Electron Corp. Waltham, MA, USA) (step size—0.02 °C, radiation—CuKα, λ = 1.540598 Å).
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