The powdered PH was analyzed with Bruker Avance III HD 500 MHz NMR Spectrometer at ambient temperature. CryoProbe™ Prodigy was used for 13C that employed both cross-polarization and magic angle spinning. 4 mm rotor was used in this detection. Acquisition time was 0.027 s, delay time was 5 s, and the proton 90° pulse time was 3.7 μs and 1024 scans for each sample. Mestrenova software was used to analyze the results.
Avance 3 hd 500 mhz nmr spectrometer
Manufactured by Bruker
Sourced in United States, Germany
The Avance III HD 500 MHz NMR spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for analytical and research applications. It provides a magnetic field strength of 500 MHz, allowing for high-resolution analysis of chemical samples.
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Lab products found in correlation
Alpha 1 2 ld plus, by Martin Christ (2 mentions)
Pall nanocep, by Pall Corporation (1 mentions)
Solarix fourier transform ion cyclotron resonance mass spectrometer, by Bruker (1 mentions)
Gcms qp2010 se gas chromatograph mass spectrometer, by Shimadzu (1 mentions)
Irtracer 100 fourier transform infrared spectrophotometer, by Shimadzu (1 mentions)
Avance 3 hd 400 mhz nmr spectrometer, by Bruker (1 mentions)
Acquity uplc system, by Waters Corporation (1 mentions)
Cryoprobe, by Bruker (1 mentions)
Uv 2600 uv vis spectrophotometer, by Shimadzu (1 mentions)
Frontier ft ir spectrometer, by PerkinElmer (1 mentions)
D8 advance x ray diffractometer, by Bruker (1 mentions)
V 730 uv vis spectrophotometer, by Jasco (1 mentions)
Microtof mass spectrometer, by Bruker (1 mentions)
P 2000 digital, by Jasco (1 mentions)
J 810, by Jasco (1 mentions)
Alpha spectrometer, by Bruker (1 mentions)
Av 300 mhz spectrometer, by Bruker (1 mentions)
Synapt hdms qtof mass spectrometer, by Waters Corporation (1 mentions)
Ct 02 50, by Martin Christ (1 mentions)
Q exactive mass spectrometer, by Thermo Fisher Scientific (1 mentions)
19 protocols using avance 3 hd 500 mhz nmr spectrometer
1
NMR Spectroscopy Analysis of Powdered PH
2
Comprehensive PPG Chemical Characterization
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The chemical composition of PPGs was analyzed using an Agilent 6520 Accurate-Mass Quadrupole Time-of-Flight (Q-TOF) LC/MS system (Agilent Technologies). The instrumentation is detailed in our previous report [22 (link)]. Analytical conditions are summarized in Tables S3 and S4 . The structural assignment of PPGs dissolved in deuterium oxide (D2O) or dimethyl sulfoxide (DMSO)-d6 was performed using an AVANCE III HD 500 MHz NMR spectrometer equipped with a QCI CryoProbe at 298 K and the TopSpin pl3.6 software (Bruker, Billerica, MA, USA).
3
NMR Analysis of Wine Samples
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Wine samples were prepared according to the method optimized from our previous works [31 (link),32 (link),52 (link)] together with the work of Mascellani et al. [26 (link)]. In brief, the pH of samples was determined and adjusted to 6.0 using 1.0 N NaOH. Insoluble particles were primarily removed by centrifugation under 4100× g at 25 °C for 15 min. The clear wine supernatant was ultrafiltrated through a centrifugal device with 3 kDa molecular weight cut-offs (Pall Nanocep®, Pall Life Sciences, Ann Arbor, MI, USA). The filtrate was then diluted 1:1 (v/v) with phosphate buffer pH 6.0 (300 mM KH2PO4, 10% (w/w) D2O) consisting of 1 mM 3-(Trimethylsilyl) propionic-2, 2, 3, 3-d4 acid sodium salt (TSP) (Merck, Darmstadt, Germany) as an internal standard. Finally, 600 μL of the mixture was transferred to a 5 mm NMR tube and subjected to a Bruker Avance III HD 500 MHz NMR spectrometer (Bruker, Rheinstetten, Germany). The temperature was set to 300 K (26.8 °C). The acquisition was operated at a time domain (TD) of 65,536, an acquisition time (AQ) requirement of 3.198 s, a number of scans (NS) of 256 and a relaxation time (D1) set to 4 s. The Bruker pulse sequence (noesygppr1d) was applied to suppress the residual water signal.
4
Spectroscopic Characterization of Chemical Samples
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Proton nuclear magnetic resonance (1H NMR) spectra were recorded on an AVANCE III HD 400 MHz NMR spectrometer (Bruker) or an AVANCE III HD 500 MHz NMR spectrometer (Bruker). Carbon-13 nuclear magnetic resonance (13C NMR) spectra were recorded on the AVANCE III HD 400 MHz NMR spectrometer with a Cryoprobe (Bruker). Mass spectra were recorded on a solariX Fourier transform ion cyclotron resonance mass spectrometer (Bruker) or a ACQUITY UPLC system (Waters) or a GCMS-QP2010 SE gas chromatograph mass spectrometer (Shimadzu). Fourier transform infrared (FT-IR) spectra were recorded on a IRTracer-100 Fourier transform infrared spectrophotometer (Shimadzu). UV/Vis spectra were acquired on a UV-2600 UV-Vis spectrophotometer (Shimadzu). The pressure in the pressure tight vessel was measured using a Krone digital pressure gauge KDM30 (Krone).
5
Synthesis and Characterization of F127-Diacrylate
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First, F127 was dissolved in 40 mL DCM. TEA was added into the stirred F127 solution. After 5 min, acryloylchloride was added slowly via syringe. The mixture was stirred at ambient temperature for 72 h. Second, the mixture was concentrated under reduced pressure to a volume of 20 mL and then filtered to remove precipitated triethylamine hydrochloride. The solution was poured into 300 mL t-butyl methyl ether to precipitate the diacrylate product. The product was then collected by filtration. Finally, the product was dissolved in 50 mL water, dialyzed for 7 days, and lyophilized to obtain F127-DA. The structures of F127 and F127-DA were inspected by the Bruker Avance-III HD 500 MHz NMR spectrometer (Billerica, MA).
6
NMR Characterization of Carrageenan
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We sent 10 mg kappa and lambda-carrageenan samples to Spectral Services, Köln, for NMR measurements. In brief, 10 mg substance was dissolved in 1 mL D2O containing 3-(trimethylsilyl) propionic acid-d4 sodium salt (0.01% as standard). Measurements for 1H spectra were done with an Avance III HD 500 MHz NMR spectrometer (Bruker, Billarica, MA, USA).
7
NMR Characterization of Agl24 Reaction Product
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The HPLC-purified Agl24 products from three to five reactions each (0.5–2 mg) were combined and dried using a Christ RVC 2–25 speed vacuum fitted with a Christ CT 02–50 cold-trap to remove excess acetonitrile, then freeze dried (Alpha 1–2 LDplus, Christ) to remove residual water. Products were subsequently dissolved in 600 µL of D2O and NMR spectra were recorded at 293 K. The spectra were acquired on a Bruker AVANCE III HD 500 MHz NMR Spectrometer equipped with a 5 mm QCPI cryoprobe. For 1D TOCSY experiments, H1’ was irradiated at 5.35 ppm, H2’ was irradiated at 3.90 ppm, and H1” was irradiated at 4.49 ppm (Figure 6—figure supplement 1 ). A combination of 1H 1H COSY, 1D TOCSY, and 1H 13C HSQC experiments were used to fully assign the 1H and 13C signals for the Agl24 reaction product. Full 1H and 13C chemical shift assignments can be found in Table 1 and are recorded with respect to the residual HDO signal at 4.7 ppm.
8
Synthetic Protocols for Functionalized Organic Compounds
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All chemicals and reagents were commercially purchased and used directly without further purification. Flash column chromatography and analytical thin layer chromatography (TLC) were performed using silica gel 60 (200–300 mesh) and silica gel aluminum sheets F254 (Qingdao Marine Chemical Ltd., Qingdao, China), respectively. The melting points of all the compounds were determined using a WRR melting point apparatus (Shanghai Jingke Industrial Co. Ltd., Shanghai, China) and were uncorrected. Then, 1H NMR and 13C NMR spectra were recorded in CDCl3 or DMSO-d6 solution at 400 MHz for 1H and 101 MHz for 13C on a Bruker Avance III HD 500 MHz NMR Spectrometer (Bruker (Beijing) Scientific Technology Co. Ltd., Beijing, China) using tetramethylsilane (TMS) as an internal standard. High-resolution mass spectra were obtained using a Bruker APEX IV Fourier-transform mass spectrometer (Bruker (Beijing) Scientific Technology Co. Ltd., Beijing, China).
9
Carrageenan NMR Characterization Protocol
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10 mg kappa and lambda-carrageenan samples were sent to Spectral Services, Köln, for NMR measurements. In brief, 10 mg substance were dissolved in 1 ml D2O containing 3-(trimethylsilyl)propionic acid-d4 sodium salt (0.01% as standard). Measurements for 1H spectra were done with an Avance III HD 500 MHz NMR spectrometer (Bruker, Billarica, MA).
10
Synthesis and Characterization of F127-SS-DA
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F127 was dissolved in 40 mL DCM followed by the addition of EDC and DMAP. After 5 min, DTP was added. The mixed solution was stirred for 24 h at room temperature. The mixture was concentrated under reduced pressure to a volume of 20 mL, poured into 200 mL t-butyl methyl ether to precipitate the product, which was further collected by filtration. The product was then dissolved in 50 mL water, dialyzed for 7 days, and lyophilized to obtain the intermediate SS-F127-SS.
SS-F127-SS was dissolved in 15 mL DCM followed by the addition of EDC and DMAP. After 5 min, 3-buten-1-ol was added and stirred for 24 h at room temperature. The mixture was then poured into 200 mL t-butyl methyl ether to precipitate the product, which was collected by filtration. The solid was then dissolved in 50 mL water, dialyzed for 7 days, and lyophilized to obtain the final product F127-SS-DA. The structures of SS-F127-SS and F127-SS-DA were confirmed by the Bruker Avance-III HD 500 MHz NMR spectrometer.
SS-F127-SS was dissolved in 15 mL DCM followed by the addition of EDC and DMAP. After 5 min, 3-buten-1-ol was added and stirred for 24 h at room temperature. The mixture was then poured into 200 mL t-butyl methyl ether to precipitate the product, which was collected by filtration. The solid was then dissolved in 50 mL water, dialyzed for 7 days, and lyophilized to obtain the final product F127-SS-DA. The structures of SS-F127-SS and F127-SS-DA were confirmed by the Bruker Avance-III HD 500 MHz NMR spectrometer.
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