All MS experiments were performed on a Bruker microTOF-Q spectrometer (Bruker Daltonik, Bremen, Germany), equipped with an Apollo II electrospray ionization source with an ion funnel. The instrument parameters were: scan range m/z 250-2000, dry gasnitrogen, temperature 200 °C, ion source voltage 4500 V, collision energy 10 eV, analyte aqueous solutions (70 μL). Solutions were introduced at a flow rate of 3 μL min -1 . The Bruker microTOF-Q spectrometer was calibrated with the Tunemix™ mixture (Bruker Daltonik, Germany) in the quadratic regression mode. The mass spectrometer operated in the positive ion mode. Each spectrum was obtained with more than 100 individual scans. The overall charge of the analysed ions was calculated on the basis of the distance between isotopic peaks. The formulae of the complexes were determined by application of the Compass Data Analysis program (Bruker Daltonik, Germany). 22 The water and D 2 O solutions of the ligand (1 × 10 -4 M) with FeCl 3 and AlCl 3 salts (1 : 3 metal to ligand molar ratio) and CuCl 2 , ZnCl 2 (1 : 2 metal to ligand molar ratio) were incubated for 15 days at room temperature before the measurements. Solutions at variable pH and pD values were obtained by adding triethylamine and HCl (water solution), or NaOD and DCl (D 2 O solutions). pH and pD were measured on a previously calibrated pHmeter.
Microtof q spectrometer
Manufactured by Bruker
Sourced in Germany, United States
The Microtof-Q spectrometer is a high-performance mass spectrometry instrument designed for accurate mass measurements and detailed structural analysis. It combines a time-of-flight mass analyzer with a quadrupole mass filter, providing high resolving power and sensitivity for a wide range of applications.
Automatically generated - may contain errors
Lab products found in correlation
Tunemix mixture, by Bruker (3 mentions)
Avance 400, by Bruker (3 mentions)
Arx 300, by Bruker (3 mentions)
Melting point b 540 apparatus, by Büchi (2 mentions)
Compass dataanalysis 4.0 program, by Bruker (2 mentions)
Av 400 instrument, by Bruker (2 mentions)
Compass data analysis program, by Bruker (1 mentions)
Superdex 200 10 300 column, by GE Healthcare (1 mentions)
Akta purifier system, by GE Healthcare (1 mentions)
Esi qtof instrument, by Agilent Technologies (1 mentions)
Arx 600 mhz or 400 mhz spectrometer, by Bruker (1 mentions)
Usb4000 uv vis spectrometer, by OceanOptics (1 mentions)
Am 250, by Bruker (1 mentions)
Melting point b 545, by Büchi (1 mentions)
Spectrometers, by Bruker (1 mentions)
Nanoled, by Horiba (1 mentions)
Lambda 265 uv vis spectrophotometer, by PerkinElmer (1 mentions)
Avance 400 mhz spectrometer, by Bruker (1 mentions)
Nicolet avatar 360 ftir, by Thermo Fisher Scientific (1 mentions)
Varian cary 100 bio spectrophotometer, by Agilent Technologies (1 mentions)
26 protocols using microtof q spectrometer
1
Mass Spectrometry Analysis of Metal Complexes
2
Characterizing Recombinant Protein Structure
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The molecular masses of purified recombinant proteins were analyzed using a Bruker microTOF-Q spectrometer (Bruker Daltonics, Bremen, Germany) equipped with an Apollo II electrospray ionization source as described previously (Couturier et al., 2011 (link)). The oligomerization state of purified recombinant proteins was analyzed on a Superdex 200 10/300 column equilibrated in 30 mM Tris-HCl pH 8.0, 200 mM NaCl and connected to an Akta purifier system (GE Healthcare) by injecting 100 μg of purified recombinant proteins at a flow rate of 0.5 ml/min. The column was calibrated using the molecular weight standards (6500–700,000 Da) from Sigma.
3
Characterization of Organic Compounds
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Reagents and starting materials in current study were of analytic grade and used without further purification unless otherwise specified. Analytical thin layer chromatography was performed on silica gel HF254 plates. Preparative column chromatography was performed using silica gel H. Melting points were determined by a Büchi melting point B-540 apparatus. All 1H and 13C NMR spectra were recorded at 600 MHz and 150 MHz on a Bruker ARX 600 MHz model spectrometer in DMSO-d6 with TMS as the internal standard. NMR spectra were analysed and interpreted using MestReNova. ESI-MS spectra were recorded on an Agilent ESI-QTOF instrument. HR-MS were obtained on a Bruker micrOTOF_Q spectrometer.
4
Detailed Characterization of Novel Organic Compounds
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All the reagents were used without further purification unless otherwise specified. Solvents were dried and redistilled prior to use according to the standard method. Analytical thin layer chromatography (TLC) was performed using silica gel HF254. Preparative column chromatography was performed with silica gel H. Melting points were determined on a Büchi melting point B-540 apparatus. 1H- and 13C-NMR spectra were recorded on a Bruker ARX 600 MHz or 400 MHz spectrometer using DMSO-d6 or C5D5N as solvents and TMS (tetramethylsilane) as the internal standard. High-resolution mass spectra (HR-MS) were obtained on a Bruker micrOTOF_Q spectrometer.
5
Chromatography and Spectroscopy Procedures
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Reagents and general procedures Commercial reagents were used without further purification. Solvents were dried and redistilled prior to use. Thin-layer chromatography (TLC) was performed on silica gel plates (Polychrom SI F254), using UV-light, phosphomolybdic acid, potassium permanganate or ninhydrin as stains. Column chromatography was performed using silica gel (0.04-0.06 mm, 230-240 mesh). 1 H and 13 C NMR spectra were measured with Bruker Avance-400 and Bruker ARX-300 spectrometers in D2O or H2O/D2O (9:1). Multiplicities are quoted as singlet (s), doublet (d), or multiplet (m). Spectra were assigned by using COSY and HSQC. All chemical shifts (δ) were recorded in ppm and coupling constants (J) are reported in Hz. High-resolution electrospray mass (ESI) spectra were recorded on a microTOF-Q-Bruker spectrometer; accurate mass measurements were achieved by using sodium formate as an external reference. UV/Vis spectra were recorded in approximately 10 -5 M solutions in DMSO by using an OceanOptics USB4000UV-Vis spectrometer and quartz cells (1 cm path length). Luminiscence measurements were recorded with same solutions by using a Jobin-Yvon-Horiba Fluorolog 3-22 Tau-3 spectrofluorometer.
6
Spectroscopic Characterization of Compounds
7
NMR and Mass Spectrometry Analysis
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Commercial reagents were used without further purification. Solvents were dried and redistilled prior to use in the usual way. 1H and 13C NMR spectra were measured with Bruker Avance-400 and Bruker ARX-300 spectrometers in D2O or H2O/D2O (9 : 1) at 298 K. Spectra were assigned by using COSY and HSQC. High-resolution electrospray ionization (ESI) mass spectra were recorded on a microTOF-Q-BRUKER spectrometer; accurate mass measurements were achieved by using sodium formate as an external reference.
8
Characterization of Organic Compounds
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All reagents were purchased from Sigma-Aldrich or Acros Company used without further purification. Reactions were monitored by thin layer chromatography (TLC) carried out on 0.25-mm Merck silica gel plates (60F-254) using ultraviolet light (254 nm) as the visualizing agent and KMnO4 solution as developing agents. NMR spectra were recorded with Bruker spectrometers operating at (360MHz, 300 MHz and 250 MHz for 1H, 90 MHz, 75 MHz or 63 MHz for 13 C and 101 MHz or 121 MHz for 31 P). Chemical shift of Solvent reference peaks used were CDCl3 (δ = 7.26 ppm) for 1H and (δ = 77ppm) for 13 C NMR spectra, while H3PO4 was used as external standard for chemical shift references for 31 P NMR. Couplings constants (J) are given in Hz, with the Following abbreviations multiplicity: s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet, br = broad signal. Mass spectra were taken by a MicrOTOF-Q Bruker spectrometer using electrospray ionization (ESI) analysis. Melting points were measured using Buchi Melting Point B-545. Optical rotations were measured on an Anton Paar's MCP 150 and Bellingham & Stanley ADS 420 polarimeters and reported as follows: ሾߙሿ ் (concentration (g/mL), solvent).
9
Comprehensive Characterization of Compounds
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FTIR spectra were measured with a Perkin-Elmer Two (Perkin-Elmer, Waltham, MA, USA) spectrophotometer equipped with a diamond crystal UATR accessory. 1H, 31P{1H}, and 1H PGSE NMR spectra were measured with a Bruker AVANCE 400 (Bruker Corporation, Fällanden, Switzerland) spectrometer in D2O solution. Chemical shifts are quoted relative to SiMe4 (1H, external) and H3PO4 85% in D2O (31P, external). 1H PGSE-NMR measurements were carried out with the doubly stimulated echo-pulsed sequence (Double STE) on a Bruker AVANCE 400 equipped with a BBI H-BB Z-GRD probe at 298 K without spinning at different times in D2O. Steady-state luminescence spectra were measured with a spectrofluorimeter of HORIBA Jobin Yvon Fluorolog-3 (HORIBA Jobin Yvon, Stow, MA, USA). Emission lifetimes with the time-correlated single photon counting technique were measured with the Datastation HUB (HORIBA Jobin Yvon) and a nanoLED (HORIBA Jobin Yvon) of 320 nm. Conductivities were measured in ca. 0.5 mM water solutions with a Jenway 4010 conductimeter (Jenway, Felsted, UK). MALDI-MS spectra in negative and positive modes were measured with a Bruker MicroTOF-Q spectrometer equipped with a MALDI-TOF ionization source (Bruker Corporation, Bremen, Germany). UV–Vis spectra in aqueous solution were measured with a LAMBDA 265 UV/Vis spectrophotometer (Perkin-Elmer).
10
Synthesis and Characterization of Pd Complexes
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Reagents used were purchased from Sigma-Aldrich and used without further purification unless otherwise stated. Solvents were purchased from Sigma-Aldrich and were distilled under nitrogen and dried using standard methods [59 ]. Ligands 1 –3 were prepared as outlined in previous work [31 (link)]. [Pd(CH3CN)2Cl2] was prepared according to a published procedure [60 ].
Infrared spectra were recorded on a Nicolet Avatar 360 FT-IR (E.S.P.) spectrophotometer (Thermo Fisher Scientific, Waltham, MA, USA) using κBr pellets. The 1H, COSY, and 13C nuclear magnetic resonance spectra were recorded at ambient temperature on a Bruker AVANCE 400 MHz spectrometer (Bruker, Billerica, MA, USA) at 400 and 101 MHz, respectively. Solvents used were D2O, DMSO-d6, and CDCl3. Electronic spectra were obtained using either Varian Cary 100 Bio spectrophotometer (Agilent, Santa Clara, CA, USA) or PerkinElmer Lambda 25 UV/Vis spectrophotometer (Thermo Fisher Scientific, Waltham, MA, USA). Mass spectra were recorded on a micrOTOF-Q spectrometer (Bruker, Billerica, MA, USA), equipped with E-spray atmospheric pressure ionization chamber (ESI). Elemental analyses were obtained from Midwest Microlab, Indianapolis, IN, USA.
Infrared spectra were recorded on a Nicolet Avatar 360 FT-IR (E.S.P.) spectrophotometer (Thermo Fisher Scientific, Waltham, MA, USA) using κBr pellets. The 1H, COSY, and 13C nuclear magnetic resonance spectra were recorded at ambient temperature on a Bruker AVANCE 400 MHz spectrometer (Bruker, Billerica, MA, USA) at 400 and 101 MHz, respectively. Solvents used were D2O, DMSO-d6, and CDCl3. Electronic spectra were obtained using either Varian Cary 100 Bio spectrophotometer (Agilent, Santa Clara, CA, USA) or PerkinElmer Lambda 25 UV/Vis spectrophotometer (Thermo Fisher Scientific, Waltham, MA, USA). Mass spectra were recorded on a micrOTOF-Q spectrometer (Bruker, Billerica, MA, USA), equipped with E-spray atmospheric pressure ionization chamber (ESI). Elemental analyses were obtained from Midwest Microlab, Indianapolis, IN, USA.
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