1H NMR and 13C{1H} NMR high-resolution nuclear magnetic resonance spectra were recorded on a Varian Mercury Plus 400 (400 MHz/101 MHz) or a Varian Unity Inova 500 (500 MHz/126 MHz) spectrometer at room temperature. Chemical shifts are reported relative to TMS (δ 0.00) or CDCl3 (δ 7.26) for 1H NMR and CDCl3 (δ 77.2) for 13C{1H} NMR. IR spectra were recorded as thin films (PerkinElmer Spectrum 100 FT-IR Spectrometer). High-resolution mass spectra were obtained on a Thermo-Electron LTQ-FT 7T Fourier transform ion cyclotron resonance (FT-ICR) spectrometer with an atmospheric pressure chemical ionization (APCI) source with direct infusion run in positive ion mode at 5 kV. Additional accurate mass measurement analyses were conducted on either a Waters GCT Premier, time-of-flight, GCMS with electron ionization (EI), or an LCT Premier XE, time-of-flight, LCMS with electrospray ionization (ESI). Samples were taken up in a suitable solvent for analysis. The signals were mass measured against an internal lock mass reference of perfluorotributylamine (PFTBA) for EI-GCMS, and leucine enkephalin for ESI–LCMS. Waters software calibrates the instruments, and reports measurements, by use of neutral atomic masses. The mass of the electron is not included.
Unity inova 500
Manufactured by Agilent Technologies
Sourced in United States
The Unity Inova 500 is a high-performance nuclear magnetic resonance (NMR) spectrometer designed for analytical and research applications. It provides a magnetic field strength of 500 MHz and is capable of performing various NMR experiments for the characterization of chemical compounds and materials.
Automatically generated - may contain errors
Lab products found in correlation
Mercury plus 400, by Agilent Technologies (3 mentions)
Sephadex lh 20, by Cytiva (2 mentions)
L 7100 pump, by Hitachi (2 mentions)
Topspin, by Bruker (2 mentions)
Ultraflex 3 maldi tof tof, by Bruker (2 mentions)
Prep els detector, by Bruker (2 mentions)
Unity inova 400, by Agilent Technologies (2 mentions)
Spectrum 100 ftir spectrometer, by PerkinElmer (1 mentions)
Gct premier, by Waters Corporation (1 mentions)
Pu 2089 plus hplc pump, by Jasco (1 mentions)
715 spectropolarimeter, by Jasco (1 mentions)
Api 2000, by Thermo Fisher Scientific (1 mentions)
Bs 997 01, by Jasco (1 mentions)
Merck silica gel 60, by Merck Group (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Snap cartridge, by Biotage (1 mentions)
Unity inova as600, by Agilent Technologies (1 mentions)
Silica gel, by Merck Group (1 mentions)
Acquity ultra performance lc, by Waters Corporation (1 mentions)
Formaldehyde, by Thermo Fisher Scientific (1 mentions)
29 protocols using unity inova 500
1
High-Resolution NMR and Mass Spectrometry
2
Novel DNA Synthesis and Characterization
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Chemicals and anhydrous solvents were purchased from Fluka-Sigma-Aldrich. TLCs were run on Merck silica gel 60 F254 plates. Silica gel chromatography was performed using Merck silica gel 60 (0.063–0.200 mm). The API 2000 (Applied Biosystems) mass spectrometer was used to perform the analyses of the intermediates and the monomer. NMR data were collected on Varian Mercury Plus400 and UNITYINOVA 500 MHz spectrometers equipped with a broadband inverse probe with z-field gradient, and on a Varian UNITYINOVA 700 MHz spectrometer equipped with a triple resonance cryoprobe. The data were processed using the Varian VNMR and the iNMR (http://www.inmr.net ) software packages. Reagents and phosphoramidites for DNA syntheses were purchased from Glenn Research. ON syntheses were performed on a PerSeptive Biosystem Expedite DNA synthesizer. HPLC purifications and analyses were carried out using a JASCO PU-2089 Plus HPLC pump equipped with a JASCO BS-997–01 UV detector. CD experiments were performed on a JASCO 715 spectropolarimeter equipped with a PTC-348 temperature controller. The fibrinogen assay was performed using a JASCO 530 UV spectrophotometer equipped with the PTC-348 temperature controller.
3
Synthesis and Characterization of Novel Compounds
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All reactions were performed in oven-dried glassware
under ambient
atmosphere wrapped with aluminum foil. All chemicals were purchased
from commercial vendors and used as received unless otherwise specified.
ACS grade acetonitrile, 1.2-dichloromethane, hexanes, and acetone
were used as solvents and used as received without drying. Reactions
were magnetically stirred and monitored using glass-backed, 250 μm
thickness, F254 hard layer SiliaPlate thin-layer chromatography (TLC)
plates purchased from Silicycle. 1H and 13C
nuclear magnetic resonance spectra were recorded at room temperature
on a Varian Mercury Plus 400 (400 MHz/101 MHz) or a Varian Unity Inova
500 (500 MHz/126 MHz) spectrometer. Chemical shifts were referenced
to either CDCl3 (δ 7.26) or dimethyl sulfoxide (DMSO)-d6 (δ 2.50) for 1H NMR and CDCl3 (δ 77.16) or DMSO-d6 (δ
39.52) for 13C NMR. High-resolution mass spectra were obtained
on a Thermo-Electron LTQ-FT 7T FFTICR-MS with an Ion Max Source (positive
electrospray ionization).
under ambient
atmosphere wrapped with aluminum foil. All chemicals were purchased
from commercial vendors and used as received unless otherwise specified.
ACS grade acetonitrile, 1.2-dichloromethane, hexanes, and acetone
were used as solvents and used as received without drying. Reactions
were magnetically stirred and monitored using glass-backed, 250 μm
thickness, F254 hard layer SiliaPlate thin-layer chromatography (TLC)
plates purchased from Silicycle. 1H and 13C
nuclear magnetic resonance spectra were recorded at room temperature
on a Varian Mercury Plus 400 (400 MHz/101 MHz) or a Varian Unity Inova
500 (500 MHz/126 MHz) spectrometer. Chemical shifts were referenced
to either CDCl3 (δ 7.26) or dimethyl sulfoxide (DMSO)-d6 (δ 2.50) for 1H NMR and CDCl3 (δ 77.16) or DMSO-d6 (δ
39.52) for 13C NMR. High-resolution mass spectra were obtained
on a Thermo-Electron LTQ-FT 7T FFTICR-MS with an Ion Max Source (positive
electrospray ionization).
4
Purification and Characterization of Surfactants
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All commercially obtained solvents and reagents were used without further purification. Analytical thin-layer chromatography was carried out on Merck silica gel 60 F254 glass plates, and flash chromatography was performed on Merck silica gel 60 (70 to 230 mesh).
Visualization was accomplished with short-wave ultraviolet (UV) light and/or KMnO4 staining solution followed by gentle heating. Surfactants were purified by preparative reverse-phase high-performance liquid chromatography (RP-HPLC) on a Biotage SP1 HPFC Flash Purification System using a reverse-phase Biotage SNAP Cartridge (KP-C18-HS, 60 g). For synthesis characterization, 1H and 13C solution-state NMR were recorded on a Varian Unity Inova 500 (500 MHz for 1H and 125 MHz for 13C) or a Varian Unity Inova AS600 (600 MHz for 1H and 150 MHz for 13C) spectrometer. Chemical shifts δ are reported relative to the resonance signal of 1H or 13C cores of tetramethylsilane and in parts per million. The 1H spectra were calibrated by setting the solvent peaks, caused by remaining traces of protons, to values known from the literature (δCHCl3 = 7.26 ppm, δCD3OH = 4.87 ppm, and δD2O = 4.79 ppm). The coupling constants J are reported in hertz.
Visualization was accomplished with short-wave ultraviolet (UV) light and/or KMnO4 staining solution followed by gentle heating. Surfactants were purified by preparative reverse-phase high-performance liquid chromatography (RP-HPLC) on a Biotage SP1 HPFC Flash Purification System using a reverse-phase Biotage SNAP Cartridge (KP-C18-HS, 60 g). For synthesis characterization, 1H and 13C solution-state NMR were recorded on a Varian Unity Inova 500 (500 MHz for 1H and 125 MHz for 13C) or a Varian Unity Inova AS600 (600 MHz for 1H and 150 MHz for 13C) spectrometer. Chemical shifts δ are reported relative to the resonance signal of 1H or 13C cores of tetramethylsilane and in parts per million. The 1H spectra were calibrated by setting the solvent peaks, caused by remaining traces of protons, to values known from the literature (δCHCl3 = 7.26 ppm, δCD3OH = 4.87 ppm, and δD2O = 4.79 ppm). The coupling constants J are reported in hertz.
5
NMR Characterization of Enzymatic Isomerization
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1H NMR
spectra at 500 MHz were recorded in D2O at 25 °C using
a Varian Unity Inova 500 spectrometer that was shimmed to give a line
width of ≤0.7 Hz for each peak of the doublet due to the C-1
proton of GAP hydrate, or ≤0.5 Hz for the most downfield peak
of the double triplet due to the C-1 proton of [1-13C]GA
hydrate. Spectra (16–64 transients) were obtained using a sweep
width of 6000 Hz, a pulse angle of 90°, an acquisition time of
6 s, and a relaxation delay of 60 s (4T1) for experiments on the TIM-catalyzed isomerization of GAP in D2O or 120 s (>8T1) for experiments
on the TIM-catalyzed reactions of [1-13C]GA in D2O.33 (link),50 (link) Baselines were subjected to a first-order
drift correction before determination of peak areas. Chemical shifts
are reported relative to HOD at 4.67 ppm.
spectra at 500 MHz were recorded in D2O at 25 °C using
a Varian Unity Inova 500 spectrometer that was shimmed to give a line
width of ≤0.7 Hz for each peak of the doublet due to the C-1
proton of GAP hydrate, or ≤0.5 Hz for the most downfield peak
of the double triplet due to the C-1 proton of [1-13C]GA
hydrate. Spectra (16–64 transients) were obtained using a sweep
width of 6000 Hz, a pulse angle of 90°, an acquisition time of
6 s, and a relaxation delay of 60 s (4T1) for experiments on the TIM-catalyzed isomerization of GAP in D2O or 120 s (>8T1) for experiments
on the TIM-catalyzed reactions of [1-13C]GA in D2O.33 (link),50 (link) Baselines were subjected to a first-order
drift correction before determination of peak areas. Chemical shifts
are reported relative to HOD at 4.67 ppm.
6
Comprehensive Analytical Characterization
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The infrared (IR) spectra were recorded on a Nicolet Avatar 320 Fourier transform IR spectrophotometer (Thermo Electron, Akron, OH, USA). The UV spectra were measured on a Hitachi U-3310 spectrophotometer (Hitachi High Technologies America, Salt Lake City, UT, USA). The NMR spectra were run on a Varian unity INOVA-500, and Varian VNMRS 600 spectrometers (Palo Alto, CA, USA). The Electrospray ionization (ESI) and High-resolution electrospray ionisation (HRESI) mass spectra were recorded on a Finnigan MAT LCQ ion trap mass spectrometer and a Finnigan MAT 95S mass spectrometer (Finnigan MAT, San Jose, CA, USA), respectively. The HPLC analyses and UPLC were run on a Hitachi L-7100 pump equipped with a binary solvent delivery and autosampler (Hitachi, Tokyo, Japan), and a Waters Acquity Ultra Performance LC (Waters, Milford, MA, USA), respectively. Column chromatography was performed using silica gel (70–230 mesh, Merck, Darmstadt, Germany) and Sephadex LH-20 (Amersham Biosciences, Uppsala, Sweden). Isoorientin and quercitrin (quercetin 3-O-α-L-rhamnoside) (as internal standard; I.S.) were bought from Tauto Biotech (Shanghai, China). Solvents were purchased from Merck (Darmstadt, Germany).
7
Synthesis of Secondary Amines
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Secondary amines were synthesized according to the described procedure24 (link). The appropriate aldehyde and primary amine derivatives were commercially available from Sigma Aldrich. Formaldehyde was available as a 37% solution in water from Fisher Bioreagents. Sodium triacetoxyborohydride was purchased from Apollo Scientific. Reactions were accomplished in an Anton Paar BM500 vibrational ball mill by using stainless-steel milling beakers (5 mL) and stainless-steel milling balls. 1H NMR spectra were recorded on a Varian Unity Inova 500 (500 MHz) spectrometer. Chemical shifts δ are reported in parts per million relative to the residual solvent peak (DMSO-d6 = 2.49 ppm for 1 H). Coupling constants are given in Hertz. High resolution mass spectra were recorded on Agilent 6545 Q-TOF. Thin-layer chromatography (TLC) was carried out with Polygram SIL G/UV254, silica gel (Macherey–Nagel GmbH & Co. KG, Duren, Germany). Compounds were visualized by means of irradiation with UV light and/or by treatment with a solution of ninhydrin. Flash chromatography was carried out using Büchi FlashPure Cartridges (silica gel 40 μm irregular) on a Büchi Pure Chromatography System with an integrated UV and ELSD detector. Melting points (uncorrected) were determined using a Stuart Scientific SMP30 apparatus. Infrared (IR) spectra were recorded using a Nicolet 8700 spectrometer.
8
Purification and Characterization of Organic Compounds
9
Acylation of Lignin Copolymer Synthesis
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The oven-dried lignin (1 g) was mixed with acetic anhydride-pyridine (3:10, v/v, and 13 mL) and vigorously stirred for 24 hours at room temperature10 (link). The mixture was added dropwise in cold water and precipitated followed by centrifugation. The resulting solid product was thoroughly washed with DI water to remove the unreacted acetic anhydride and acetic acid byproducts. The product was dried overnight in an oven at 40 °C. 1H-NMR spectra of lignin and lignin-PCL copolymer were obtained by NMR spectroscopy (Varian UNITY INOVA 500).
10
NMR Spectroscopy of Organic Compounds
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The 1D 1H NMR and 2D homo- and heteronuclear NMR (COSY, TOCSY, ROESY, HSQC, and HMBC) were acquired with the application of a Varian Unity Inova 500 spectrometer (500 MHz). Spectra were recorded in dimethyl sulfoxide-d6 (DMSO-d6). NMR data were processed and analyzed by TopSpin (Bruker, Billerica, MA, USA) and SPARKY software (3.114, Goddard and Kneller, freeware (https://www.cgl.ucsf.edu/home/sparky ).
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