Melting points were determined using a BÜCHI B-540 (Flawil, Switzerland) melting point apparatus. The elemental analysis (C, H, N) was performed on Perkin-Elmer 2400. The IR spectra were measured with a Perkin-Elmer FT-IR 1725X spectrophotometer (in KBr) or a Varian 670-IR FT-IR spectrometer (ATR) in the range of 600–4000 cm−1. NMR spectra were recorded in DMSO-d6 using a Bruker DRX 500 instrument. Chemical shifts (δ/ppm) were described in relation to tetramethylsilane (TMS). The MS spectra (EI, 70 eV) were recorded using the apparatus AMD-604.
B 540
Manufactured by Büchi
Sourced in Switzerland
The B-540 is a laboratory evaporation system designed for sample preparation and concentration. It features a heating bath and a vacuum pump to facilitate the evaporation process. The core function of the B-540 is to efficiently remove solvents from liquid samples.
Automatically generated - may contain errors
Lab products found in correlation
Mini 2 nitrogen adsorption apparatus, by Microtrac (5 mentions)
Equinox 55, by Bruker (3 mentions)
X pert mpd diffractometer, by Philips (3 mentions)
Cm120, by Philips (3 mentions)
Ft ir 1725x spectrophotometer, by PerkinElmer (2 mentions)
Silica gel 60 pf254 cards, by Merck Group (2 mentions)
Drx 500 instrument, by Bruker (1 mentions)
Avance 300, by Bruker (1 mentions)
Gf254, by Merck Group (1 mentions)
Sps 800, by MBraun (1 mentions)
Synapt g1 ms, by Waters Corporation (1 mentions)
Microflex lt, by Bruker (1 mentions)
Mercury 400, by Agilent Technologies (1 mentions)
Drx 500, by Bruker (1 mentions)
2400 series 2 chns o elemental analyzer, by PerkinElmer (1 mentions)
Chns o analyzer, by PerkinElmer (1 mentions)
Drx 400, by Bruker (1 mentions)
Jms hx110 spectrometer, by JEOL (1 mentions)
Chiralpak od h, by Daicel (1 mentions)
Mcp 200 polarimeter, by Anton Paar (1 mentions)
41 protocols using b 540
1
Characterization of Novel Compounds
2
Characterization of Organic Compounds
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Melting points were measured with a Büchi B-540 apparatus. NMR spectra were recorded with a Bruker Avance 300 (300.13 MHz for 1H and 75.47 MHz for 13C) spectrometer. Chemical shifts (δ) are reported in ppm and coupling constants (J) in Hz; the internal standard was TMS. Unequivocal 13C assignments were made with the aid of 2D gHSQC and gHMBC (delays for one-bond-long range JC/H couplings were optimized for 145 and 7 Hz, respectively) experiments. Positive-ion ESI mass spectra were acquired with a QTOF 2 instrument [dilution of 1 µL] of the sample in chloroform solution (ca. 10–5 mL) in 200 µL of 0.1% trifluoroacetic acid/methanol solution. Nitrogen was used as the nebuliser gas and argon as the collision gas. The needle voltage was set at 3000 V, with the ion source at 80 °C and the desolvation temperature at 150 °C. The cone voltage was 35 V. Other low- and high-resolution mass spectra (EI, 70 eV) were measured with VG Autospec Q and M spectrometers. Preparative thin-layer chromatography was performed with Merck silica gel (60 DGF254). All chemicals and solvents used were obtained from commercial sources and used as received or dried using standard procedures. MW-assisted reactions were carried out in a CEM Discover SP apparatus.
3
Synthesis and Characterization of Novel α-Aminophosphonic Acids
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All chemicals were purchased from Sigma-Aldrich and used without purification. All reactions were monitored by thin-layer chromatography (TLC) on silica Merck GF254 plates. Microwave assisted reactions were carried out using MWO720CR6S microwave. The melting points (m. p) of the obtained α-aminophosphonic acids were measured by open capillary method in BÜCHI melting point B-540. UV-Vis spectra in ethanol were measured with a UV-Vis spectrophotometer (V-650 Jasco double beam). The FT-IR spectra were recorded in transmittance mode from 4000 to 600 cm−1 on a spectrometer type: FT-IR-4200 Jasco. 1H NMR, 13C NMR and 31P NMR are recorded on a Bruker spectrometer at 400, 133, 100 MHz, respectively using DMSO-d6 as solvent. Chemical shifts are reported in units (ppm) with tetramethylsilane (TMS) as a reference.
4
Solid-Phase Peptide Synthesis with Anhydrous Conditions
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Chemicals and reagents were used as commercially supplied without any further purification unless otherwise stated. Low loading Wang resin (0.38 mmol/g) was purchased from Novabiochem. Ghosez reagent was purchased from Sigma Aldrich. N,N-diisopropylethylamine (DIPEA) was distilled over calcium hydride. Anhydrous THF and CH2Cl2 for solid phase synthesis were dispensed from an MBRAUN SPS-800 solvent purification system. Reactions requiring anhydrous conditions were performed under nitrogen atmosphere. Melting points were determined using a Buchi B-540 melting point apparatus.
5
Microsphere Melting Point Analysis
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The melting temperature range of all microspheres batches was investigated by using a Buchi melting point apparatus model B-540. Briefly, the sample was placed in a capillary glass and analyzed at a heating rate of 5 °C/min, until microspheres entirely melted.
6
Synthesis and Characterization of Thiolated CoQ Analogs
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Reagents and solvents were of analytical grade and were purchased from commercial suppliers with a minimum purity of 95%), and used as received. Melting points (mp) were determined on electrical melting point (Büchi B-540) and are uncorrected. The Fourier transform infrared spectra were recorded on a Alpha T FTIR spectrometer equipped with single reflection diamond ATR module. 1H NMR and 13C NMR spectra were acquired on a Bruker for the characterization of the purified analogs. The 1H NMR spectra data is expressed in the form: chemical shifts in units of parts per million (ppm) in CDCl3 and coupling constants (J) are in hertz (Hz). Mass spectra were recorded on a BRUKER Microflex LT by MALDI (Matrix Assisted Laser Desorption Ionization)-TOF technique via addition of 1,8,9-anthracenetriol (DIT, dithranol) as matrix. High-resolution mass spectra electrospray ionization (HRMS-ESI) were obtained on a Waters SYNAPT G1 MS by dissolving analogs (2–3 mg) in acetonitrile. Thin layer chromatography (TLC) was performed with silica gel coated aluminum sheets from Merck KGaA. TLC visualization was carried out by using UV light (254 nm). All synthesized thiolated CoQ analogs were purified by column chromatography with a silica gel 60 (63–200 μm particle sized) with appropriate solvent system as eluent.
7
Analytical Characterization of Organic Compounds
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Melting points (m.p.) were determined using a BÜCHI B-540 (Flawil, Switzerland) melting point apparatus and were uncorrected. The elemental analysis (C, H, N) was performed on a CHNS/O Elemental Analyzer 2400 Series II (Perkin-Elmer, Waltham, MA, USA). The IR spectra were measured with a Perkin-Elmer FT-IR 1725X spectrophotometer (Perkin-Elmer, Waltham, MA, USA) (in KBr) in the range of 600–4000 cm−1. The NMR spectra (1H NMR) were recorded in DMSO-d6 using a Mercury 400 (Varian, Palo Alto, CA, USA) or Bruker DRX 500 (Bruker Daltonics, Inc., Billerica, MA, USA). Chemical shifts (δ, ppm) were described in relation to tetramethylsilane (TMS) and coupling constants (J) expressed in Hz. The MS spectra (EI, 70 eV) were recorded using the apparatus AMD-604 (AMD Analysis & Technology AG, Harpstedt, Germany).
8
Melting Point and Spectroscopic Analysis
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The melting points of compounds were determined using a Buchi melting point apparatus (B-540). High pure analytical grade reagents were used throughout all experiments and were purchased from Sigma Aldrich Chemical Co. (St. Louis, MO, USA) and Alfa Aesar Chemical Co. (St. Parkridge Ward Hill, MA, USA). 1H-NMR and 13C-NMR spectra were measured in CDCl3 and CD3OD (Bruker Aspect AM-300 instrument) at 300/75 MHz respectively. The chemical shift values (δ) were given in ppm and coupling constant was measured in Hertz (Hz). EI-MS spectra were recorded on a JMS-HX-110 spectrometer with a data system. Elemental analysis was carried out by using CHNS/O analyzer (Perkin-Elmer 2400 series). For column chromatography, silica gel (70–230 mesh) and silica gel (230–400 mesh) were used. The reactions were monitored on TLC, using Merck silica gel 60 PF254 cards. The compounds were visualized by UV lamp (254–365 nm).
9
Comprehensive Physicochemical Characterization of Catalysts
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Chemicals were purchased from Merck, Fluka and Aldrich Chemical Companies.
Fourier transform infrared (FT-IR) spectra recorded by ATR method on a Bruker (EQUINOX 55) spectrometer. The nuclear magnetic resonance (NMR) spectra were recorded in DMSO-d6 on Bruker (DRX-400, Avance) NMR 400 MHz. Melting points were determined by a Büchi B-540 instrument. Field emission scanning electron microscopy (FESEM) apparatus (Mira 3-XMU) was used for recording of FESEM images. The XRD graph of catalyst was obtained by X-ray diffractometer (XRD, Bruker-binary V3) using a Cu kα anode (k = 1.54 Å, radiation at 36 kV and 36 mA) in the 2θ range from 10° to 80°. Energy-dispersive X-ray spectrometer (EDS) and maps of catalyst were recorded by Phenom pro X. Thermal gravimetric analysis (TGA) was done using “BÄHR-(model: STA 503)” instrument. BELSORP MINI II nitrogen adsorption apparatus (Japan) was used for recording of Brunauer–Emmett–Teller (BET) specific surface area of catalyst at 77 K. Inductively coupled plasma mass spectrometry (ICP-MS) was recorded by AGILENT 7500 apparatus. All IR and 1H NMR spectra data are available in ESI (Fig. S1–S20).†
Fourier transform infrared (FT-IR) spectra recorded by ATR method on a Bruker (EQUINOX 55) spectrometer. The nuclear magnetic resonance (NMR) spectra were recorded in DMSO-d6 on Bruker (DRX-400, Avance) NMR 400 MHz. Melting points were determined by a Büchi B-540 instrument. Field emission scanning electron microscopy (FESEM) apparatus (Mira 3-XMU) was used for recording of FESEM images. The XRD graph of catalyst was obtained by X-ray diffractometer (XRD, Bruker-binary V3) using a Cu kα anode (k = 1.54 Å, radiation at 36 kV and 36 mA) in the 2θ range from 10° to 80°. Energy-dispersive X-ray spectrometer (EDS) and maps of catalyst were recorded by Phenom pro X. Thermal gravimetric analysis (TGA) was done using “BÄHR-(model: STA 503)” instrument. BELSORP MINI II nitrogen adsorption apparatus (Japan) was used for recording of Brunauer–Emmett–Teller (BET) specific surface area of catalyst at 77 K. Inductively coupled plasma mass spectrometry (ICP-MS) was recorded by AGILENT 7500 apparatus. All IR and 1H NMR spectra data are available in ESI (Fig. S1–S20).
10
Characterization of Synthesized Nanomaterials
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Chemicals were purchased from Merck, Fluka, and Aldrich Chemical Companies. 1H NMR and 13C NMR spectra were recorded at 400 and 100 MHz, respectively. Fourier transform infrared (FT-IR) measurements (in KBr pellets or ATR) were recorded on a Brucker spectrometer. Melting points were determined on a Büchi B-540 apparatus. The X-ray diffraction (XRD) pattern was obtained by a Philips XpertMPD diffractometer equipped with a Cu Kα anode (k = 1.54 Å) in the 2θ range from 10 to 80˚. Field Emission Scanning Electron Microscopy (FESEM) was obtained on a Mira 3-XMU. VSM measurements were performed by using a vibrating sample magnetometer (Meghnatis Daghigh Kavir Co. Kashan Kavir, Iran). Energy-dispersive X-ray spectroscopy (EDS) of nano-catalyst was measured by an EDS instrument and Phenom pro X. The EDX-MAP micrographs were obtained on MIRA II detector SAMX (France). Thermal gravimetric analysis (TGA) was conducted using the “STA 504” instrument. BELSORP MINI II nitrogen adsorption apparatus (japan) for recording Brunauer–Emmett–Teller (BET) of nano-catalyst at 77 K [4 (link), 12 (link)]. X-Ray Photoelectron Spectroscopy (XPS) analysis was done with BESTEC (EA 10). Transmission electron microscopy (TEM) was obtained using a Philips CM120 with a LaB6 cathode and accelerating voltage of 120 kV.
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