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8 protocols using v 560 spectrometer

1

Green Synthesis of Au-Chitosan Composite

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Fine graphite powder (<50 μm) was received from Sigma-Aldrich, India. Tetrachloroauric (III) acid trihydrate, chitosan, sulfuric acid (AR grade), potassium permanganate, hydrogen peroxide (30%), sodium nitrate, sodium nitrite, sodium fluoride, sodium bromide, sodium thiocyanate, calcium oxalate, disodium phosphate, sodium bicarbonate, sodium sulphate, and succinic acid were obtained from Merck, India. All chemicals were of analytical grade and used as received. The stock solutions were prepared using doubly distilled water and the experiments were performed under ambient conditions.
UV–vis spectral measurements were performed using a Jasco (V-560) spectrometer. The morphological studies of the as-synthesized composite were characterized by FEI Tecnai G2 20 S-TWIN TEM with an accelerating voltage of 200 kV. FEI Tecnai G2 20 S-TWIN TEM attached BRUKER AXS elemental analyzer was used for the EDS and elemental mapping of the composite. XRD analysis was performed using from Panalytical X′ per PRO X-ray diffractometer equipped with Cu Kα radiation (λ = 0.15406 nm). FTIR was performed by a Shimadzu model FT-IR spectrometer.
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2

Spectroscopic Characterization of Biomolecules

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Absorption spectra have been measured on a Shimadzu UV-2600 spectrometer or on a JASCO V-560 spectrometer, to both of which a temperature controller has been attached, using quartz cells with 1 mm or 10 mm path-length. Circular dichroism (CD) spectra have been measured on a JASCO J-720 spectropolarimeter. Electron paramagnetic resonance (EPR) spectrum has been measured on a JEOL JES-RE1X X-band spectrometer at 77 K.
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3

Thin Film Characterization of Azulene-Based Compounds

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Thin films containing four azulene based compounds were obtained by the spin-coating technique on glass substrate using a spin-coater from Laurell Technologies Corporation, model WS-400B-6NPP/LITE. Then, the films were dried for 1 h at 70 °C to evacuate the remaining solvent. Their spectroscopic properties within UV-VIS range were characterized with the JASCO V560 spectrometer. The absorption spectra of the films are shown in Fig. 2. The thin films thicknesses were determined by the profilometry technique using DEKTAK 120 apparatus of KLA Tencor Company. The device allows the thickness measurement of each deposited film on a hard and smooth glass surface. Measurements were done in triplicate, and the values are listed in Table 1.

Absorption spectra of the investigated azulenylpyrydine-azo dyes, 14 in PMMA films.

Fig. 2

Dye concentration, film thickness and maximum absorption wavelength λmax of investigated azulenylpyrydine-azo dyes in PMMA films.

Table 1
CompoundConcentration (w%)Thickness (nm)Absorption maxima (nm)
12394.6433
5327.8430
10357.1431
22255.3432
5280.2433
10292.1433
32252.8474
5272.2476
10287.3476
42310.7485
5621.3486
10903.8487
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4

Analytical Characterization of Compounds

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Reactions were monitored with thin-layer chromatography (TLC) silica gel 60 F₂₅₄ (Merck KGaA, Darmstadt, Germany). Medium-pressure liquid chromatography was performed with a Smart Flash AI-580S instrument (Yamazen Corp., Osaka, Japan) using a silica gel cartridge column. NMR spectra were recorded using an AVANCE Neo 400 NMR spectrometer (Bruker Japan K.K., Kanagawa, Japan). Tetramethylsilane was used as the internal standard in the 1H and 13C NMR spectrometry experiments. BF3·Et2O in toluene-d8 was used as the external standard in the 11B NMR spectroscopy experiments. Mass spectrometry (MS) data were collected using a JMS-700(2) MStation (JEOL Ltd., Tokyo, Japan); elemental analyses were conducted using an MT-6 CHN analyzer (Yanaco Technical Science Corp., Tokyo, Japan); ultraviolet–visible (UV–Vis) absorption spectra were recorded using a V-560 spectrometer (JASCO Corp., Tokyo, Japan); and fluorescence spectra were recorded using an RF-5300PC instrument (Shimadzu Corp., Kyoto, Japan).
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5

Inert Atmosphere Organometallic Spectroscopy

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All reactions and manipulations were performed under nitrogen atmosphere using Schlenk techniques. All solvents used were dried and freshly distilled under nitrogen prior to use, using standard methods. 1H, 13C, and 31P NMR spectra were recorded on a Bruker Avance 400 spectrometer at probe temperature using commercially available deuterated solvents. 1H and 13C chemical shifts (s = singlet; d = duplet; t = triplet; m = multiplet) are reported in parts per million (ppm) downfield from internal standard Me4Si and the 31P NMR spectra are reported in ppm downfield from external standard, 85% H3PO4. Coupling constants are reported in Hz. All assignments were attributed using COSY, HMBC and HMQC NMR techniques. Infrared spectra were recorded on KBr pellets using a Mattson Satellite FT-IR spectrophotometer and only relevant bands were cited in the text. Electronic spectra were obtained at room temperature on a Jasco V-560 spectrometer from solutions of 10−3-10−5 M in quartz cuvettes (1 cm optical path). Elemental analyses were performed at Laboratório de Análises, at Instituto Superior Técnico, using a Fisons Instruments EA1 108 system. Data acquisition, integration and handling were performed using a PC with the software package EAGER-200 (Carlo Erba Instruments).
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6

Synthesis and Characterization of Salt(Cl⁻)

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Salt(Cl) was prepared according to the literature.3 (link) Other reagents were purchased and used without further purification. Solvents were dried, distilled, and stored under N2. Reactions were carried out using standard Schlenk techniques under nitrogen.
IR and NMR spectra were recorded on a JASCO FT/IR-660 PLUS spectrophotometer and JEOL AL-400 and ECX-500 spectrometers, respectively. The IR measurement was conducted using a KBr method. UV-Vis and CD spectra were obtained by a JASCO V-560 spectrometer and a JASCO J-720WS, respectively. Multi angle light scattering (MALS) and GPC measurements were conducted with a SHOKO science DAWN HELEOS II and a TOSO HLC-8220 with polystyrene gel columns (Shodex LF-804) using DMF containing 0.06 M LiBr as an eluent, respectively. Cyclic voltammetry was performed on a DMSO solution containing 0.10 M [Et4N]BF4 with a Hokuto Denko HSV-110. 1 cm × 1 cm and 1 cm × 2 cm Pt plates and Pt wire were used as working, counter, and reference electrodes, respectively.
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7

Schlenk Synthesis and Spectroscopic Characterization

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All reactions and manipulations were performed under nitrogen atmosphere using Schlenk techniques. All solvents used were dried and freshly distilled under nitrogen prior to use, using standard methods [38] . 1 H, 13 C, 19 F and 31 P NMR spectra were recorded on a Bruker Avance 400 spectrometer at probe temperature using commercially available deuterated solvents. 1 H and 13 C chemical shifts (s ¼ singlet; d ¼ duplet; t ¼ triplet; m ¼ multiplet; comp ¼ complex) are reported in parts per million (ppm) downfield from internal standard Me 4 Si. 19 F and 31 P NMR spectra are reported in ppm downfield from external standard CFCl 3 and 85% H 3 PO 4, respectively. Coupling constants are reported in Hz. All assignments were attributed using DEPT-135, COSY, HMBC and HMQCNMR techniques. Infrared spectra were recorded on KBr pellets using a Mattson Satellite FT-IR spectrophotometer. Only considered relevant bands were cited in the text. Electronic spectra were obtained at room temperature on a Jasco V-560 spectrometer from solutions of 10 À4 -10 À6 M in quartz cuvettes (1 cm optical path). Elemental analyses were performed at Laborat orio de An alises, at Instituto Superior T ecnico, using a Fisons Instruments EA1 108 system. Data acquisition, integration and handling were performed using a PC with the software package EAGER-200 (Carlo Erba Instruments).
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8

Caffeic Acid-Cyclodextrin Complexation

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In order to determine the stoichiometry and stability constant (K) of the three ICs, solutions with different concentrations of each CD (between 0 and 6 Â 10 À3 M) were added to the same concentration of caffeic acid (1 Â 10 À5 M), at each pH (buffer H 3 PO 4 /NaOH pH 3 or 5). The solutions were placed in ultrasounds bath during 30 min, and they were maintained 24 h at 25 C and 50 rpm on dark. Samples of each solution were taken (0 and 24 h) for absorbance measurements.
The absorbance of caffeic acid or IC was measured at the caffeic acid l max (217 nm). The caffeic acid concentration was calculated based on the calibration curve, as previously determined. Moreover, the CDs had no influence on the caffeic acid spectra, at the conditions used. The absorption spectra of each solution were recorded on a Jasco V560 spectrometer (Cremella, Italy), using a 1-cm quartz cuvette.
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