D8 focus powder diffractometer

For crystal-phase composition analysis, the XRD patterns of FA and MFA were obtained via the D8 focus powder diffractometer (Bruker, Germany) using Cu Kα radiation with the tube voltage of 40 kV and tube current of 40 mA. Data was obtained at an increment of 0.019° and the scanning speed of 5 degrees s⁻¹. The quantitative phase analysis was performed by the Rietveld method using the Topas5.0 software package. Moreover, the micro-morphology of the fractured surface of MFA was investigated via the Nova Nano SEM450 field-emission electron microscope (FESEM) obtained from FEI using an acceleration voltage of 1.00 kV. An FTIR spectrum was obtained by the Tensor27 Fourier-transform infrared spectrometer (Bruker, Germany) using thin films prepared on KBr. Lastly, the element and valence of FA and MFA were analyzed by X-ray photoelectron spectroscopy (Thermofisher, America) using Al Kα radiation with a full-spectrum pass energy of 100.0 eV, step size of 1.00 eV, narrow-spectrum pass energy of 30.0 eV, step length of 0.05 eV, and a binding energy that was corrected based on the binding energy of C 1s (binding energy = 284.8 eV).

The chemical co-precipitation process was used for the fabrication of pure ZnO (Al Bitar et al., 2022 (link)), Zn_0.9La_0.1O, Zn_0.9Ce_0.1O, and Zn_0.9La_0.05Ce_0.05O. An adequate amount of ZnCl₂, LaCl₃, CeCl₃·7H₂O, and 0.1 M EDTA were weighed and then dissolved in distilled water as a dispersing solvent. The solutions were then titrated by 4 M NaOH, added in drop-wise with constant stirring, until pH reached 12. The solutions were then heated for 2 h at 60 ℃ with constant stirring, and washed several times with distilled water until the pH reduced to 7. The obtained white precipitates were then dried at 100 ℃ for 18 h, ground and calcinated at 550 ℃ for 4 h. From now on, pure ZnO, Zn_0.9La_0.1O, Zn_0.9Ce_0.1O, and Zn_0.9La_0.05Ce_0.05O will be referred to as ZnO-Pure, ZnO-La, ZnO-Ce, and ZnO-LaCe, respectively.
The prepared samples were characterized by X-ray Diffraction (XRD) using Bruker D8 Focus powder diffractometer, with Cu $K_{\alpha }$ radiation (λ = 1.54056 Å) in the range of 25° ≤ 2θ ≤ 80°. The surface morphology of the prepared NPs was measured using Transmission electron microscope (TEM) JEM-1400 Plus. Using the photoluminescence spectrophotometer FP-8600 with an excitation wavelength of 325 nm and a wavelength ranges from 350 to 700 nm, the emission spectra of the synthesized NPs were examined.

TLC was performed on silica gel GF254 plates (Qingdao Haiyang Chemical Co., Ltd., Qingdao, China). Compounds were visualized by irradiation with UV light or by treatment with 0.05 g/mL ninhydrin in ethanol or potassium iodide reagent. ¹H-NMR and ¹³C-NMR were recorded on a Bruker Avance-400 MHz instrument (Bruker BioSpin AG, Fällanden, Switzerland). HRMS were obtained with a LC-ESI-Q-TOF-MS apparatus (Waters, Milford, MA, USA). HPLC analysis of GLYX-13 was performed on an Agilent LC 1100 system (Agilent Technologies Inc., Santa Clara, CA, USA) equipped with a diode array detector. Chiral analysis of intermediate were carried out using a Shimadzu LC 20AD system (SIMADZU, Kyoto, Japan) with a SPD-20A UV detector or an Agilent LC 1100 system equipped with a diode array detector. Single crystal diffraction analysis of 7 was performed on a MicroMax-003 (Rigaku Corporation, Tokyo, Japan) X-ray single crystal diffractometer and powder diffraction analysis of 7 was performed by a Bruker D8 FOCUS powder diffractometer (Bruker BioSpin AG, Fällanden, Switzerland). The L-amino acids (protected or free) were obtained from GL Biochem Ltd. (Shanghai, China). Other reagents were provided by Aladdin (Shanghai, China). The organic solvents were commercially available products (Lingfeng Chemical Reagent Co., Ltd., Shanghai, China) and were used without further purification.