FTIR analyses were performed using a Jasco FT-IR 4100 spectrometer (Japan) equipped with an attenuated total reflectance module (ATR, ZnSe crystal). Spectrums were recorded in a range from 4000 to 600 cm -1 as the average of 64 scans with a resolution of 4 cm -1 . The spectra from starch films were normalized with respect to the 1149 cm -1 peak, which is expected to not change with the incorporation of additives. Experiments were carried out in triplicate.
Ft ir 4100 spectrometer
Manufactured by Jasco
Sourced in Japan, United States
The FT/IR-4100 spectrometer is a laboratory instrument used for infrared spectroscopy. It is designed to analyze the absorption and transmission characteristics of a sample by measuring the intensity of infrared light as a function of wavelength or frequency.
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Lab products found in correlation
P 2000 polarimeter, by Jasco (13 mentions)
Sephadex lh 20, by GE Healthcare (6 mentions)
Agilent 1100 dad, by Agilent Technologies (6 mentions)
Avance 3 spectrometer, by Bruker (5 mentions)
Tci microcryoprobe, by Bruker (5 mentions)
Hplc pump l 7100, by Hitachi (4 mentions)
Q exactive plus hybrid quadrupole orbitrap mass spectrometer, by Thermo Fisher Scientific (4 mentions)
Ft ir 410 spectrometer, by Jasco (4 mentions)
Silica gel 60 f254, by Merck Group (4 mentions)
P 1020 polarimeter, by Jasco (4 mentions)
Avance 400, by Bruker (4 mentions)
Sephadex lh 20, by Merck Group (3 mentions)
Silica gel, by Merck Group (3 mentions)
Aviii 500 spectrometer, by Bruker (3 mentions)
Q500 thermogravimetric analyzer, by TA Instruments (3 mentions)
Lcq fleet, by Thermo Fisher Scientific (3 mentions)
Dip 1000 polarimeter, by Jasco (3 mentions)
Gf254, by Qingdao Haiyang Chemical (3 mentions)
P 1010 polarimeter, by Jasco (3 mentions)
Lc esi it tof ms equipment, by Shimadzu (2 mentions)
138 protocols using ft ir 4100 spectrometer
1
FTIR Analysis of Starch Films
2
Spectroscopic Characterization of Analytical Compounds
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All the chemicals and
reagents were of analytical grade and purchased from Sigma-Aldrich
and used without purification. A JASCO FT IR 4100 spectrometer was
used to record the absorption frequencies for the compounds. Bruker
Advance instruments (400 MHz for 1H and 100 MHz for 13C) were used to record the 1H and 13C NMR spectra using DMSO-d6 as solvent.
The reactions were monitored by using silica gel-precoated TLC F254
Merck plates. A Shimadzu UV-240 spectrophotometer and JASCO FP-8200
spectrofluorimeter were used to record absorption and fluorescence
spectra of the compounds using standard quartz cuvettes of 1 cm in
path length. The recorded excitation and emission slit width was 5.0
nm at 24 ± 1 °C
temperature. A PerkinElmer 2400 series II Elemental CHNS analyzer
was used to perform the elemental analysis. Mass spectra of the compounds
were obtained on an HR mass spectrometer.
reagents were of analytical grade and purchased from Sigma-Aldrich
and used without purification. A JASCO FT IR 4100 spectrometer was
used to record the absorption frequencies for the compounds. Bruker
Advance instruments (400 MHz for 1H and 100 MHz for 13C) were used to record the 1H and 13C NMR spectra using DMSO-d6 as solvent.
The reactions were monitored by using silica gel-precoated TLC F254
Merck plates. A Shimadzu UV-240 spectrophotometer and JASCO FP-8200
spectrofluorimeter were used to record absorption and fluorescence
spectra of the compounds using standard quartz cuvettes of 1 cm in
path length. The recorded excitation and emission slit width was 5.0
nm at 24 ± 1 °C
temperature. A PerkinElmer 2400 series II Elemental CHNS analyzer
was used to perform the elemental analysis. Mass spectra of the compounds
were obtained on an HR mass spectrometer.
3
Fourier Transform Infrared Spectroscopy of Glass System
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Fourier transform infrared spectroscopy (FT-IR) was performed in order to identify the correlation between absorption wavelengths and the chemical structure of the samples. The analysis was performed on powder samples for xCuO (100 − x)(CaF2∙3P2O5∙CaO) glass system with 0 ≤ x ≤ 16 mol%). In this regard, 0.005 g of vitreous oxide powders were homogenized with 0.2 g of potassium bromide (KBr), which were subsequently pressed in the form of pellets with a Manual Hydraulic Press (Specac Ltd, Orpington, UK) for 3 min/10 tons. The spectra were recorded using the Jasco FT-IR 4100 spectrometer with a spectral resolution of 4 cm−1, in the range of 350–4000 cm−1 wave numbers, with 256 scans/sample.
4
Synthesis and Characterization of Quinoline-2-carbohydrazide Derivatives
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1 H NMR spectra were recorded using a JEOL AL-400 or a JEOL ECA-500 spectrometer. Chemical shifts are reported in δ (ppm) relative to Me4Si as an internal standard. 13 C NMR spectra were recorded using a JEOL AL-400 or a JEOL ECA-500 and referenced to the residual solvent signal. Exact mass (HRMS) spectra were recorded on Shimadzu LC-ESI-IT-TOF-MS equipment. IR spectra were obtained on a JASCO FT/IR-4100 spectrometer. Melting points were measured by a hot stage melting points apparatus (uncorrected). Optical rotations were measured with a JASCO P-1020 polarimeter.
For chromatography, Wakogel C-300E (Wako) was employed. (158 mg, 1.00 mmol) in EtOH (2.00 mL) was added quinoline-2-carbohydrazide [28] (187 mg, 1.00 mmol). After being stirred for 17 h at 70 °C, the reaction mixture was concentrated. The residue was dissolved with EtOAc, and the whole was washed with 1 M NaOH and brine, and dried over Na2SO4.
After the filtrate was concentrated, the residue was purified by column chromatography on silica gel (n-hexane/EtOAc = 1/3) to give the title compound 6 (107 mg, 26%): pale yellow amorphous solid;
[α] 24
For chromatography, Wakogel C-300E (Wako) was employed. (158 mg, 1.00 mmol) in EtOH (2.00 mL) was added quinoline-2-carbohydrazide [28] (187 mg, 1.00 mmol). After being stirred for 17 h at 70 °C, the reaction mixture was concentrated. The residue was dissolved with EtOAc, and the whole was washed with 1 M NaOH and brine, and dried over Na2SO4.
After the filtrate was concentrated, the residue was purified by column chromatography on silica gel (n-hexane/EtOAc = 1/3) to give the title compound 6 (107 mg, 26%): pale yellow amorphous solid;
[α] 24
5
Spectroscopic Characterization of Compounds
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NMR spectra were measured on a Bruker Avance III 500 NMR spectrometer (Bruker Corp., Billerica, MA, USA). Low and high resolution EI mass spectra were determined on an Autospec Premier P776 mass spectrometer at 70 eV (Waters Corp., Milford, MA, USA). ECD spectra were acquired on a Chirascan CD spectrometer (Applied Photophysics Ltd., Surrey, UK). IR spectra were recorded on a JASCO FT/IR-4100 spectrometer (JASCO, Tokyo, Japan). Optical rotations were obtained on an SGW-3 polarimeter with a 2 mL (length 10 cm) cell (Shanghai Shenguang Instrument Co., Ltd., Shanghai, China). HPLC separation was operated on an Agilent HPLC system (1260 infinity quaternary pump, 1260 infinity diode-array detector) using an Eclipse SB-C18 (5 μm, 9.4 × 250 mm) column (Agilent Technologies Inc., Santa Clara, CA, USA). Column chromatography (CC) was carried out with silica gel (200–300 mesh, Qingdao Haiyang Chemical Co., Qingdao, China), RP-18 (AAG12S50, YMC Co., Ltd., Kyoto, Japan), and Sephadex LH-20 (GE Healthcare, Uppsala, Sweden). Thin-layer chromatography (TLC) was performed with precoated silica gel plates (GF-254, Qingdao Haiyang Chemical Co., Qingdao, China).
6
Isolation of Compounds via HPLC
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The ethyl acetate layer (112.00 g) was chromatographed on silica gel and eluted stepwise with mixed solutions of n-hexane:ethyl acetate:methanol (10:0:0, 9:1:0, 8:2:0, 7:3:0, 6:4:0, 4:6:0, 2:8:0, 0:10:0, and 0:0:10 v/v) as mobile phases. A total of nine fractions were collected.
All compounds were obtained from Fr. 2, 3, 4, and 5 by normal phase, semi-preparative, high-performance liquid chromatography (HPLC) (Phenomenex® Luna semi-preparative column: 250 × 10 mm), cooperating with an infrared radiation (IR) detector recorded on a JASCO FT/IR 4100 Spectrometer (Jasco, Tokyo, Japan) for detection. The flow rate was 3 mL/min and eluted with n-hexane and EA (Figure 3 ).
All compounds were obtained from Fr. 2, 3, 4, and 5 by normal phase, semi-preparative, high-performance liquid chromatography (HPLC) (Phenomenex® Luna semi-preparative column: 250 × 10 mm), cooperating with an infrared radiation (IR) detector recorded on a JASCO FT/IR 4100 Spectrometer (Jasco, Tokyo, Japan) for detection. The flow rate was 3 mL/min and eluted with n-hexane and EA (
7
Fourier Transform Infrared Spectroscopy
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The IR spectra of samples were measured in the wavenumber range of 400–4000 cm−1 by a Jasco FT-IR-4100 spectrometer (Tokyo, Japan) coupled with a TGS detector and a ZnO crystal sampling accessory with transmission mode. The spectral resolution was 4 cm−1. Each spectrum was the average of 100 scans. During the whole experiment, the temperature was kept at about 25 °C and the humidity was kept at a stable level in the laboratory.
Raw spectra frequently contained noises besides sample information, so the first 500 and last 400 spectral data were deleted to remove noises, and the following analysis was based on the spectra in range of 881–3581 cm−1.
Raw spectra frequently contained noises besides sample information, so the first 500 and last 400 spectral data were deleted to remove noises, and the following analysis was based on the spectra in range of 881–3581 cm−1.
8
Palladium-Catalyzed Arylation of Diarymethanols
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All the reagents and solvents were commercially available and used as received. The 1H NMR spectra were measured on a JEOL 400 spectrometer at 400 MHz with TMS as an internal standard. The 13C NMR spectra were measured on a JEOL 400 spectrometer at 100 MHz. The IR spectra were recorded on a JASCO FT/IR-4100 spectrometer. The melting points were determined on an As-one melting-points apparatus ATM-02, and were uncorrected. High-resolution mass spectra were obtained on an AB SCEIX Triplet TOF 4600 mass spectrometer. Gas chromatography (GC) was performed with Shimadzu GC 8A. Flash column chromatography was performed with Wako-gel C-200 (100–200 mesh, Wako).
Theoretical calculations for the complexes were carried out with 16W software.14 Optimizations of the ground-state geometries of the complexes were performed by using the this pro density functional theory (DFT).15 (link) The LanL2DZ16 (link) and 6-31G(d,p)17 (link) basis sets were used to treat the palladium and all other atoms, respectively. Optimized geometries of the complexes were plotted using GaussView 6.0.18 All diarylmethanes 6, 11 and 12 are commercially available. Hence, the structures of these products were confirmed by comparison of spectral data with those of authentic samples.
Theoretical calculations for the complexes were carried out with 16W software.14 Optimizations of the ground-state geometries of the complexes were performed by using the this pro density functional theory (DFT).15 (link) The LanL2DZ16 (link) and 6-31G(d,p)17 (link) basis sets were used to treat the palladium and all other atoms, respectively. Optimized geometries of the complexes were plotted using GaussView 6.0.18 All diarylmethanes 6, 11 and 12 are commercially available. Hence, the structures of these products were confirmed by comparison of spectral data with those of authentic samples.
9
Comprehensive Material Characterization Techniques
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Powder X-ray diffraction (PXRD) patterns were obtained using a Bruker New D8 Advance diffractometer (40 kV, 40 mA, step size = 0.02°). X-ray photoelectron spectroscopy (XPS) measurement was performed using an ESCA 2000 equipped with Al Kα as an X-ray source. The spectrum was calibrated by using C 1s signal at 284.6 eV. FT-IR spectra in attenuated total reflection (ATR) mode were recorded on a Jasco FT/IR-4100 spectrometer (Jasco, Japan). UV/Vis spectra were recorded on a Scinco S-3100 spectrophotometer (Scinco, Korea).
10
Comprehensive Spectroscopic Analysis of Proligand H5L
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Elementar Vario EL III CHNS analyzer was used for the CHN analysis of the compound. MALDI mass spectrum was taken using Bruker Autoflex spectrometer at Sophisticated Test and Instrumentation Centre (STIC), CUSAT, Kochi, India. Electronic spectrum (200–900 nm) was recorded on a UV-Thermo scientific evolution 220 spectrometer and the diffuse reflectance UV-visible spectral (UV-DRS) data were recorded on Ocean Optics DH-2000-BAL instrument at the Department of Applied Chemistry (DAC), CUSAT. The NMR spectra of the proligand H5L was recorded on a Bruker Avance-III HD spectrometer at 600 MHz for 1H NMR and 150 MHz for 13C NMR at NCBS-TIFR, Bangalore, India. Infrared spectrum in the range between 4000 and 400 cm−1 was recorded on a JASCO FT-IR 4100 spectrometer with KBr pellets and the fluorescence emission studies were conducted on a Horiba fluorolog 3 (FL-1057) Spectrofluorimeter and Jazz Ocean Optics Spectrofluorimeter at the DAC.
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