Solution 1H NMR spectra were recorded at 500 or 600 MHz using a Bruker Avance 500 or 600 NMR spectrometer. Powder X-ray diffraction (PXRD) data were collected on a Rigaku Ultimate-IV X-ray diffractometer operating at 40 kV/30 mA using the Mo Kα line (λ = 1.5418 Å). Data were measured over the range of 5 − 40° in 5°/min steps over 7 min. Thermogravimetric analysis (TGA) was carried out using a Q5000IR analyzer (TA Instruments) with an automated vertical overhead thermobalance. The samples were heated at 10 °C/min using N2 as the protective gas. Single crystal X-ray diffraction data were collected on a Bruker D8 VENTURE CMOS X-ray diffractometer with graphite monochromated Mo Kα radiation (λ = 0.71073 Å). Diffuse reflectance spectra were recorded with a SHIMADZU UV-2550 spectrometer. UV-vis absorption spectra were recorded using a PerkinElmer Lambda 35 UV-vis spectrophotometer. Differential Scanning Calorimetric study (DSC) was carried out using a DSC Q100 analyzer (TA Instruments). The samples were heated at 10 °C/min using N2 as the protective gas. The FT-IR spectra were measured on a Perkin Elmer 480 FT-IR spectrophotometer (KBr pellet). The Raman spectra were measured on a Horiba scientific-LabRAM HR evolution.
Ultimate 4 x ray diffractometer
Manufactured by Rigaku
Sourced in Japan
The Ultimate IV X-ray diffractometer is a versatile laboratory instrument designed for the analysis of crystalline materials. It utilizes X-ray diffraction technology to provide detailed information about the atomic and molecular structure of a wide range of samples. The instrument is capable of performing various X-ray diffraction measurements, including powder diffraction, single-crystal diffraction, and thin-film analysis.
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Lab products found in correlation
Q5000ir analyzer, by TA Instruments (1 mentions)
Dsc q100 analyzer, by TA Instruments (1 mentions)
Scientific labram hr evolution, by Horiba (1 mentions)
Lambda 35 uv vis spectrophotometer, by PerkinElmer (1 mentions)
Uv 2550 spectrometer, by Shimadzu (1 mentions)
Tecnai g2 spirit transmission electron microscope, by Thermo Fisher Scientific (1 mentions)
Ntegra prima atomic force microscope, by NT-MDT (1 mentions)
5 protocols using ultimate 4 x ray diffractometer
1
Comprehensive Characterization of Solid-State Materials
2
Characterization of GK-OCMC Nanoparticles
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X-ray diffraction (XRD) patterns of GK, OCMC, and GK–OCMC were acquired by a Rigaku Ultimate IV X-ray diffractometer scanned at speed of 5°/min with ranging from 5° to 80°. The particle size and zeta potential of the GK–OCMC Nps were determined using dynamic light scattering (DLS) with the Nano-ZS90 Malvern Zetasizer (Malvern, UK) in triplicate at 25°C. The morphology of the GK–OCMC Nps was observed under a Tecnai G2 Spirit transmission electron microscope (FEI, USA) after negative staining with 2% (w/v) phosphotungstic acid. Furthermore, the surface characteristics of the Nps were reconfirmed by the NTEGRA Prima atomic force microscope (Nt-Mdt, Zelenograd, Russia), while Nova RC1 software (V1.0.26.1138, Nt-Mdt, Russia) was used for formation of images.
3
X-ray Diffraction Characterization
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WAXD measurements were carried on the Rigaku Ultimate IV X-ray diffractometer (Rigaku, Tokyo, Japan) with Cu Kα radiation (λ = 0.154 nm). The tests were under reflection mode with a range of 5°–40° and a scanning rate of 4°/min. The interplanar spacing d and the grain size Lhlk are calculated by Equations (2) and (3), respectively:
where d is the interplanar spacing, λ is the wavelength of the Cu Kα radiation (0.154 nm), θ is half of the diffraction angle, Lhlk is the average grain size perpendicular to the hlk crystal plane, Kα is the grain size constant (0.89), β is the full width at half maximum.
where d is the interplanar spacing, λ is the wavelength of the Cu Kα radiation (0.154 nm), θ is half of the diffraction angle, Lhlk is the average grain size perpendicular to the hlk crystal plane, Kα is the grain size constant (0.89), β is the full width at half maximum.
4
Comprehensive Physicochemical Characterization of Adsorbent
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The characteristic functional groups of the adsorbent were analyzed by Fourier Transform Infrared (FT−IR). FT−IR was performed by using Nicolet 6700 infrared spectroscopy (Thermo, Waltham, MA, USA). An X−ray diffractogram (XRD) of the sample was obtained by means of an Ultimate IV X−ray diffractometer (Rigaku, Japan), which was operated at 40 kV and 40 mA of CuKα radiation (λ = 0.154 nm). The surface morphology of the adsorbent was captured by scanning electron microscopy (SEM). SEM images were obtained on a JSM−7900F electron microscope instrument (JEOL, Tokyo, Japan). The pore property of the adsorbent was characterized by a fully automated specific surface and porosity analyzer (Nova 4000e, Quantachrome, Boynton Beach, FL, USA). The surface area and pore diameter of the adsorbents were obtained by Brunner−Emmet−Teller (BET) and Barret–Joyner−Halenda (BJH) methods [23 (link)]. Gas chromatography–mass spectrometry (GC−MS, 7890A-5975C, Agilent, Santa Clara, CA, USA) was used to analyze the organic composition of the coking wastewater before and after treatment. Before the GC−MS test, dichloromethane was used as the extractant to extract organic matter in the coking wastewater, and then the extract was concentrated by nitrogen purging.
5
Characterization of Porous Sand Media
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The sand was washed with a 0.1% HCl solution and later thoroughly washed with deionized water to remove any soluble impurities. To remove any organic compounds still present, it was calcined at 600 °C for 12 h. The resulting sand presented 30% of porosity and size distribution between 362 and 635 µm.
The mineral composition of the sand used as porous media was determined by X-ray diffraction (XRD) using a RIGAKU Ultimate IV X-ray diffractometer (Rigaku Corporation, Tokyo, Japan) which recorded the 2θ range 10–80° at a scan rate of 0.02°/min, using CuKα (λ = 1.54 Å) radiation. Also, thermogravimetric analysis (thermogravimetric analyzer TGA-51 from Shimadzu Brasil, Barueri, Brazil) was carried out in a heating rate of 10 °C/min and temperature range of 25–800 °C under a O2 atmosphere in order to evaluate the existence of organic matter adsorbed.
The mineral composition of the sand used as porous media was determined by X-ray diffraction (XRD) using a RIGAKU Ultimate IV X-ray diffractometer (Rigaku Corporation, Tokyo, Japan) which recorded the 2θ range 10–80° at a scan rate of 0.02°/min, using CuKα (λ = 1.54 Å) radiation. Also, thermogravimetric analysis (thermogravimetric analyzer TGA-51 from Shimadzu Brasil, Barueri, Brazil) was carried out in a heating rate of 10 °C/min and temperature range of 25–800 °C under a O2 atmosphere in order to evaluate the existence of organic matter adsorbed.
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