The melting points (uncorrected) were determined on a Fisher-Johns (Fisher Scientific Company, Pittsburgh, PA, USA) apparatus. The optical rotations were measured on a Perkin-Elmer 323 polarimeter (Perkin Elmer Inc., London, UK). The ECD spectra were recorded on a Jasco J-1500 spectropolarimeter (Jasco, Tokyo, Japan) in MeOH at 1000 ppm. The IR spectra were obtained on a Bruker Tensor 27 spectrometer (Bruker, Ettlingen, Germany); 1D and 2D NMR experiments were performed on a Bruker Advance III HD spectrometer (Bruker BioSpin GmbH, Rheinstetten, Germany) at 500 MHz for 1H and 125 MHz for 13C and on a Bruker Advance III HD spectrometer (Bruker BioSpin GmbH, Rheinstetten, Germany) at 700 MHz for 1H and 175 MHz for 13C, using CDCl3 as solvent. Chemical shifts were referred to residual CHCl3 (δH = 7.26, δC = 77.16). The DART-MS data were obtained on a Jeol, The AccuTOF JMS-T100LC mass spectrometer. (Jeol Ltd., Tokyo, Japan) The X-ray data were collected on a Bruker D8 Venture (Bruker AXS GmbH, Karlsruhe, Germany) using CuKα (λ = 1.54178 Å). Silica gel 230-400 mesh (Macherey-Nagel, Nagel, Macherey Nagel, Düren, Germany), Sephadex LH-20 (Pharmacia Biotech AB, Uppsala, Sweden) and octadecyl-functionalized silica gel (Sigma-Aldrich, St. Louis, MO, USA) were used for column chromatography.
Advance 3 hd spectrometer
Manufactured by Bruker
Sourced in Germany
The Advance III HD spectrometer is a high-performance nuclear magnetic resonance (NMR) spectrometer developed by Bruker. The core function of this instrument is to provide researchers and scientists with a powerful tool for analyzing the structure and properties of chemical compounds, materials, and biological samples through the use of NMR spectroscopy.
Automatically generated - may contain errors
Lab products found in correlation
Tensor 27 spectrometer, by Bruker (2 mentions)
Perkin elmer 323 polarimeter, by PerkinElmer (2 mentions)
Octadecyl functionalized silica gel, by Merck Group (2 mentions)
J 1500 spectropolarimeter, by Jasco (1 mentions)
D8 venture, by Bruker (1 mentions)
D8 diffractometer, by Bruker (1 mentions)
Ta sdt q600, by TA Instruments (1 mentions)
Agtfsi, by Merck Group (1 mentions)
4 mm mas probe, by Bruker (1 mentions)
Uv160u spectrophotometer, by Shimadzu (1 mentions)
Silica gel 230 400 mesh, by Macherey-Nagel (1 mentions)
Accutof jms t100lc mass spectrometer, by JEOL (1 mentions)
5 mm tci probe, by Bruker (1 mentions)
Spectrum two ft ir spectrometer, by PerkinElmer (1 mentions)
Advance 3 spectrometer, by Bruker (1 mentions)
Matlab, by MathWorks (1 mentions)
Nmr suite 8, by Chenomx (1 mentions)
3 mm tci cryoprobe, by Bruker (1 mentions)
Avance 400, by Bruker (1 mentions)
5 mm bbfo probe, by Bruker (1 mentions)
10 protocols using advance 3 hd spectrometer
1
Spectroscopic Characterization of Compounds
2
Characterization of IRMOF-3 and Derivatives
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XRD was performed with Brüker D8 diffractometer operated with a Cu Kα radiation (λ = 1.541 Å) at 40 mA and 40 kV. Nitrogen physisorption measurements were carried out using a Quantachrome instrument at 77 K. Samples weighing 80–100 mg were outgassed for 12 h at 50 °C prior to measurement. FT-IR spectrum (400–4000 cm−1) was recorded from KBr pellet in NICOLET 5700 FT-IR spectrometer. 1H-NMR spectra were recorded on Brüker Advance III HD spectrometer (500 MHz). Approximately 5 mg of IRMOF-3 and IRMOF-3-LA samples were dried under vacuum at 90 °C for 12 h and digested with sonication in 500 μL DMSO-d6 and 100 μL dilute DCl (23 μL of 35% DCl in D2O diluted with 1.0 mL of DMSO-d6). Approximately 10–20 mg of IRMOF-3, IRMOF-3-LA, or IRMOF-3-LA-Au was used for TGA measurements. Samples were analyzed under a stream of N2 using a TA SDT Q600 running from room temperature to 700 °C with a scan rate of 15 °C/min. ICP-AES analysis was performed on a Perkin–Elmer Optima 7000 DV apparatus. TEM studies were carried out with a FEI TECNAI F20 Transmission Electron Microscope. H2-TPR was conducted on a ChemStar apparatus equipped with a TCD detector. A 50-milligram portion of each sample was loaded in a U-shaped quartz microreactor and heated at a ramping rate of 10°C/min in 5 vol% H2 in Ar (a total flow of 50 mL/min).
3
Synthesis and Characterization of Ferrocene Derivatives
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All
solvents were purchased from Sigma-Aldrich
and were of reagent grade except for dried tetrahydrofuran (THF) which
was at 99.9% purity. Ferrocene (Fc) and 1,1′-dimethylferrocene
(Me2Fc) were purchased from Fisher Scientific. Bis(η5-pentamethylcyclopentadienyl)iron(II) (Me10Fc)
was purchased from Acros Organics. AgTFSI, 2,3,4-tetramethyl-1,3-cyclopentadiene,
1,2,3,4-tetramethyl-1,3-cyclopentadiene,1,3-ditertiarybutylcyclopetadiene,
1.9 mol/L t-BuLi in pentane, and 3 mol/L n-BuLi solution in hexane were purchased from Sigma-Aldrich. 1H, and 13C NMR spectra were recorded on a Bruker
400 MHz ADVANCE III HD spectrometer at 400 and 100 MHz, respectively.
When necessary, assignments of 1H and 13C signals
were performed using correlation spectroscopy and heteronuclear single
quantum correlation. High-resolution electrospray mass spectra (HRMS)
in the positive ion mode were obtained on a Q-Tof Ultima Global hybrid
quadrupole/time-of-flight instrument.
solvents were purchased from Sigma-Aldrich
and were of reagent grade except for dried tetrahydrofuran (THF) which
was at 99.9% purity. Ferrocene (Fc) and 1,1′-dimethylferrocene
(Me2Fc) were purchased from Fisher Scientific. Bis(η5-pentamethylcyclopentadienyl)iron(II) (Me10Fc)
was purchased from Acros Organics. AgTFSI, 2,3,4-tetramethyl-1,3-cyclopentadiene,
1,2,3,4-tetramethyl-1,3-cyclopentadiene,1,3-ditertiarybutylcyclopetadiene,
1.9 mol/L t-BuLi in pentane, and 3 mol/L n-BuLi solution in hexane were purchased from Sigma-Aldrich. 1H, and 13C NMR spectra were recorded on a Bruker
400 MHz ADVANCE III HD spectrometer at 400 and 100 MHz, respectively.
When necessary, assignments of 1H and 13C signals
were performed using correlation spectroscopy and heteronuclear single
quantum correlation. High-resolution electrospray mass spectra (HRMS)
in the positive ion mode were obtained on a Q-Tof Ultima Global hybrid
quadrupole/time-of-flight instrument.
4
Solid-State Tin Oxide NMR Analysis
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The 119Sn MAS NMR spectra were recorded on a Bruker Advance III HD spectrometer equipped with a 4 mm MAS probe, operating at 186.5 MHz with the samples spinning at 12 kHz, high power proton decoupling, a 30 s recycle delay, and typically 2048 scans. SnO2 was used as a secondary reference at –604.3 ppm.
5
Characterization of Organic Compounds
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The melting points (uncorrected) were determined on a Fisher-Jhons apparatus (Fisher Scientific Company, Pittsburgh, PA, USA). The optical rotations were measured on a Perkin-Elmer 323 polarimeter (Perkin Elmer Inc., London, UK). The UV spectra were recorded on a Shimadzu UV 160U spectrophotometer (Shimadzu, Kyoto, Japan). VCD data were acquired on a BioTools dualPEM ChiralIR FT-VCD spectrophotometer (Jupiter, FL, USA). The IR spectra were obtained on a Bruker Tensor 27 spectrometer (Bruker, Ettlingen, Germany); 1D and 2D NMR experiments were performed on a Bruker Advance III HD spectrometer (Bruker Corporation, Billerica, MA, USA) at 700 MHz for 1H and 175 MHz for 13C. Chemical shifts were referred to CDCl3 (δH = 7.26, δC = 77.16). The HR-DART-MS data were acquired on a Jeol, AccuTOF JMS-T100LC mass spectrometer (Jeol Ltd., Tokyo, Japan); silica gel 230–400 mesh (Macherey-Nagel, Macherey Nagel, Düren, Germany), Sephadex LH-20 (Pharmacia Biotech AB, Uppsala, Sweden), and octadecyl-functionalized silica gel (Sigma-Aldrich, St. Louis, MO, USA) were used for column chromatography. The X-ray data were collected on an Agilent Xcalibur Atlas Gemini diffractometer (Agilent Technologies, Oxfordshire, UK).
6
NMR Spectroscopy of Organic Compounds
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1H NMR and 2D ROESY NMR spectra were performed on a Bruker Advance III HD spectrometer (600 MHz, Bruker BioSpin, Switzerland) fitted with a 5-mm TCI probe at 298 K, and TMS used as the calibration signal. The solvent in the experiment was D2O (99%), CDCl3 (99%), or DMSO-d6 (99%).
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1H NMR and 2D ROESY NMR spectra were performed on a Bruker Advance III HD spectrometer (600 MHz, Bruker BioSpin, Switzerland) fitted with a 5-mm TCI probe at 298 K, and TMS used as the calibration signal. The solvent in the experiment was D2O (99%), CDCl3 (99%), or DMSO-d6 (99%).
7
Spectroscopic Characterization of Dissolved Cellulose
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NMR spectra were acquired by a Bruker Advance III HD spectrometer at the frequency of 400 MHz for 1H (100 MHz for 13C). High-resolution mass spectrometry (HR-MS) was performed on an Agilent accurate-mass 6520B Q-TOF mass spectrometer. A Perkin Elmer Spectrum Two FTIR spectrometer equipped with a universal diamond ATR unit was used for the analysis of dissolved cellulose. Spectra of samples were recorded between range of 450 cm−1 and 4500 cm−1, at a resolution of 4 cm−1. The spectra shown in Fig. 4 represent the accumulation of 4 scans/sample with baseline correction applied. All purchased chemicals were used without purification.
8
NMR Characterization of PAP9 Peptides
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One milligram of the 34 amino-acids C-terminal peptide of PAP9 was dissolved in 25 mM Na phosphate, pH 6.5 to a final concentration of 1 mM. For assignment of the peptide, homonuclear TOCSY, NOESY, and sensitivity-enhanced 13C-HSQC experiments were recorded at 25°C on a Bruker ADVANCE III spectrometer operating at 1H frequency of 600 MHz and equipped with a triple resonance pulsed field gradient cryoprobe.
For assignment of 6His-PAP9, 100 μM of 15N,13C-6His-PAP9 in a 90:10 H2O:D2O, 10 mM Tris pH 8.0, 50 mM NaCl were used. Heteronuclear 3D Best-TROSY-HNCA, Best-TROSY-HNCACB, Best-TROSY-HNCOCANH (Favier and Brutscher, 2011 (link); Solyom et al., 2013 (link)), sensitivity-enhanced 13C-HSQC and 15N-SOFAST experiments were recorded at 298 K on Bruker ADVANCE III HD spectrometers operating either at 1H frequency of 600 or 700 MHz and equipped with a triple resonance pulsed field gradient cryoprobe. [15N,1H]-TRACT (to estimate the global correlation time) (Lee et al., 2006 (link)) and DOSY experiments (for measuring the translational diffusion) (Morris and Johnson, 1992 (link)) were recorded at 298 K on a Bruker ADVANCE III HD spectrometer operating at 1H frequency of 700 MHz.
For assignment of 6His-PAP9, 100 μM of 15N,13C-6His-PAP9 in a 90:10 H2O:D2O, 10 mM Tris pH 8.0, 50 mM NaCl were used. Heteronuclear 3D Best-TROSY-HNCA, Best-TROSY-HNCACB, Best-TROSY-HNCOCANH (Favier and Brutscher, 2011 (link); Solyom et al., 2013 (link)), sensitivity-enhanced 13C-HSQC and 15N-SOFAST experiments were recorded at 298 K on Bruker ADVANCE III HD spectrometers operating either at 1H frequency of 600 or 700 MHz and equipped with a triple resonance pulsed field gradient cryoprobe. [15N,1H]-TRACT (to estimate the global correlation time) (Lee et al., 2006 (link)) and DOSY experiments (for measuring the translational diffusion) (Morris and Johnson, 1992 (link)) were recorded at 298 K on a Bruker ADVANCE III HD spectrometer operating at 1H frequency of 700 MHz.
9
Comprehensive NMR Metabolite Profiling
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1H-NMR analysis has been described in detail previously [31 (link)]. In short, spectra were recorded at 800 MHz with a Bruker Advance III HD spectrometer with a 3-mm TCI cryoprobe. NMR data were recoded using the Bruker pulse sequence “zgespe”. A total of 128 scans were collected into 64 k data points. Data processing was performed with TopSpin 3.2p16 (Bruker BioSpin) and MatLab (MathWorks Inc., Natick, MA, USA), using TSP-d4 for referencing. In total 237 peaks were manually aligned and integrated peak-by-peak, and these variables represent ∼70 metabolites. A variable could also reflect more than one metabolite. Only variables of interest were identified.
For annotation Chenomx NMR suite 8.31 (Chenomx Inc., Edmonton, AB, Canada), the Human Metabolome Database [37 (link)] and an in-house implementation of the statistical total correlation spectroscopy (STOCSY) routine [38 (link)] were used.
For annotation Chenomx NMR suite 8.31 (Chenomx Inc., Edmonton, AB, Canada), the Human Metabolome Database [37 (link)] and an in-house implementation of the statistical total correlation spectroscopy (STOCSY) routine [38 (link)] were used.
10
Synthesis and Characterization of Mn(II) Complexes
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General procedures. Solvents and starting materials were purchased from Aldrich, Acros and Alfa Aesar and used without further purification, unless stated otherwise. Solvents for high-performance liquid chromatography (HPLC) were HPLC-grade. All aqueous solutions were prepared with Milli-Q water (ρ < 18MΩ). MnCl2.4H2O was obtained from Carlo Erba. Chromium powder 99 %, 100 mesh metal basis density = 2.0-3.0g/cm², was obtained from Alfa-Aesar. Intermediates 2H, 3, 8 and ligand H3L 2 were obtained according to the procedures described previously. [15, 20] IR spectra were recorded on a Perkin Elmer Spectrum One Spectrophotometer as solid samples and only the most significant absorption bands are given in cm -1 . 1 H and 13 C NMR spectra and 2D COSY, NOESY, HSQC, and HMBC experiments were recorded either on Bruker Avance 400 and Avance 500 spectrometers (in Strasbourg) or on a Bruker Advance III HD Spectrometer using a 5 mm BBFO probe (in Orléans). 13 C NMR spectra were measured with 1 H decoupling. All chemical shifts () values are given in parts per million and are referenced to the solvent. [30] Elemental analyses and mass spectrometry analysis were carried out by the Service Commun d'Analyses of the University of Strasbourg.
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