X-ray diffraction patterns of powders (obtained from tablets dried and ground after exposure to SGF and/or SIF) were recorded using a Siemens D-5000 diffractometer [with silicon detector] in reflectance mode at a Co Kα wavelength of 1.79018 Å over an angular range 5–50°. The spectra obtained were analyzed using Diffract-AT software.
D5000 diffractometer
Manufactured by Siemens
Sourced in Germany, United States
The D5000 diffractometer is a laboratory equipment product manufactured by Siemens. It is designed to perform X-ray diffraction analysis, a widely used technique for the characterization of crystalline materials. The core function of the D5000 diffractometer is to measure and analyze the diffraction patterns produced when a sample is exposed to an X-ray beam, providing information about the structure and composition of the material.
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Lab products found in correlation
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Nicolet 6700, by Thermo Fisher Scientific (3 mentions)
Ultrospec 2100 biochrom spectrophotometer, by Harvard Bioscience (2 mentions)
Jem 1400 transmission electron microscope, by JEOL (2 mentions)
S 4800, by Hitachi (2 mentions)
Stadi p diffractometer, by STOE (2 mentions)
8101m ft ir, by Shimadzu (2 mentions)
Quanta 450, by Thermo Fisher Scientific (2 mentions)
Spectrum one spectrophotometer, by PerkinElmer (2 mentions)
Jsm 7610f, by JEOL (2 mentions)
Em10c 100 kv, by Zeiss (2 mentions)
Vector 22, by Bruker (2 mentions)
Supra 40, by Zeiss (2 mentions)
Pulverisette 6, by Fritsch (1 mentions)
Diamond tg dta, by PerkinElmer (1 mentions)
S 4800 scanning electron microscope, by Hitachi (1 mentions)
Lambda 35 spectrophotometer, by PerkinElmer (1 mentions)
Model 744, by Metrohm (1 mentions)
Ppp nchr tips, by Nanosensors (1 mentions)
81 protocols using d5000 diffractometer
1
X-ray Diffraction Analysis of Tablet Powders
2
XRPD Analysis of Polymorphic Forms of Compound 1
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Example 19
XRPD analysis of amorphous and Forms II, III, IV, V, VI, VII, and VIII of Compound 1 was carried out on a Siemens D5000 diffractometer, scanning the samples between 3 and 30 degrees 2θ. Material was gently compressed on a glass disc inserted into a sample holder. The sample was then loaded into the diffractometer running in reflection mode, and the analysis was conducted using the following experimental conditions.
3
Mineralogical Analysis of TCC Material
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Mineralogical analysis was first carried out to determine the mineral components of the TCC material using an X-ray diffraction method. A powdered sample was prepared from the scrapings of the freshly exposed TCC surface, excluding visually-observable coarse particles from the sample blocks, and this was then ground with anhydrous ethanol (used as coolant and lubricant) in a McCrone micronizing mill (Verder Scientific Inc., Nwetown, PA, USA) for three minutes to obtain binder particles smaller than 45 μm in size.
X-ray diffraction (XRD) was conducted on the powdered sample, which had a random particle orientation, in a Siemens D-5000 diffractometer (Karlsruhe, Germany) using Cu-Kα radiation generated at 40 kV and 30 mA, using a scan range of 2°–70° (2θ, where θ is the diffraction angle). The scan used a 0.996° divergence slit, 0.501° scatter slit, and 0.1 mm receiving slit at a rotating speed of 1° 2θ/min and a step size of 0.02° 2θ. XRD patterns were analyzed both qualitatively and quantitatively. A computer program, Jade 9.0 (MDI, Livermore, CA, USA), was used to identify and match the XRD reflections, while semi-quantitative analysis was based on the methodology developed by Cook et al. [15 ], and an in-house computer program, XRDPhil (Philips electronic Co., Eindhoven, The Netherlands), was used to estimate the mass fractions of the major identified mineral phases.
X-ray diffraction (XRD) was conducted on the powdered sample, which had a random particle orientation, in a Siemens D-5000 diffractometer (Karlsruhe, Germany) using Cu-Kα radiation generated at 40 kV and 30 mA, using a scan range of 2°–70° (2θ, where θ is the diffraction angle). The scan used a 0.996° divergence slit, 0.501° scatter slit, and 0.1 mm receiving slit at a rotating speed of 1° 2θ/min and a step size of 0.02° 2θ. XRD patterns were analyzed both qualitatively and quantitatively. A computer program, Jade 9.0 (MDI, Livermore, CA, USA), was used to identify and match the XRD reflections, while semi-quantitative analysis was based on the methodology developed by Cook et al. [15 ], and an in-house computer program, XRDPhil (Philips electronic Co., Eindhoven, The Netherlands), was used to estimate the mass fractions of the major identified mineral phases.
4
High-Energy Ball Milling Synthesis of (K0.5Na0.5)NbO3
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For high-energy ball milling synthesis of (K0.5Na0.5)NbO3, all analytical grade K2CO3, Na2CO3, and Nb2O5, which were purchased from Aldrich (Germany), were dried at 200°C for 2 h prior to use in order to remove moisture. Stoichiometric mixtures of these raw materials were placed in a 125 mL stainless-steel vial of a Fritsch Pulverisette 6 planetary mill. The rotational speed was changed from 300 to 600 rpm. Different numbers of stainless-steel milling balls with diameters of 10 and 20 mm were used depending on the ball-to-powder weight ratio ranging from 25/1 to 40/1. For investigation of thermal decomposition of intermediate carbonate complex, as-milled samples synthesized at optimized conditions were calcined at temperatures ranging from 300 to 1000°C for 3 h. X-ray diffraction diagrams of obtained samples were recorded using Siemens D-5000 diffractometer (Siemens, Germany) with CuKα radiation. For the determination of lattice parameters, Si (Aldrich, Germany) was used as an internal standard. The synthesized samples were also characterized by field-emission scanning electron microscopy (FE-SEM, Hitachi S 4800 microscope, Japan), Fourier transform infra-red spectroscopy (FTIR, GX-Perkin-Elmer, USA), and thermal analysis (Setaram Labsys Evo thermal analyser, France).
5
XRPD Characterization of Compound 1 Polymorphs
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Example 19
XRPD analysis of amorphous and Forms II, III, IV, V, VI, VII, and VIII of Compound 1 was carried out on a Siemens D5000 diffractometer, scanning the samples between 3 and 30 degrees 2θ. Material was gently compressed on a glass disc inserted into a sample holder. The sample was then loaded into the diffractometer running in reflection mode, and the analysis was conducted using the following experimental conditions.
6
Structural and Surface Analysis of Nanofibers
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The crystal structure of the as-prepared nanofibers was characterized using powder X-ray diffraction [XRD, Siemens D-5000 diffractometer with Cu–Kα irradiation (λ = 1.5406 Å)]. The microstructure of the samples was characterized using a HITACHI S4800 scanning electron microscope (SEM), a transmission electron microscope (TEM), and a high-resolution TEM operating at 200 kV. The samples were also analyzed by X-ray photoelectron spectroscopy (XPS, Surface Science Instruments S-probe spectrometer). The Raman spectrum was acquired at room temperature with excitation laser lines of 514 nm (Renishaw). Specific surface areas were measured using a Tristar II 3020 instrument by adsorption of nitrogen at 77 K. The pore diameter distribution of the mesopores was tested by nitrogen adsorption/desorption analysis (MicroActive ASAP 2460). The thermal gravimetric analysis was recorded on a thermogravimetric analyzer (TGA, PerkinElmer, Diamond TG/DTA) with a heating rate of 10 °C min−1 in air from 30 to 800 °C.
7
Optoelectronic Characterization Protocol
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The UV-vis spectra were performed using a Perkin Elmer Lambda 35 spectrophotometer. Photoluminescence spectra have been performed with a “Jobin Yvon-Spex Spectrum One” CCD detector, cooled at liquid nitrogen temperature. The X-ray diffraction (XRD) patterns of films were measured by A Siemens D5000 diffractometer. The current–voltage characteristics under illumination with Xe Oriel solar simulator were obtained with a Keithley 6430 source.
8
Structural Analysis of Thin Films
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Film structures were determined by x-ray diffraction (XRD) using a Siemens D5000 diffractometer operating with CuKα radiation at a wavelength of 0.154 nm. XRD analysis indicated amorphous structures. Elemental compositions and atomic concentrations were determined by Rutherford Backscattering Spectrometry (RBS) at the Uppsala Tandem Laboratory, specifically using 2 MeV 4He ions backscattered at an angle of 170 degrees. The RBS data were fitted to a model of the film–substrate system by use of the SIMNRA program24 . Film density ρ was ~5.5 g cm−3 as computed from
where M is molar mass, Ns is areal density of atoms, natoms is the number of atoms in a molecule, and NA is Avogadro’s constant.
where M is molar mass, Ns is areal density of atoms, natoms is the number of atoms in a molecule, and NA is Avogadro’s constant.
9
Synthesis and Characterization of TiO2 Nanoparticles
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All spectrophotometric measurements and the characterization of the synthesized nanoparticles were carried out by measuring the UV-Vis spectrum of the as-prepared TiO2 nanoparticles using an Ultrospec 2100-Biochrom spectrophotometer (Biochrom Ltd., Cambium, Cambridge, UK). Fourier-transform infrared (FTIR) spectra of the formed nanoparticles and their bionanocomposites were recorded using PerkinElmer FT-IR spectrophotometer (PerkinElmer Ltd., Yokohama, Japan). The morphologies of TiO2 NPs and the polymeric P. cylindraceus oil/TiO2/PEG bionanocomposite were measured by scanning electron microscope (JEM-2100F, JEOL Ltd., Akishima, Tokyo, Japan) and JEM-1400 transmission electron microscope (JEOL Ltd., Akishima, Tokyo, Japan). XRD patterns of TiO2 nanoparticles and the bionanocomposite were obtained by Siemens D-5000 diffractometer (Siemens, Erfurt, Germany). The pH-meter Metrohm model 744 (Metrohm Co., Herisau, Switzerland) was used to control the pH condition of the test solution. Distilled water (H2O) was used throughout the experimental study. Thermal stability analysis was conducted using a Shimadzu thermogravimetric analyzer (TGA-502 model). Nikon ECLIPSE fluorescence microscopy (Ti-E, Japan) was used to analyze cancer cell apoptosis.
10
X-Ray Powder Diffraction Characterization
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XRPD diffractogram at 25˚C provided another piece of information for the identification and crystallinity of starting materials and co-crystals. Moreover, the powder diffraction patterns generated with the single-crystal data of compounds (I-V) using Mercury [20 (link)] matches accurately these experimental XRPD spectra measured using the D5000 powder diffractometer, thereby confirming the purity of the synthesized co-crystals. XRPD diffractograms were collected by SIEMENS D5000 DIFFRACTOMETER. The source of XRPD was CuKα (1.542 Å) and the diffractometer was operated at 40 kV and 30 mA. The X-ray was passed through a 1 mm slit and the signal a 1 mm slit, a nickel filter, and another 0.1 mm slit. The detector type was a scintillation counter. The scanning rate was set at 0.05° ranging from 5° to 35°. The quantity of sample used was around 20–30 mg.
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