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7 protocols using ac 400 nmr spectrometer

1

Spectroscopic Characterization of Chemical Compounds

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All chemicals used for synthesis were of laboratory grade. The NMR spectra was taken by using a Bruker AC-400 NMR spectrometer and TMS as an internal standard. FTIR spectra were recorded using a Schmadzu FTIR spectrophotometer. The melting point was assessed by open capillary method and were uncorrected. TLC analysis was performed on pre-coated silica plates (Merck).
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2

Characterization of Synthesized Polymers

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The composition of synthesized polymers was determined by 1H and 31P NMR. Spectra were recorded on a Bruker AC-400 NMR spectrometer (Karlsruhe, Germany) at 25 °C using THF and DMSO-d6 as solvents.
Molecular weight (Mn) and dispersity (Đ) were established using size exclusion chromatography (SEC) (Shimadzu LC-20 Prominence, Kyoto, Japan) equipped with refractometric detector (RID 10-A).
The hydrodynamic diameter and zeta potential of prepared nanoobjects were measured on a ZetasizerNano-ZS (Malvern, UK) at a scattering angle of 173° at 25 °C. The content of rhodamine 6G was determined by UV–Vis spectroscopy using a UV-1800 (Shimadzu, Kyoto, Japan) spectrometer at 527 nm.
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3

Spectroscopic Characterization of Organic Compounds

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Infrared spectra were obtained using a schimadzu FT-IR 8201 PC, spectrophotometer (Kyoto, Japan). 1H and 13C neuclear magnetic resonance (NMR) spectra were obtained using a Bruker AC 400 NMR spectrometer (Billerica, MA, USA) at 400 and 100 MHz, respectively. All 1H and 13C nuclear magnetic resonance (NMR) spectral results are recorded as chemical shifts (d) relative to the internal transcranial magnetic stimulation (TMS). Microanalysis was performed by Chemical and Micro-Analytical Services (CMAS), (Highton, VIC, Australia). Melting point determinations were carried out using a Stuart Scientific (SMP3) melting point apparatus (Staffordshire, UK) and all melting points are uncorrected. Reaction courses and product mixtures were routinely monitored by thin-layer chromatography (TLC) on silica gel pre-coated F254 Merck plates (Darmstadt, Germany).
Starting Materials:
The starting reagents, methyl 2-aminobenzoate, picolinoyl chloride, cesium carbonate, triethylamine, dimethylformamide (DMF), acetonitrile, substituted benzylamine, substituted sulphonamide, potassium tert-butoxide, hydrazine hydrate and substituted aryl aldehyde were purchased from Sigma-Aldrich (St. Louis, MO, USA) and were used as received.
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4

Spectroscopic Characterization of Compound

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The 1H and 13C APT NMR spectra in DMSO-d6 were recorded with a Bruker AC-400 NMR spectrometer. The IR spectrum was recorded in the KBr pellet with a PerkinElmer Spectrum One FT-IR system. The melting point was determined using the Gallenkamp melting point apparatus. Microanalysis was performed using a LECO 932 CHNS-O elemental analyzer.
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5

Characterization of AuNC Nanoparticles

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High-resolution transmission electron microscopy (HRTEM) measurements were recorded on a JEOL 2010 transmission electron microscope (Tokyo, Japan) operating at an accelerating voltage of 200 kV. Proton nuclear magnetic resonance (1H NMR) spectra were performed on a Bruker AC 400 NMR spectrometer (Rheinstetten, Karlsruhe, Germany) in concentrated D2O solutions. At the same time, the fractions were investigated by a matrix-assisted laser desorption ionization time-of-flight mass spectrometer (MALDI-TOF MS) (Autoflex, Bruker, Germany). X-ray photoelectron spectroscopy (XPS) measurements were conducted with a Leybold Heraeus SKL-12 X-ray photoelectron spectrometer (Shenyang, China) modified with a VG CLAM 4 multichannel hemispherical analyzer using a Mg Kα excitation source at 1253.6 eV (10 kV, 20 mA). Thermogravimetric analysis (TGA) measurements were conducted with a Perkin-Elmer TGA 6 thermogravimetric analyzer (Waltham, MA, USA). In addition, the UV–vis absorption spectra of the crude AuNC product and the AuNC fractions were recorded on a Cary 100 Scan UV–vis spectrophotometer (Varian, Palo Alto, CA, USA). The PL properties of the samples were acquired on a QM4 spectrofluorometer (Photon Technology International, Lawrenceville, NJ, USA).
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6

Characterization of Metal Complexes

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Elemental analyses (C, H, N)
were performed with a PerkinElmer 2400 CHNS/O Series II elemental
analyzer. Analyses of copper contents in the complexes was performed
by an iodometric titration method (using Na2S2O3) in aqueous solution, after digesting their crystalline
powder samples in a concentrated HCl/HNO3 mixture. NMR
spectra of H3cpdp were obtained with a Bruker AC 400 NMR
spectrometer. Fourier transform infrared (FTIR) spectra were recorded
on a PerkinElmer L120–000A spectrometer. The solution electrical
conductivity and electronic spectra were obtained using a METTLER
TOLEDO Five EASY Plus FEP 30 digital conductivity meter with a solute
concentration of ∼10–3 M and a Shimadzu UV
1800 spectrophotometer, respectively. Magnetic susceptibility studies
of the complexes were determined in the solid state with a home-built
Gouy balance at room temperature using Hg[Co(SCN)4] as
the calibrant. Diamagnetic corrections were made by using Pascal’s
constants. The powder X-ray diffraction (PXRD) spectra were obtained
using a Rigaku (Mini Flex II, Japan) X-ray diffractometer having Cu
Kα = 1.54059 Å radiation with a Bragg angular range of
2θ (5° < 2θ < 50°). Thermal studies were
executed with a PerkinElmer Diamond TG/DTA thermal analyzer with a
heating rate of 10 °C/min.
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7

Spectroscopic Analysis of Samples

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FT-IR spectra were obtained
using a PerkinElmer System 2000 FT-IR spectrometer. A PerkinElmer
TGA 7 thermogravimetric analyzer was applied. A PerkinElmer 2400 Series
II analyzer was used to determine the percentage of N in the samples.
A Bruker AC-400 NMR spectrometer was used to record the 1H and 13C NMR spectra. Deuterated dimethyl sulfoxide (d6-DMSO) was used as the solvent.
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