For the alignments of the samples, 750 MHz nuclear magnetic resonance (Bruker, Billerica, MA, USA), equivalent to 17.4 T as the magnetic field strength, was used. The sample concentrations in the 0.1 mm inner diameter soda glass capillary (Müller, Germany) were 50 mM in ultrapure water. The sample alignments were confirmed by the polarized-light microscope Eclipse E600 POL (Nikon, Tokyo, Japan) and then each sample was lyophilized. The polarized IR measurements were performed using an FT/IR-6100 Fourier transform infrared spectrometer (JASCO, Tokyo, Japan) with an MCT detector and IRT-3000 infrared microscope accessory. The background spectra for the perpendicular alignment of the target fibril were collected in the air near the capillary and then 64 perpendicular scans from a light polarizer were measured at 4 cm−1 resolution. Next, 64 parallel scans were collected in the same condition. The background spectra for the parallel scans were measured for the last time as single-beam spectra. The resulting interferogram was Fourier-transformed using an application, Spectra manager (JASCO).
Ft ir 6100 fourier transform infrared spectrometer
Manufactured by Jasco
Sourced in Japan
The FT/IR-6100 Fourier transform infrared spectrometer is a laboratory instrument that measures the infrared spectrum of a sample. It employs the principles of Fourier transform spectroscopy to rapidly collect high-resolution data.
Automatically generated - may contain errors
Lab products found in correlation
Spectra manager, by Jasco (1 mentions)
Eclipse e600 pol, by Nikon (1 mentions)
High performance digital ft nmr spectrometer advance 3, by Bruker (1 mentions)
Eca 600 spectrometer, by JEOL (1 mentions)
Dip 370 digital polarimeter, by Jasco (1 mentions)
Eca 800, by JEOL (1 mentions)
Kieselgel 60, by Merck Group (1 mentions)
Avance 3 500 spectrometer, by Bruker (1 mentions)
P 1010 polarimeter, by Jasco (1 mentions)
Kieselgel 60 f254 dc fertigplatten, by Merck Group (1 mentions)
7 protocols using ft ir 6100 fourier transform infrared spectrometer
1
NMR and IR Analysis of Aligned Protein Fibrils
2
Synthesis and Characterization of 3-Amino-6-Phenylthieno[2,3-b]Pyridine-2-Carboxamides
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Melting points were determined by open glass capillary tubes using an Electro thermal IA9100 digital melting point apparatus and were uncorrected. Elemental microanalyses were carried out at the Micro Analytical Unit at Cairo University and were found within ± 0.5%. 1H NMR and 13C NMR spectra were recorded on a Bruker High Performance Digital FT-NMR Spectrometer Advance III (400/100 MHz) in the presence of TMS as the internal standard. Infrared spectra were recorded by using the KBr disc technique on a Jasco FT/IR-6100, Fourier transform, Infrared spectrometer (Japan) at the cm−1 scale. The ESI-mass spectra were measured using an Advion Compact Mass Spectrometer (CMS) NY, USA. Follow-up of the reactions and checking the purity of the compounds were made by TLC on silica gel aluminum sheets (Type 60, F 254, Merck, Darmstadt, Germany) and the spots were illustrated by exposure to UV analysis lamp at λ 254/366 nm or by iodine vapor. The nomenclature of the new synthesized compounds is according to the IUPAC system. The starting 3-amino-6-phenylthieno[2,3-b]pyridine-2-carboxamides 1a ,b were prepared as per reported methods [44 ,45 ].
3
Photografting of Arylazo Sulfones on Gold
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Chemicals. Arylazo sulfones were prepared from the corresponding anilines by following a known method. 43 Spectroscopical data of the compounds are in accordance with the literature. Dry and purified acetonitrile was obtained from a Pure Solv system from Innovative Technology.
Photografting was achieved by placing a gold plate in a test tube with a septum screw cap; the tube was filled with argon and a 0.1 mM solution of the chosen azosulfone in ACN was deposited with a needle, through the septum, on the gold surface. Irradiation was performed using a Kessil Lamp (40 W, 456 nm) as the light source for 8 h (Scheme 1).
Scheme 1. Experimental setup.
Substrates. Gold coated (100 nm) silicon wafers obtained from Sigma-Aldrich, were cut into 1 × 1 cm 2 pieces and successively rinsed in a bath of sulfuric acid (95%) for 2 s, and with distilled water and under sonication in distilled water, acetone, and absolute ethanol (380 s each) and finally dried by an argon stream.
Infrared reflection absorption spectroscopy (IRRAS). Spectra of modified plates were recorded using a purged (low CO 2 , dry air) Jasco FT/IR-6100 Fourier Transform InfraRed Spectrometer equipped with an MCT (mercury-cadmium-telluride) detector. For each spectrum, 1000 scans were accumulated with a spectral resolution of 4 cm -1 . The background recorded before each spectrum was that of a cleaned substrate.
Photografting was achieved by placing a gold plate in a test tube with a septum screw cap; the tube was filled with argon and a 0.1 mM solution of the chosen azosulfone in ACN was deposited with a needle, through the septum, on the gold surface. Irradiation was performed using a Kessil Lamp (40 W, 456 nm) as the light source for 8 h (Scheme 1).
Scheme 1. Experimental setup.
Substrates. Gold coated (100 nm) silicon wafers obtained from Sigma-Aldrich, were cut into 1 × 1 cm 2 pieces and successively rinsed in a bath of sulfuric acid (95%) for 2 s, and with distilled water and under sonication in distilled water, acetone, and absolute ethanol (380 s each) and finally dried by an argon stream.
Infrared reflection absorption spectroscopy (IRRAS). Spectra of modified plates were recorded using a purged (low CO 2 , dry air) Jasco FT/IR-6100 Fourier Transform InfraRed Spectrometer equipped with an MCT (mercury-cadmium-telluride) detector. For each spectrum, 1000 scans were accumulated with a spectral resolution of 4 cm -1 . The background recorded before each spectrum was that of a cleaned substrate.
4
FT-IR Spectroscopic Analysis of Hydrated Samples
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IR absorption spectra were recorded using an FT/IR–6100 Fourier transform infrared spectrometer of JASCO (Tokyo, Japan). 15 µL of a hydrated sample was loaded into a CaF2 cell with 10-µm optical path length (Biocell, Biotools, FL, USA). Each spectrum was measured with 512-times accumulation at a spectral resolution of 4 cm–1. The data generated in this study are provided in the Source Data.
5
Lipolysis Kinetics via FTIR Spectroscopy
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Lipolysis experiments were carried out by adding 5µL of rGPLRP2 solution (500 or 1000 nM) to 45 µL of substrate dispersions (C8-MGDG micelles, LC MGDG micelles or CRF suspensions) to obtain 50 or 100 nM final enzyme concentration. The reaction mixtures were placed and squeezed between two CaF 2 transmission crystals with a 50 μm polytetrafluoroethylene (Teflon) spacer. IR-spectra were then recorded each 5 min during 2 h at 37 °C using a JASCO™ FT/IR-6100 Fourier-transform infrared spectrometer. The sample chamber was continuously purged with a flow of dry air to avoid the presence of water vapour and the formation of semiheavy water (HDO) molecules in the sample. All the spectra are an average of 128 scans, with 4 cm -1 of resolution, apodized with a cosine function.
6
Structural Characterization of Compounds
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Optical rotation was measured with a DIP-370 digital polarimeter (Jasco). IR spectra were recorded on an FT/IR 6100 Fourier transform infrared spectrometer (Jasco). 1 H-, 13 C-, and 2D-NMR spectra were recorded on an ECA-800 or ECA-600 spectrometer (JEOL), and the chemical shifts were referenced to TMS as the internal standard.
7
Analytical Techniques for Chemical Characterization
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Optical rotation was measured using a JASCO P-1010 Polarimeter. Nuclear magnetic resonance (NMR) spectra were recorded on a Bruker Avance III 500 spectrometer in CDCl 3 .
Chemical shifts and coupling constants were given as δ and Hz, respectively, and 1 H and 13 C chemical shifts were referenced to the residual solvent peaks (δ H = 7.26 and δ C = 77.24).
Infrared (IR) spectra were recorded on a JASCO FT/IR-6100 Fourier Transform Infrared Spectrometer. High-resolution mass spectra (HRMS) were obtained on an LTQ Orbitrap hybrid mass spectrometer (Thermo Scientific, Bremen, Germany) equipped with a nanospray ionizat ion (NSI) source . Open column chromatography was performed on Kieselgel 60 (70-230 mesh, Merck). Highperformance liquid chromatography (HPLC) was performed using a COSMOSIL Si60 HPLC column (5SL, 10 × 250 mm). Analytical thin-layer chromatography (TLC) was performed using Kieselgel 60 F 254 DC-fertigplatten (Merck). All solvents were reagent grade.
Chemical shifts and coupling constants were given as δ and Hz, respectively, and 1 H and 13 C chemical shifts were referenced to the residual solvent peaks (δ H = 7.26 and δ C = 77.24).
Infrared (IR) spectra were recorded on a JASCO FT/IR-6100 Fourier Transform Infrared Spectrometer. High-resolution mass spectra (HRMS) were obtained on an LTQ Orbitrap hybrid mass spectrometer (Thermo Scientific, Bremen, Germany) equipped with a nanospray ionizat ion (NSI) source . Open column chromatography was performed on Kieselgel 60 (70-230 mesh, Merck). Highperformance liquid chromatography (HPLC) was performed using a COSMOSIL Si60 HPLC column (5SL, 10 × 250 mm). Analytical thin-layer chromatography (TLC) was performed using Kieselgel 60 F 254 DC-fertigplatten (Merck). All solvents were reagent grade.
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