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24 protocols using iraffinity 1 ftir spectrometer

1

FTIR Spectroscopy with ATR Accessory

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An IRaffinity-1 FTIR Spectrometer, (Shimadzu, Japan) fitted with a high energy ceramic light source (single beam), He–Ne laser for alignments, germanium-coated potassium bromide beam splitter, and DLATGS detector equipped with a temperature controlling unit was used in the analysis. A horizontal ATR accessory model 8200HA (PIKE Technology, USA) fitted with a zinc selenide (ZnSe) crystal, which is a rectangular-shaped yellow prism (dimensions: 80 mm long, 10 mm wide, 4 mm thick), was used.
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2

Spectroscopic Characterization of Organic Compounds

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Melting points are uncorrected. NMR spectra were recorded using a Bruker Ascend 600 spectrometer (Bruker, Billerica, MA, USA). To assign the structures, the following 2D experiments were employed: 1H-13C gradient selected HSQC and HMBC sequences. Standard experimental conditions and standard Bruker programs were used. The 1H- and 13C-NMR spectral data are given relative to the TMS signal at 0.0 ppm. HR mass spectra were recorded with Bruker Impact II (Bruker, Billerica, MA, USA). Solid-state infrared spectra were recorded in the range of 4000–1000 cm−1 using the Shimadzu IRAffinity-1 FTIR spectrometer (Shimadzu, Kyoto, Japan) and KBr pellet method. CHNS elemental analysis was performed using EuroVector 3018 analyser (EuroVector, Pavia, Italy). Total halides were determined using titration (after mineralization) with mercuric nitrate solution.
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3

Synthesis and Characterization of ASBDs

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The ASBDs (Figure 1) were synthesized in the Department of Organic Chemistry at the Medical University of Silesia in Sosnowiec, as previously described [25 (link)]. The reaction of Bet with propynoic acid was carried by the Steglich method to give 28-O-propynoylbetulin (EB5). Bet was converted to the 28-O-propargyloxycarbonylbetulin (EB25/1) by esterification with propargyl chloroformate with the presence of pyridine in benzene (Figure 7. Both ASBDs were purified using gel column chromatography. The structures of ASBDs were determined on the basis of their 1H- and 13C-NMR (Bruker AVANCE III HD 600, Billerica, MA, USA, deuterated chloroform), IR (IRAffinity-1 FTIR spectrometer; Shimadzu Corporation, Kyoto, Japan, KBr pellet), and MS spectra (Bruker Impact II, Billerica, MA, USA). The 1H- and 13C-NMR spectral data for ASBDs were consistent with the literature values (Supplementary Materials, Figures S1–S4).
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4

FTIR Analysis of OSA-COS Samples

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After overnight drying of the OSA-COS samples in a 70 °C oven, 1 mg of material was ground with 100 mg of KBr to a uniform powder, as described in our previous publication [28 (link)]. A manual press and pellet die were used to obtain a thin pellet. The samples were analyzed on an IR Affinity-1 FTIR spectrometer (Shimadzu, Nagoya, Japan) between 4000 and 400 cm−1. Sixty-four scans were performed at a 4.0 cm−1 resolution.
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5

Characterization of Organic Compounds

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Melting points were determined in the open capillary tubes on an Electrothermal IA 9300 melting point apparatus Electrothermal Engineering Ltd, Rochford, UK. The values given are uncorrected. Optical rotation properties were measured with an ATAGO SAC-I polarimeter (Atago, Tokyo, Japan) using a sodium lamp (589 nm) at 20 °C. The NMR spectra (600/150 MHz) were recorded on a Bruker Avance (Bruker , Billerica, MA, USA) III 600 spectrometer in CDCl3. Chemical shifts were reported in ppm (δ), and J values in Hz. Multiplicity was designated as the singlet (s), doublet (d), triplet (t), quartet (q) and multiplet (m). High-resolution mass spectral (HR-MS) analysis was performed on a Bruker Impact II instrument. Solid state infrared spectra were recorded in the range of 4000–1000 cm−1 using the Shimadzu IRAffinity-1 FTIR spectrometer (Shimadzu, Kyoto, Japan) and KBr pellet method. Thin layer chromatography (TLC) was performed on silica gel 60 254F plates (Merck, Darmstadt, Germany) using a mixture of different organic solvents as an eluent. The chromatographic spots were detected by spraying with a solution of 5% sulfuric acid, followed by heating. Column chromatography was performed on silica gel 60, <63 μm (Merck), with the mixture of chloroform and ethanol (15:1, v/v) or hexane and ethyl acetate (3:2, v/v) as an eluent. Solvents were dried and purified according to usual procedures.
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6

Studying Lipopolymer-Amino Acid Interactions via FTIR

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Fourier-transform infrared (FTIR) spectroscopy was used to study the interaction between lipopolymers and amino acids as well as the changes induced by the polymerization process. To this end, 0.4 ml of the liposomal suspension with or without amino acids or polymerization was lyophilized. The solid was then resuspended in D2O in order to avoid interference induced by H2O. The lipid suspension was pipetted onto ATR cells and dried with a hair drier. Infrared spectra were recorded from 3000 to 1000 cm−1 in an IRAffinity-1 FTIR spectrometer (Shimadzu). Data were analyzed, normalized, and baseline corrected with the IRsolution software (Shimadzu). Frequencies were determined by the peak identification routine of the software.
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7

FT-IR Spectroscopy of Modified Agar

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The FT-IR spectra of the unmodified and modified agar samples were obtained using the method described by Gope et al. [37 (link)] with an IRAffinity-1 FT-IR spectrometer (Shimadzu, Kyoto, Japan).
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8

FTIR Spectroscopy of Oil Samples

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Fourier transform infrared spectroscopy (FTIR) was performed using a Shimadzu IRAffinity‐1 FTIR spectrometer. The oil samples were applied to the surface of KBr pellets. After 24 hr of vacuum drying, the FTIR spectra of oil samples were recorded in the region of 4,000–1,660 cm−1, with 120 scans acquired at a resolution of 4 cm−1.
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9

Electrochemical Analysis of Cu@Ni-MOF Catalyst

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The metal ion (Cu/Ni) content in the Cu@Ni-MOF was recorded by inductively coupled plasma mass spectrometry (ICP–MS) (Icap Qc). The electrochemical measurements were carried out on a CHI 660E potentiostat electrochemical workstation (Thermo-Fisher, Berlin, Germany). X-ray diffraction (XRD) patterns were recorded with a Rigaku Miniflex 600 X-ray diffractometer (Rigaku, Tokyo, Japan) from 5° to 50°. An infrared spectrum was recorded using an IR Affinity-1 FT-IR spectrometer (Shimadzu, Kyoto, Japan) in the range of 400–4000 cm−1. Cu(NO3)2, Ni(NO3)2, 2,6-pyridinedicarboxylic acid were bought commercially(Jinan Henghua Technology Co., Ltd., Jinan, China), acetylene carbon black and PolyVinylidene Fluoride were bought commercially(TIMCAL, Changzhou, China)
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10

Characterization of Organic Compounds Using Advanced Analytical Techniques

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FT-IR spectra were recorded on an IRAffinity-1 FT-IR spectrometer (Shimadzu, Japan) with KBr pellet. EA was carried out on a Euro EA 3000 Elemental Analyzer (Leeman Labs, the USA). The purity of (Z)-4-oxo-4-(phenylamino)but-2-enoic acid was confirmed by titration. The purity of N-PMI was recorded on an LC-20A liquid chromatograph (Shimadzu, Japan). 13C-NMR and high-resolution mass spectrum (HRMS) of both (Z)-4-oxo-4-(phenylamino)but-2-enoic acid and N-PMI were recorded on a Bruker Avance III 400 MHz nuclear magnetic resonance spectrometer (the USA) and a Thermo Fisher TSQ Quantum Ultra mass spectrometer (the USA), respectively.
Analytical instruments of the polymers are given in Table 1 as a list.10.1080/15685551.2019.1581490-T0001

A list of the analytical instruments.

Characterization methodsBrand modelsCorporation and country
EAEuro EA 3000 Elemental AnalyzerLeeman Labs, the USA
SEMS4800 scanning electron microscopeHITACHI, Japan
GPCPLGPC220 gel permeation chromatographyAgilent, the USA
TGASTA2500 simultaneous TG-DSC apparatusNETZSCH, Germany
DSCDSC1 differential scanning calorimeterMettler Toledo, Switzerland
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