1H and 13C NMR spectra were recorded on a Bruker AVANCE 500 spectrometer (500 MHz for 1H, 125 MHz for 13C). Chemical shift values are given in δ (ppm) relative to the residual solvent signals for δH 7.26 ppm and δC 77.16 ppm (CDCl3), and for δH 2.04 ppm and δC 20.00 ppm (CD3COOD). Melting points were measured on a Boetius apparatus and are uncorrected. High-resolution mass spectra (HRMS) were recorded on a 6550 iFunnel Q-TOF LC/MS (Agilent Technologies) micro mass spectrometer by electrospray ionization (ESI). The elemental analyses were performed on a Eurovector EA3000 CHNS-O analyzer. Follow-up of the reactions and evaluation of the purity of the compounds were performed by thin layer chromatography (TLC) on Silica gel (60 Å medium pore diameter) on TLC Al foils with a fluorescent indicator 254 nm (Sigma-Aldrich). Chemicals were purchased from Sigma-Aldrich or Acros Organics and used as received. Solvents were dried and freshly distilled according to the common practice.
Ea3000 chns o analyzer
Manufactured by Eurovector
The EA3000 CHNS-O analyzer is a laboratory instrument designed to determine the elemental composition of organic and inorganic samples. It can analyze the content of carbon, hydrogen, nitrogen, sulfur, and oxygen in a wide range of materials.
Automatically generated - may contain errors
3 protocols using ea3000 chns o analyzer
1
NMR Spectroscopy for Structure Elucidation
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1H and 13C NMR spectra were recorded on a Bruker AVANCE 500 spectrometer (500 MHz for 1H, 125 MHz for 13C). Chemical shift values are given in δ (ppm) relative to the residual solvent signals for δH 7.26 ppm and δC 77.16 ppm (CDCl3), and for δH 2.04 ppm and δC 20.00 ppm (CD3COOD). Melting points were measured on a Boetius apparatus and are uncorrected. High-resolution mass spectra (HRMS) were recorded on a 6550 iFunnel Q-TOF LC/MS (Agilent Technologies) micro mass spectrometer by electrospray ionization (ESI). The elemental analyses were performed on a Eurovector EA3000 CHNS-O analyzer. Follow-up of the reactions and evaluation of the purity of the compounds were performed by thin layer chromatography (TLC) on Silica gel (60 Å medium pore diameter) on TLC Al foils with a fluorescent indicator 254 nm (Sigma-Aldrich). Chemicals were purchased from Sigma-Aldrich or Acros Organics and used as received. Solvents were dried and freshly distilled according to the common practice.
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1H and 13C NMR spectra were recorded on a Bruker AVANCE 500 spectrometer (500 MHz for 1H, 125 MHz for 13C). Chemical shift values are given in δ (ppm) relative to the residual solvent signals for δH 7.26 ppm and δC 77.16 ppm (CDCl3), and for δH 2.04 ppm and δC 20.00 ppm (CD3COOD). Melting points were measured on a Boetius apparatus and are uncorrected. High-resolution mass spectra (HRMS) were recorded on a 6550 iFunnel Q-TOF LC/MS (Agilent Technologies) micro mass spectrometer by electrospray ionization (ESI). The elemental analyses were performed on a Eurovector EA3000 CHNS-O analyzer. Follow-up of the reactions and evaluation of the purity of the compounds were performed by thin layer chromatography (TLC) on Silica gel (60 Å medium pore diameter) on TLC Al foils with a fluorescent indicator 254 nm (Sigma-Aldrich). Chemicals were purchased from Sigma-Aldrich or Acros Organics and used as received. Solvents were dried and freshly distilled according to the common practice.
2
Comprehensive Materials Characterization Protocol
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All reagents were purchased from
commercial sources and used without further purification. Carbon,
nitrogen, and hydrogen were determined on a EuroVector EA 3000 CHNSO
analyzer. Fourier transform-infrared (FT-IR) spectra were recorded
on KBr pellets using a Shimadzu FTIR-8400S spectrophotometer (400–4000
cm–1 range, 4 cm–1 resolution,
20 scans per spectrum). Thermogravimetric analyses (TGA) were carried
out from room temperature to 600 °C at a rate of 5 °C min–1 on a Mettler-Toledo TGA/SDTA 851e thermobalance
under a 50 cm3 min–1 flow of synthetic
air. Powder X-ray diffraction (PXRD) patterns were collected on a
Bruker D8 Advance diffractometer operating at 40 kV/40 mA and equipped
with Cu Kα radiation (λ = 1.5418 Å), a Vantec-1 PSD
detector, an Anton Parr HTK2000 high-temperature furnace, and Pt sample
holder. Data sets were acquired in 2θ steps of 0.033° in
the 5 ≤ 2θ ≤ 40 range (a) from 30 to 600 °C
every 10 °C, (b) from 30 to 150 °C every 5 °C, and
(c) from 150 to 30 °C every 5 °C. Electron spin resonance
(ESR) spectra were recorded on Bruker ELEXSYS 500 (superhigh-Q resonator
ER-4123-SHQ) and Bruker EMX (ER-510-QT resonator) continuous wave
spectrometers for the Q- and X-bands, respectively.
commercial sources and used without further purification. Carbon,
nitrogen, and hydrogen were determined on a EuroVector EA 3000 CHNSO
analyzer. Fourier transform-infrared (FT-IR) spectra were recorded
on KBr pellets using a Shimadzu FTIR-8400S spectrophotometer (400–4000
cm–1 range, 4 cm–1 resolution,
20 scans per spectrum). Thermogravimetric analyses (TGA) were carried
out from room temperature to 600 °C at a rate of 5 °C min–1 on a Mettler-Toledo TGA/SDTA 851e thermobalance
under a 50 cm3 min–1 flow of synthetic
air. Powder X-ray diffraction (PXRD) patterns were collected on a
Bruker D8 Advance diffractometer operating at 40 kV/40 mA and equipped
with Cu Kα radiation (λ = 1.5418 Å), a Vantec-1 PSD
detector, an Anton Parr HTK2000 high-temperature furnace, and Pt sample
holder. Data sets were acquired in 2θ steps of 0.033° in
the 5 ≤ 2θ ≤ 40 range (a) from 30 to 600 °C
every 10 °C, (b) from 30 to 150 °C every 5 °C, and
(c) from 150 to 30 °C every 5 °C. Electron spin resonance
(ESR) spectra were recorded on Bruker ELEXSYS 500 (superhigh-Q resonator
ER-4123-SHQ) and Bruker EMX (ER-510-QT resonator) continuous wave
spectrometers for the Q- and X-bands, respectively.
3
Organic Modifications Analysis on Silica
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EA on C, H, N, and S was done using
a Eurovector EA3000 CHNS-O analyzer. The method has been proven to
be capable of detecting the organic modifications on various silica
materials with the usual accuracy and precision. The uncertainty is
below 0.2 wt % for carbon at 20 wt %. The sample amount weighed for
an analysis was between 3.5 and 5.0 mg when a sufficient sample amount
was available.
a Eurovector EA3000 CHNS-O analyzer. The method has been proven to
be capable of detecting the organic modifications on various silica
materials with the usual accuracy and precision. The uncertainty is
below 0.2 wt % for carbon at 20 wt %. The sample amount weighed for
an analysis was between 3.5 and 5.0 mg when a sufficient sample amount
was available.
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