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17 protocols using ifs 66

1

Comprehensive Characterization of Synthesized Graphene Oxide

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A UV-Visible spectrometer (Bruker, Billerica, MA, USA), FTIR spectrometer (Bruker IFS 66, Billerica, MA, USA), XRD using Ni-filters Cu Kα radiation (ν = 1.54 Å) at 40 kV and 40 mA (BrukerMeasSrV D2 Phaser, Billerica, MA, USA), Raman spectroscopy (Oxford Instruments, WITec alpha 300 R, Concord, MA, USA), SEM (JEOL, JSM-7610F, Tokyo, Japan), TEM (FEI TECNAI G2 F20, OR, USA) and EDS (Oxford Instruments, INCA-xart, Concord, MA, USA) were employed to characterize the optical properties, morphology, size, structure and composition of the synthesized GO.
A Bruker Lambda 35 UV–Vis absorption spectrometer was used in the range of 200–800 nm with steps of 0.5 nm at room temperature. FTIR spectra with a wave number 400–4000 cm−1 were developed using a Bruker IFS 66. The diffraction data of the finely powdered samples were recorded for 2θ angles between 5 and 80°. The Raman spectrum was recorded between 400 and 4000 cm−1 on an INCA-xart Raman spectrometer using a 514.5 nm Ar laser at 0.5 mW power. Images were obtained at magnifications ranging from 45× to 30,000×. TEM measurements were carried out in an TECNAI G2 series transmission electron microscope operating at 200 kV.
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2

Matrix Isolation of Cyanogen Azide

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The standard infrared and Raman spectra were measured using Bruker IFS 66 FT-IR and Nicolet Magna 860 FT-Raman spectrometers in the solid state with a 2 cm−1 resolution, respectively. The In–Ga–Ar laser line at 1064 nm was employed for the Raman excitation measurements. To obtain matrices containing CNK, the crystalline sample was allowed to sublimate from a small electric oven located inside the vacuum vessel of the cryostat. The CNK vapours, mixed with a large excess of matrix gas (argon), were deposited onto a CsI window kept at 15 K in a closed cycle helium cryostat (APD-Cryogenics). The sample temperature was maintained with a temperature controller (Scientific Instruments 9700) equipped with a silicone diode and a resistive heater. Infrared spectra were recorded at 11 K between 4000 and 50 cm−1 with a resolution of 0.5 cm−1 by means of a Fourier transform IR spectrometer (Bruker IFS 66) equipped with a liquid N2 cooled MCT detector.
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3

Characterization of Organic Compounds

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All the commercially obtained chemicals were used as received, without further purification. The solvents were dried and distilled using conventional methods. For the melting point studies, Heiztisch Mikroskop–Polytherm A (Wagner & Munz, München, Germany) was used. The 1H, 13C{1H} NMR spectra were recorded on an Agilent 400-MR DDR2 and JEOL-ECZL400G (1H: 400 MHz, 13C: 100 MHz). The chemical shifts (δ) are reported in parts per million (ppm) and were referenced to the residual peaks of the solvent or TMS as an internal standard; the coupling constants (J) are expressed in Hz. All the NMR data were processed and displayed using MestReNova software. The IR spectra were measured on an FT–IR spectrometers Nicolet 740 or Bruker IFS66 equipped with a heatable Golden Gate Diamond ATR–Unit (SPECAC) in KBr. A total of 100 scans for one spectrum were co-added at a spectral resolution of 4 cm–1. The electrospray ionization mass spectra (ESI-MS) were recorded using an LTQ Orbitrap Velos-hybrid ion-trap-orbitrap (Thermo Scientific, Waltham, MA, USA). The purity of the substances and courses of the reactions were monitored using thin layer chromatography (TLC), using silica gel 60 F254 on aluminum-backed sheets (Merck) and analyzed at 254 nm. The column chromatography was conducted on silica gel 60 with particle sizes of 0.063–0.200 mm (Merck).
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4

Morphological and Textural Characterization

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The morphological characterization of samples was carried out with a scanning electron microscope (SEM, FEI Model QUANTA 200 FEG) equipped with energy dispersive spectroscopy (EDS). The samples were coated with gold prior to analysis. The identification of the chemical elements present in the material was performed by EDS. Fourier transformed infrared (FTIR) spectra in the 4000–400 cm−1 range were recorded for all samples in a BRUKER instrument model IFS 66. The samples were pressed into pellets with KBr. The specific surface area and the porosity were determined for all materials with a Micromeritics ASAP 2420 porosimeter. The isotherms were obtained at 77 K using N2 as an adsorbate. The specific surface area was calculated using the Brunauer-Emmett-Teller (BET) model. Pore size distribution and pore volume were determined from the desorption branch of the isotherms using the Barrett-Joyner-Halenda (BJH)-plot method.
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5

Characterization of Nanoadsorbent Materials

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Be(ii) determination was performed using a FAAS instrument model AA-680 Shimadzu (Japan) consisting an acetylene/nitrous oxide flame and a Be hollow cathode lamp with wavelength of 234.9 nm. Manufacturer's manual was used to set up the instrument. A digital 827 WTW Metrohm pH-meter composed of a combined glass-calomel electrode (Herisau, Switzerland) was employed for the pH measurements. Fourier transform infra-red (FT-IR) analysis carried out on a Bruker spectrophotometer model IFS-66. Elemental analysis of the nanoadsorbent was conducted using an EA112 flash elemental analyzer (Thermo Finnigan, Okehampton, UK). Scanning electron microscopy (SEM) study was performed on a KYKY-3200 instrument (Beijing, China). Magnetic features of the nanoadsorbents were recorded on a vibrating sample magnetometer (VSM) (AGFM/VSM 117 3886 Kashan, Iran). A Bahr STA-503 instrument (Behrthermo, Germany) was used for thermogravimetric analysis (TGA). Surface analysis was explored by nitrogen adsorption–desorption method employing a Micromeritics ASAP 2010 instrument. X-ray diffraction (XRD) analysis was conducted on a Philips-PW 12C diffractometer (Amsterdam, The Netherlands) using Cu Kα radiation.
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6

Synthesis and Characterization of Chiral Vanadium Complexes

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All reagents for synthesis of the complexes, i.e., chiral amino alcohols, salicylaldehyde derivatives, and vanadium(V) oxytripropoxide were purchased from Aldrich company. The other chemicals were obtained from local sources and used without further purification. Carlo Erba MOD 1106 instrument was used to perform elemental analyses. UV-Vis spectra were conducted using a Perkin-Elmer LAMBDA 18 spectrophotometer, and CD spectra were conducted using a Jasco J-815 spectropolarimeter. IR spectra were recorded on Bruker IFS 66 as KBr pellets. Bruker AVANCE III 700 MHz spectrometer was employed for all NMR spectra measurements using TMS as a reference and DMSO-d6 as a solvent. The catalytic reactions progress was monitored on a Shimadzu GC-2025 gas chromatograph with an FID detector, and Zebron ZB-5 capillary column and Shimadzu GCMS-QP2010 SE equipment were used for the confirmation of the identities of all oxidation products. The absorbance of the cells during the MTT assay was measured at 570 nm and 660 nm (reference value) by an ASYS Hitech GmbH microplate reader. Microscopic images were taken at 1 × 4 magnification with an Olympus microscope.
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7

Characterization of Organic Compounds

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All chemicals were purchased from commercial sources and used without further purification. Solvents were dried and distilled using conventional methods. Melting points were measured on Heiztisch Mikroskop—Polytherm A (Wagner & Munz, Germany). NMR spectra were performed on Agilent 400-MR DDR2 (1H: 400 MHz, 13C: 100 MHz). Deuterated solvents used are indicated in each case. Chemical shifts (δ) are expressed in ppm and refer to the residual peak of the solvent or TMS as an internal standard; coupling constants (J) are in Hz. The mass analyses were performed using the ESI technique on a Q–TOF (Micromass) spectrometer. Elemental analyses were carried out on Perkin–Elmer 240, Elementar vario EL (Elementar, Germany) or Mitsubishi TOX–100 instruments. All samples were dried in the desiccator over P2O5 under vacuum (1 Torr) at 80 °C for 8 h. The IR spectra were measured on an FT–IR spectrometer Nicolet 740 or Bruker IFS66 spectrometers equipped with a heated Golden Gate Diamante ATR–Unit (SPECAC) in KBr. A total of 100 Scans for one spectrum were co–added at a spectral resolution of 4 cm−1. The courses of the reactions were monitored using TLC aluminium sheets with Silica gel 60 F254 (Merck). The column chromatography was performed on Silica gel 60 (Merck). HPLC was performed on Büchi Pure 850 FlashPrep chromatography instrument using Prontosil, 150 × 20 mm, 5 μm column.
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8

Specular Reflectance of IPA Adsorption

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The specular reflectance
was measured under controlled pressure of IPA. To control the vapor
pressure in the sample chamber, a container with liquid IPA was connected
to the chamber through a needle valve. The internal pressure of the
chamber was measured with a dual capacitance manometer (MKS model
PDR 2000). Samples were annealed at 200 °C for 1 h to remove
any moisture from the voids in the porous structures before carrying
out the gas adsorption–desorption process. The chamber containing
a sample was kept under dynamic vacuum (10–2 Torr)
for 30 min. In adsorption measurements, IPA gas was injected into
the chamber, and the reflectance spectra were measured at each fixed
pressure, P, by using a FTIR spectrometer (IFS-66,
Bruker). This process was repeated sequentially at different vapor
pressures until saturation pressure (Ps) was reached. Desorption experiments were conducted following the
same protocol, with a gradual decrease in the pressure being obtained
by opening the valve connected to the vacuum pump. Again, spectra
were taken at slowly decreasing pressures until the initial value
was attained. All measurements were made at room temperature (∼20
°C).
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9

Characterization of CP/O300 Nanocomposites

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CHN analysis of CP/O300 nanocomposites was successfully conducted using a Carlo Erba 1106 (Carlo Erba, Milano, Italy) (combustion temperature of 1,030°C, atmosphere of oxygen). TEM images were obtained on a TEM125K (SELMI, Ukraine) microscope working at 100 kV. Amorphous carbon film which covered the copper grid was used as a carrier for samples. UV–vis spectra were measured on double beam spectrophotometer 4802 (UNICO, Fairfield, NJ, USA) with a resolution of 1 nm. Photoluminescence (PL) and Fourier transform infrared spectroscopy (FTIR) spectra were registered using LS55 (PerkinElmer, Waltham, MA, USA) and IFS-66 (Bruker, Karlsruhe, Germany) spectrophotometers. Kinetics of fluorescence decay of the studied materials was measured with the Edinburg Instruments TCSPC Fluorescence Spectrometer F900 (Edinburgh Instruments Ltd., West Lothian, UK) using different lasers for the sample excitation. The fluorescence spectra were corrected for the instrument sensitivity.
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10

Infrared Spectroscopy of Solid Samples

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The IR spectra were recorded on the BRUKER IFS 66 spectrophotometer in a KBr pellet over the 4400–650 cm−1 range.
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