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5 protocols using unity 300 mhz spectrometer

1

Characterization of Polymeric Micelles

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1H NMR spectra were obtained using a Varian Unity 300 MHz spectrometer. Either chloroform-d1 or methanol-d4 was used as a solvent, depending on polymer solubility. Fourier transform infrared spectroscopy (FTIR) spectral studies were performed using a Nicolet/Nexus 670 FTIR spectrometer in a range between 4,000 cm−1 and 500 cm−1 with a resolution of 2 cm−1. All powder samples were compressed into KBr pellets prior to FTIR measurements. The Mws and Mw distribution of the polymers were estimated using a gel permeation chromatography (GPC) system consisting of a styroldivinylbenzole-copolymer linear column (Polymer Standard Service, Mainz, Germany) with dichloromethane as an eluent (1 mL/min); polystyrene was used as a standard for calibration. Samples for scanning electron microscopy (SEM, Quanta 400F) analysis were prepared by drying a dispersion of the micelle solution on a clean glass slide, which was first washed with deionized water and then with acetone for 24 hours in a desiccator. A thin layer of gold was sputter coated on the samples for charge dissipation during SEM imaging.
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2

Characterization of PEG-PLL Nanoparticles

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1H NMR spectra were recorded on a Varian Unity 300 MHz spectrometer by using dimethyl sulfoxide-d6 (DMSO-d6) or D2O as the solvent. The molecular weight and polydispersity index (PDI) of PEG-PLL were evaluated by gel permeation chromatographic (GPC) system consisting of Waters 2690D separations module and Waters 2410 refractive index detector. Tetrahydrofuran (THF) was used as the eluent at a flow rate of 0.3 mL/min. The particle size and zeta potential were measured using Malvern Zetasizer Nano-ZS ZEN3600. Nitrogen adsorption−desorption isotherms were measured on a micromeritics instrument (ASAP2020). Thermal gravitational analysis (TGA) was performed with a Thermo Gravimetric Analyzer (TGS--II, Perkin-Elmer). Fluorescence analysis was performed on a RF-530/PC spectrofluorophotometer (Shimadzu). The morphologies of nanoparticles were observed on scanning electron microscopy (SEM, FEI-QUANTA 200) and transmission electron microscopy (TEM, JEM-2100).
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Synthesis and Characterization of Organophosphorus Compounds

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All reagents were commercially available and used as supplied without further purification. Deuterated solvents were purchased from Cambridge Isotope Laboratory (Andover, MA). Compounds 1,12b (link)4,17 (link) and 517 (link) were prepared according to the published procedures. NMR spectra were recorded on a Varian Unity 300 MHz spectrometer. 1H and 13C NMR chemical shifts are reported relative to residual solvent signals, and 31P{1H} NMR chemical shifts are referenced to an external unlocked sample of 85% H3PO4 (δ 0.0). The UV–vis experiments were conducted on a Hitachi U-4100 absorption spectrophotometer. Mass spectra were recorded on a Micromass Quattro II triple-quadrupole mass spectrometer using electrospray ionization with a MassLynx software suite. The melting points were collected on a SHPSIC WRS-2 automatic melting point apparatus.
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Synthesis and Characterization of Luminescent Platinum Complexes

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All reagents were commercially available and used as supplied without further purification. 4-bromo-N,N-bis(p-(pyrid-4-yl)phenyl)aniline58 (link) and diplatinum acceptor Pt-1 and Pt-2 were prepared according to the reported procedures.29 (link) 1H NMR and 13C NMR spectra were recorded in the designated solvents on a Varian Inova 500 or 400 MHz spectrometer. 31P{1H} NMR spectra were recorded on a Varian Unity 300 MHz spectrometer, using an external unlocked sample of 85% H3PO4 (δ = 0) as reference. Mass spectra were recorded on a Micromass Quattro II triple-quadrupole mass spectrometer using electrospray ionization with a MassLynx operating system. Absorption and fluorescence spectra were recorded on a Hitachi U-4100 and Hitachi F-7000 Spectrophotometer, equipped with 1 cm quartz cuvette from Starna Cells, Inc. The temperature-dependent fluorescent experiments were conducted on a Hitachi F-3000 fluorescence spectrophotometer. The luminescence lifetime was obtained on Quantaurus-Tau Fluorescence lifetime spectrometer C11367 from Hamamatsu Photonics.
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5

Spectroscopic Characterization of Novel Compounds

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All reagents were commercially available and used as supplied without further purification (I assume that they are still available). 1H NMR and 13C NMR spectra were recorded on a Varian Inova 500 MHz spectrometer. 31P{1H} NMR spectra were measured on a Varian Unity 300 MHz spectrometer, using an external unlocked sample of 85% H3PO4 (δ = 0) as reference. ESI-TOF-MS were recorded on a Waters Synapt G2 mass spectrometer. Absorption and fluorescence spectra were recorded on a Hitachi U-4100 and Hitachi F-7000 Spectrophotometer, equipped with 1 cm quartz cuvettes from Starna Cells, Inc. DFT and TDDFT calculations were carried out using the B3LYP exchange correlation function and implemented in the Gaussian 09 package.62
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