Ultima 4 diffractometer

The analysis was performed with a Rigaku Ultima IV Diffractometer (CuKα source with λ = 1.54184 Å) with a scintillation counter and diffracted beam monochromator, using a scanning range (2θ) of 10°–90° with a 0.02° step size at a scan rate of 0.5°/min.

The chemical formulas of the samples were determined by elemental analyses. The ratios of the metals (Cs, K, Mn, and Fe) were obtained by inductively coupled plasma mass spectroscopy using Agilent 7700. The amounts of C, H, and N contained in the samples were determined by standard microanalytical methods. The chemical formula, K^I_aCs^I_bMn^II[Fe^II(CN)₆]_c[Fe^III(CN)₆]_d·zH₂O, was determined considering charge neutrality. Because the valences of K^I, Cs^I, Mn^II, [Fe^II(CN)₆], and [Fe^III(CN)₆] are +1, +1, +2, −4, and −3, respectively, a + b + 2 − 4c − 3d = 0 should be satisfied. For the far-infrared measurements, a JASCO 6100 spectrometer was used. XRD measurements were performed with a Rigaku Ultima IV diffractometer with a Cu K_α radiation (λ = 1.5418 Å). The PDXL program of Rigaku was used for Rietveld analyses.

DSC, TGA, and PXRD analyses were carried out for the evaluation of the pure TMZ and equilibrated TMZ samples acquired from the bottom phase of the solubility sample in water [17 (link),18 (link)]. DSC and TGA characterization of TMZ and its equilibrated sample from water were evaluated using the “DSC 8000 (Perkin Elmer, Shelton, CT, USA)” and “Pyris 1 TGA analyser (Perkin Elmer, Shelton, CT, USA)” respectively, in the temperature range from 323.2 K to 573.2 K. PXRD analysis was performed using the “Ultima IV Diffractometer (Rigaku Inc. Tokyo, Japan)”, and both TMZ and its equilibrated sample were analyzed from the 3° to 80° 2-theta range.

XRD evaluation of GA powder was performed for crystal size and phase detection using Ultima IV diffractometer (Rigaku Corporation, Tokyo, Japan) over 3–140° 2θ range at 2.0 deg./min scan speed. Based on the reported procedures, the crystallinity and crystallite were determined [16 (link)]. The tube anode was Cu with Ka = 0.154 nm monochromatized with a graphite crystal. The pattern was collected at tube voltage (40 kV) and tube current (40 mA) in step scan mode (step size 0.02°, counting time 1 s per step).

X-ray diffraction measurements of pure QTF and the optimum formula were performed using an Ultima IV Diffractometer (Rigaku Inc. Tokyo, Japan at College of Pharmacy, King Saud University, Riyadh, KSA). The XRD spectra were scanned in the range of 0–60° (2θ) at a rate of 10°/min speed.

X-ray diffractogram of samples were recorded at a room temperature using PXRD (Rigaku Ultima IV diffractometer, Rigaku Corporation, Tokyo, Japan) operated at 40 kV and 40 mA power settings. About 300 mg of NCSD was placed in a polymethyl methacrylate sample holder, and analysis was carried out in a continuous scan mode with a step size of 0.01° over 1 sec in range of 3° to 50° 2θ values. The diffraction patterns were analyzed using OriginPro version 9.1 software (OriginLab Corporation, Massachusetts, MA, USA, 2018).

For the characterization of nanobioconjugates, we used X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), high-resolution transmission electron microscopy (HR-TEM) and dynamic light scattering (DLS) techniques, presented in detail in our previous reference [18 (link)].
XRD was used to determine the crystalline phases and the average size of the nanocrystallites. A Rigaku UltimaIV Diffractometer with Cu Kα radiation was used for this.
FT-IR was used for the study of ferrite formation and the determination of specific Me–O bonds (Me: metal, O: oxygen) in the magnetite structure. A Shimadzu IR Affinity-1S spectrophotometer was used in the 400–4000 cm⁻¹ range.
The morphology of the sample, and the size and distribution of the nanoparticles was studied via HR-TEM, using a Hitachi TEM system (HT7700) with 0.2 nm resolution.
Using the Vasco Particle Size Analyzer, the average hydrodynamic diameter of the nanobioconjugates in dispersion and their distribution was determined using DLS.