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16 protocols using emx 10 12

1

X-band ESR Spectra Acquisition

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The room temperature X-band ESR spectra were obtained by using a ESR spectrometer of Bruker EMX 10/12 with the center field of 3480G. The low temperature X-band ESR spectra were obtained by using a liquid He cooled spectrometer of Bruker EMX 10/12+ with the center field of 3360G.
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2

EPR Spectral Analysis at 120K

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The EPR spectra were
recorded at 120 K
and 31.81 mW microwave power with a field modulation amplitude of
5 G. The spectrometer was Bruker EMX-10/12 (Bruker BioSpin GmbH, Karlsruhe,
Germany) operating in the X-band and equipped with a ER4119HS cavity
and temperature control. The spectral simulations were made using
the Bruker WinEPR Simfonia package.
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3

Synthesis and Characterization of TPB Derivatives

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All experiments were carried out under a nitrogen atmosphere using standard Schlenk techniques and a glove box. 1,2,4,5-tetrakis(isopropyl-thio)benzene (TPB) and NOSbF6 (Alfa Aesar) were purchased and used upon arrival. 1,2,4,5-tetrakis(ethylthio)benzene (TEB) were prepared according to literatures25 . Solvents were dried prior to use. EPR spectra were obtained using Bruker EMX-10/12 at room temperature. UV-Vis spectra were recorded on Lambda 35 spectrometers. Element analyses were performed on Elementar Vario EL III at Shanghai Institute of Organic Chemistry, the Chinese Academy of Sciences. X-ray crystal structures were obtained by Bruker APEX-II CCD and PHOTON100 CMOS detectors. Single crystals were coated with Paratone-N oil and mounted using a glass fiber. Crystal data and structure refinement details are listed in the supporting information (Table 1, SI). For conductivity measurements, single-crystal samples were affixed on glass carriers and silver paste was used to connect samples and electrodes along the crystallogarphic axises. I-V curves were measured by using a computer-controlled Keithley 2400 source meter.
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4

Characterization of Purified P. marneffei Pigment

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The solubility of purified P. marneffei pigment from FRR2161 and GXMU110608 strains and synthetic DOPA-melanin (2 mg) were tested with distilled water, hot 1.0 M NaOH solution and common organic solvents (methanol, absolute ethanol, propanol, acetone, acetonitrile, iso-amyl alcohol, and chloroform). Reactions with oxidizing agents such as 30% hydrogen peroxide (H2O2) were determined. Purified P. marneffei melanin was subjected to various analyses such as UV-visible absorption (Varian Cary50), Fourier transform infrared (FT-IR) spectra (Perkin Elmer Spectrum100) and electron-paramagnetic resonance (EPR) (Bruker EMX-10/12). The UV absorption was performed using 40 μg/ml P. marneffei melanin dissolved in sodium hydroxide scanning at approximately 200–800 nm wavelength. The dried 2 mg P. marneffei melanin was mixed with 200 mg potassium bromide by grinding in an agate mortar for 5 min, and the sample was examined by infrared spectral scanning at approximately 4000–400 cm-1. The various instrumental parameters of EPR were set at 100 kHZ modulation frequency, 1.0 G modulation amplitude, 5.0 mW microwave power, 9.75 GHZ microwave frequency, 3475.0 G center magnetic field strength, 100.0 G scan width and 83.89 s scan time.
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5

Comprehensive Spectroscopic Characterization of Compounds

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Elemental analyses for C, H, N, and S were performed on Perkin-Elmer 240C analyzer. FT-IR data were recorded on Vector27 Bruker Spectrophotometer with KBr pellets in the 4000–400 cm−1 region. TGA data were obtained on an STA 449C thermal analysis system with a heating rate of 10 °C min−1 under N2 atmosphere. The PXRD were collected with a scan speed of 0.1 s deg−1 on a Bruker Advance D8 (40 kV, 40 mA) diffractometer with Cu radiation (λ = 1.54056 Å) at room temperature. Calculated PXRD patterns were generated using Mercury 3.0. Magnetic susceptibility measurements were performed using a Quantum Design SQUID VSM magnetometer on microcrystalline samples for all compounds. EPR spectra were obtained by using a Bruker EMX-10/12 variable-temperature apparatus at 110 K. Gas sorption measurements were conducted using a Micrometritics ASAP 2020 system. See Supplementary Methods for details.
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6

In Situ EPR Analysis of CO2 Photocatalyst

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The in situ EPR experimental data were obtained over a commercial EPR spectrometer Bruker EMX-10/12 at a X-band (9 GHz). Samples were prepared by mixing the catalyst in a glass tube with 0.5 mL solution of CH3CN/TEOA (20:1). The sample was degassed by N2 and then sealed. Then the glass tube was fixed into the EPR resonator. When needed, the CO2 were introduced into the sample. The experiments were performed under visible-light irradiation.
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7

Characterization of B-nZVI/BC Composite

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The crystalline phase pattern of B-nZVI/BC was analyzed with X-ray diffraction using Cu Kα radiation (XRD, X’TRA, Geneva, Swiss). The surface morphology and the elemental composition of the composite were measured by scanning electron microscopy (SEM, Hitachi S-4800, Tokyo, Japan) and transmission electron microscopy (TEM, FEI Tecnai G2 spirit, Eindhoven, Holland) equipped with energy dispersive spectroscopy (EDS, Bruker, QUANTAX 400, Saarland, Germany). The Brunauer-Emmett-Teller specific surface areas (SABET) of B-nZVI/BC were observed using the N2 adsorption method (Micromeritics, ASAP 2020 M + C, Norcross, GA, USA). The surface compositions and the valence states of the composites were determined by X-ray photoelectron spectroscopy (XPS, Shimadzu, AXIS UltraDL, Kyoto, Japan). Reactive free radicals were recorded through an electron paramagnetic resonance (EPR) spectrometer (Bruker, EMX-10/12, Saarland, Germany).
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8

Photocatalytic RhB Degradation by NF/ZIF-67

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The activation of PMS using NF/ZIF-67 was evaluated by batch-type experiments of RhB dye degradation. In a typical experiment, a piece of NF/ZIF-67 (3 cm × 3 cm) was added into a beaker containing RhB solution (200 mL, 100 mg L−1). NaOH (0.1 M) and HCl (0.1 M) were used to adjust the initial pH value. The solution was stirred for 30 min to adsorb saturated RhB on NF/ZIF-67. Then, a certain dosage of PMS was immediately mixed into the RhB solution, which was stirred continually and maintained at a pre-set temperature (25 °C). Sample aliquots of 1 mL were withdrawn from the solution at regular intervals. Then, 1 mL methanol was immediately mixed into the sample to quench the residual radicals. The residual RhB concentration was determined with a UV-Vis spectrophotometer (Alpha-1500, Shanghai, China) at a maximum wavelength of 554 nm. 5,5-Dimethyl-1-pyrroline N-oxide (DMPO, >99 wt%) was utilized to capture the generated hydroxyl and sulfate radicals, which were then detected by electron spin resonance (EMX-10/12, Bruker, Germany). The cobalt ions released in the solution were detected by atomic absorption spectroscopy (AAS, PinAAcle900T, PerkinElmer, US).
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9

Comprehensive Characterization of Nano-Enabled Materials

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X-ray diffraction (XRD) patterns were characterized using an X-ray powder diffractometer (Rigaku, SmartLab SE). UV-vis spectra were determined via UV-vis spectrophotometer (Shimadzu, UV-1750). Transmission electron microscopy (TEM) images were obtained by JEM-1400 (Jeol) at 100 kV. Elemental analysis was carried out by F200s (Talos). Scanning electron microscopy (SEM) images were obtained by SU-70 (Hitachi) at 5 kV. Hydrodynamic diameter and zeta potential were measured by dynamic light scattering (DLS) using the Malvern ZEN 3600. The release of Zn2+ ions was detected via an inductively coupled plasma optical emission spectrometer (ICP-OES, OPTIMA 2 × 00/5000). Thermal weight loss was evaluated by a simultaneous thermal analyzer (NETZSCH, STA 449F5). Reactive oxygen species were determined by electron spin resonance spectrometer (Bruker, EMX-10/12). Fluorescence images were observed and recorded by Leica DM 6000 B. Bacterial counting and Area calculating are obtained by NIH ImageJ Software. Agar blocks were cut into ultra-thin slices by Ultra-thin microtome (Leica Microsystems, Leica UC7).
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10

Magnetic Susceptibility of Crystalline Solids

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The temperature-dependent molar magnetic susceptibility of crystalline solid samples was measured on a Quantum Design SQUID-VSM magnetometer with an applied field of 5000 G or 2000 G. The magnetic susceptibility data were corrected for the diamagnetic contribution of the capsule and the sample holder. Molar susceptibility data were corrected for diamagnetic contribution of Pascal’s constants53 (link), The ESR measurements were obtained with a Bruker EMX-10/12 and EPR-plus X-band (9.4 GHz) digital EPR spectrometer with Bruker N2-temperature controller. Spectral analysis and simulations were performed using the EasySpin program.
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