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20 protocols using jnm ecz600r

1

Structural Characterization of COS Precipitates

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The crystal structures of the as-prepared COS and collected precipitates were studied using the X-ray diffractometer (XRD, Bruker, model D8ADVANCE, Berlin, Germany) with Cu Kα radiation (=0.15406 nm). Fourier transform infrared spectra (FT-IR, Bruker Optic VERTEX 70, Germany) were collected with wavelengths of 400–4000 cm−1. X-ray photoelectron spectroscopy (XPS, Thermo Fisher Scientific, ESCALAB 250, Waltham, MA, USA) analyses of precipitates were carried out in an ultrahigh vacuum chamber. Solid 11B-nuclear magnetic resonance (11B-NMR, JEOL JNM ECZ600R, JEOL Ltd., Akishima, Japan) spectra of the precipitates which resulted from removing P and B with COS were acquired using 4 nm probes and a single pulse method. The resonance frequency for 11B was 192.56 MHz at a field strength of 600 MHz. Typical acquisition parameters were pulse length 0.1 ms and relaxation delay 2 s.
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2

Comprehensive Compound Characterization

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The prepared compounds were
characterized using 1H NMR and 13C NMR spectroscopy.
The purity of all
prepared compounds was >95% as determined using elemental analysis
(fluorine-free compounds) or HPLC–HRMS experiments (fluorine-containing
compounds and oily compounds). All chemicals used in the syntheses
were obtained from Sigma-Aldrich (Schnelldorf, Germany) and PENTA
s.r.o. (Prague, Czech Republic) and were used as received. TLC separations
were performed on Merck aluminum plates with silica gel 60 F254. Merck Kieselgel 60 (0.040–0.063 mm) was used for column
chromatography. Melting points were recorded with a Büchi B-545
apparatus (BUCHI Labortechnik AG, Flawil, Switzerland) and are uncorrected. 1H and 13C NMR spectra were recorded using Varian
Mercury Vx BB 300, VNMR S500 NMR (Varian, Palo Alto, CA, USA) or Jeol
JNM-ECZ600R (JEOL Ltd., Akishima, Tokyo, Japan) spectrometers. Chemical
shifts are reported as δ values in parts per million (ppm) and
were indirectly referenced to tetramethylsilane (TMS) via the solvent
signal. Elemental analyses were performed on an Automatic Microanalyzer
EA1110CE (Fisons Instruments S.p.A., Milano, Italy). HPLC–HRMS
(ESI) experiments were performed using an HRMS system Acquity UPLC
I-class and a Synapt G2Si Q-TOF mass spectrometer (Waters, Milford,
MA, USA).
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3

Degree of Functionalization in GelMA Hydrogels

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The degree of functionality (DoF) of GelMA was evaluated using 1H NMR spectroscopy according to the previous studies.34 (link),35 (link)1H NMR spectra were collected using a 600 MHz Fourier
transform-NMR spectrometer (JNM-ECZ600R, JEOL, Japan) installed in
the Center for University-Wide Research Facilities (CURF) at Jeonbuk
National University. Fifty milligrams of gelatin and GelMA were dissolved
in 1 mL deuterium oxide (D2O) before the measurement, respectively.
The DoF was investigated by calculating the percentage of ε-amino
groups in gelatin that was modified in GelMA by reaction with MA using
the following equation:36 (link)
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4

Purification and Characterization of Organic Compounds

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All solvents were treated using standard techniques before use. All reagents and catalysts were purchased from Sigma-Aldrich Co. LLC or Fluorochem Ltd. and were used without additional purification. Analytical thin-layer chromatography (TLC) was carried out using plates coated with silica gel 60 with a fluorescent indicator F254 (Merck, Prague Czech Republic). TLC plates were visualized by exposure to ultraviolet light (254 and 366 nm). The NMR spectra were obtained in CDCl3 at ambient temperature on a VNMR S500 (Varian) spectrometer operating at 500 MHz for 1H and 126 MHz for 13C and on a JNM-ECZ600R (Jeol) instrument operating at 600 MHz for 1H and 151 MHz for 13C. Chemical shifts were recorded as δ values in parts per million (ppm) and were indirectly referenced to tetramethylsilane (TMS) via the residual solvent signal of chloroform-d1 (CDCl3 – 7.26 (H), 77.0 (C) ppm). Coupling constants (J) are given in Hz. ESI-HRMS data were obtained with a Waters Synapt G2-Si hybrid mass analyzer of quadrupole-time-of-flight (Q-TOF) type, coupled to a Waters Acquity I-Class UHPLC system. Chromatographic analysis data were obtained with a Waters HPLC-PDA-MS system (Waters Corporation, Milford, Massachusetts, USA). Analysis confirmed the purity of all the compounds >95% (PDA detection, UV-vis, uncalibrated).
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5

Multimodal Characterization of Nanomaterials

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A JEOL 2200FS HRTEM operated at 200 kV, was used to obtain the STEM images. A Cary 50 UV-Vis Spectrophotometer from Agilent Technologies and a JASCO J-815 CD spectropolarimeter were used for UV-Vis spectrum and CD spectrum characterizations, respectively. The XRD data were measured with a Bruker D8 with IµS-XR Source. The zeta potential and titration were conducted with a Malvern Zetasizer Nano ZSP equipped with an Autotitrator. FTIR spectra were measured with a Cary 630 FTIR Spectrometer from Agilent. XPS data were measured by ESCALAB Xi+ X-ray Photoelectron Spectrometer from ThermoFisher Scientific. Solid-state NMR spectra were recorded by a JNM-ECZ600R from JEOL.
UV-titration was conducted by coupling the titration experiments with an Ocean optics USB2000 fiber optic spectrometer. Titration experiments were performed using a commercial, computer-controlled system from Metrohm (Filderstadt, Germany), operated with the custom-designed software Tiamo (v2.2). The setup consists of a titration device (Titrando 809) that regulates two dosing units (Dosino 807) capable of dispensing titrant solution in steps as small as 0.2 µL.
CD titration was conducted by manual addition of concentrated KOH solutions into the cuvettes followed by the measurement of the CD spectrum. The pH was recorded by a Mettler Toledo pH meter. All the pH electrodes were calibrated before use.
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6

Comprehensive Characterization of COF Nanoparticles

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X-ray diffraction (XRD, Bruker D8Focus, Bremen, Germany) was utilized to analyze the physical topology crystallization of COF nanoparticles. The chemical composition of COF nanoparticles was characterized by Fourier transform infrared (FTIR, Bruker Tensor II, Bremen, Germany). The thermal stability of SPEEK and SPEEK/COF membranes were evaluated through thermal gravimetric analysis under the nitrogen atmosphere in the range of 40 °C to 800 °C (TGA, TA Q5000, New Castle, DE, USA) (Figure S1). The scanning electron microscope (SEM, HITACHI SU8010, Tokyo, Japan) and transmission electron microscopy (TEM, FEI F20, Oregon, USA) were utilized to characterize the COF feature and the cross-section morphologies of as-prepared membranes. Solid-state nuclear magnetic resonance (13C SSNMR, JEOL JNM-ECZ600R, Japan) was used to characterize the structure of COF. The mechanical properties of the composite membranes were measured on a universal material testing machine (KQL, WDL-10, Yangzhou, China) at a strain rate of 10 mm/min.
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7

Comprehensive Characterization of Quantum Materials

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Absolute quantum yields, prompt and delayed PL spectra and phosphorescence decay curves were measured on an Edinburg FLS1000 fluorescence spectrophotometer (Edinburgh Instruments, UK). X-ray diffraction (XRD) analyses were carried out on Bruker AXS D8 X-ray diffractometer (Germany) using a Cu Kα X-ray source (40 kV, 100 mA). Field emission scanning electron microscopy (SEM) was operated on a Hitachi S-4800 microscope. Fourier transform infrared spectra (FTIR) were collected on a Nicolet 380 FTIR spectrometer. Raman spectroscopic studies were carried out on a LabRAM HR Evolution spectrometer with a 785 nm laser as the excitation source. X-ray photoelectron spectroscopy (XPS) data were recorded by using an X-ray photoelectron spectrometer (K-Alpha +) with an Al Kα X-ray source. The binding energy was calibrated by the C1s peak at 284.8 eV as the reference. High-resolution mass spectra (HRMS) were recorded on a Bruker Daltonics microTOF-QII instrument. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) analyses were performed on a Simultaneous Thermal Analyzer (STA) 8000 with a heating rate of 5 °C·min-1. The 1H NMR of the sample were analyzed with JEOL JNM ECZ600R at room temperature.
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8

NMR and Mass Spectrometric Characterization of Organic Compounds

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All solvents were treated by using standard techniques before use. All reagents and catalysts were purchased from commercial sources (Sigma Aldrich, Prague, Czech Republic) and used without purification. The NMR spectra were obtained in CDCl3 at ambient temperature on a VNMR S500 (Varian) spectrometer operating at 500 MHz for 1H and 125.7 MHz for 13C and on a JNM-ECZ600R (Jeol) instrument operating at 600 MHz for 1H and 151 MHz for 13C. Chemical shifts were recorded as δ values in parts per million (ppm) and were indirectly referenced to tetramethylsilane (TMS) via the solvent signal (CDCl3–7.26 ppm for 1H and 77.0 ppm for 13C). Coupling constants (J) are given in Hz. ESI-HRMS were obtained with a Waters Synapt G2-Si hybrid mass analyzer of a quadrupole-time-of-flight (Q-TOF) type, coupled to a Waters Acquity I-Class UHPLC system. TLC was carried out on Merck precoated silica gel 60 F254 plates. Compounds on the plate were observed under UV light (254 and 366 nm) and visualized by spraying with Dragendorff’s reagent.
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9

High-Resolution Solid-State NMR Spectroscopy

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All NMR experiments were recorded at ambient temperature on either 600 MHz (JNM-ECZ600R, JEOL RESONANCE Inc., Tokyo, Japan) or 700 MHz (JNM-ECZ700R, JEOL RESONANCE Inc., Tokyo, Japan) spectrometers equipped with 1.0 mm 1H/X double-resonance ultrafast MAS probes. The sample was packed into a 1.0 mm zirconia rotor. The following three experiments were performed at the 700 MHz spectrometer at νR of 70 kHz and the recycling delay (RD) of 10.0 s, unless otherwise stated. The SERP experiment was performed at the 600 MHz spectrometer at νR of 68.03 kHz and the RD of 8.5 s.
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10

Characterization of Avermectin-Loaded Nanospheres

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The hydrodynamic diameter (Dp) and polydispersity index (PDI) of Av-NDs were measured in triplicate by dynamic light scattering (DLS) using a Horiba SZ-100-Z Nano Particle Analyzer (HORIBA Instruments Co., Ltd, Japan) at 25 °C. The sample was diluted with deionized water to a solid content of about 0.1 wt%.
Identification of the chemical structure in Av-NDs was qualitatively determined via UV–Vis absorption spectrum (Shimadzu UV–Vis spectrophotometer, UV-2600, Shimadzu Instrument (Suzhou) Co. LTD) under the maximum absorption wavelength (λmax) of 245 nm, fourier transform infrared spectrum (Nicolet IS-10, Thermo Scientific; using the technical avermectin and the Av-NDs nanosphere powder in KBr) and 1H NMR (JNM-ECZ600R, JEOL Co. LTD, Japan; D2O was used as solvent).
The morphology of the nanospheres was verified by scanning electron microscope (SEM, Hitachi s-3400 N, Japan) operating at 15 kV using samples prepared by dropping on cleaned tinfoil, dried naturally. Morphology of the dried nanospheres was observed by transmission electron microscope (TEM, JEM-1200EX, JEOL Co. LTD, Japan) operating with 100 kV accelerating voltage, and the samples were prepared by mounting and drying the diluted Av-NDs on the carbon-coated copper grid at room temperature.
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