31P MAS NMR spectra were collected at 161.97 MHz (magnetic field of 9.4 T) on a Bruker AV-400-WB with a 4 mm triple channel probe with ZrO rotors, Kel-F-plug at room temperature and 10 kHz slew rate. A single π/2 pulse of 60 kHz and spectral width of 100 kHz was used in the direct irradiation tests. The relaxation time was 40 seconds and samples were accumulated for 128 scans. In the CP-MAS tests a 1H excitation pulse of 3 μs, 3 ms contact time, 100 kHz spectral width, ppm 15 decoupling at 80 kHz were used, and samples accumulated with 512 scans were used. The relaxation time was 5 seconds. In both cases, (NH4)H2PO4 (ADP) at 0.81 ppm was used as secondary reference with respect to H3PO4 (85%) as the primary reference. The chemical shift resolution was ± 0.2 ppm.
Av 400 wb
Manufactured by Bruker
The AV-400-WB is a nuclear magnetic resonance (NMR) spectrometer manufactured by Bruker. It operates at a magnetic field strength of 9.4 Tesla and is capable of performing wide-band (WB) experiments. The core function of the AV-400-WB is to analyze the molecular structure and properties of various chemical compounds through the detection and measurement of nuclear magnetic resonances.
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5 protocols using av 400 wb
1
Solid-State 31P NMR Characterization
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31P MAS NMR spectra were collected at 161.97 MHz (magnetic field of 9.4 T) on a Bruker AV-400-WB with a 4 mm triple channel probe with ZrO rotors, Kel-F-plug at room temperature and 10 kHz slew rate. A single π/2 pulse of 60 kHz and spectral width of 100 kHz was used in the direct irradiation tests. The relaxation time was 40 seconds and samples were accumulated for 128 scans. In the CP-MAS tests a 1H excitation pulse of 3 μs, 3 ms contact time, 100 kHz spectral width, ppm 15 decoupling at 80 kHz were used, and samples accumulated with 512 scans were used. The relaxation time was 5 seconds. In both cases, (NH4)H2PO4 (ADP) at 0.81 ppm was used as secondary reference with respect to H3PO4 (85%) as the primary reference. The chemical shift resolution was ± 0.2 ppm.
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31P MAS NMR spectra were collected at 161.97 MHz (magnetic field of 9.4 T) on a Bruker AV-400-WB with a 4 mm triple channel probe with ZrO rotors, Kel-F-plug at room temperature and 10 kHz slew rate. A single π/2 pulse of 60 kHz and spectral width of 100 kHz was used in the direct irradiation tests. The relaxation time was 40 seconds and samples were accumulated for 128 scans. In the CP-MAS tests a 1H excitation pulse of 3 μs, 3 ms contact time, 100 kHz spectral width, ppm 15 decoupling at 80 kHz were used, and samples accumulated with 512 scans were used. The relaxation time was 5 seconds. In both cases, (NH4)H2PO4 (ADP) at 0.81 ppm was used as secondary reference with respect to H3PO4 (85%) as the primary reference. The chemical shift resolution was ± 0.2 ppm.
2
Solid-State 31P NMR Characterization
Check if the same lab product or an alternative is used in the 5 most similar protocols
31P MAS NMR spectra were collected at 161.97 MHz (magnetic field of 9.4 T) on a Bruker AV-400-WB with a 4 mm triple channel probe with ZrO rotors, Kel-F-plug at room temperature and 10 kHz slew rate. A single π/2 pulse of 60 kHz and spectral width of 100 kHz was used in the direct irradiation tests. The relaxation time was 40 seconds and samples were accumulated for 128 scans. In the CP-MAS tests a 1H excitation pulse of 3 μs, 3 ms contact time, 100 kHz spectral width, ppm 15 decoupling at 80 kHz were used, and samples accumulated with 512 scans were used. The relaxation time was 5 seconds. In both cases, (NH4)H2PO4 (ADP) at 0.81 ppm was used as secondary reference with respect to H3PO4 (85%) as the primary reference. The chemical shift resolution was ± 0.2 ppm.
+ Expand
31P MAS NMR spectra were collected at 161.97 MHz (magnetic field of 9.4 T) on a Bruker AV-400-WB with a 4 mm triple channel probe with ZrO rotors, Kel-F-plug at room temperature and 10 kHz slew rate. A single π/2 pulse of 60 kHz and spectral width of 100 kHz was used in the direct irradiation tests. The relaxation time was 40 seconds and samples were accumulated for 128 scans. In the CP-MAS tests a 1H excitation pulse of 3 μs, 3 ms contact time, 100 kHz spectral width, ppm 15 decoupling at 80 kHz were used, and samples accumulated with 512 scans were used. The relaxation time was 5 seconds. In both cases, (NH4)H2PO4 (ADP) at 0.81 ppm was used as secondary reference with respect to H3PO4 (85%) as the primary reference. The chemical shift resolution was ± 0.2 ppm.
3
Characterization of Polymer Structure
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FTIR and NMR were used to characterize the structure of the polymer. A Varian 800 FT-IR in Attenuated Total Reflectance (ATR) mode was used to verify the successful introduction of functional groups. 1H NMR and 13C NMR spectra were recorded on a Bruker Av-400-WB instrument using CDCl3 as solvent.11,35 (link) Besides, HSQC (Heteronuclear Single Quantum Coherence) NMR technique was also characterized.
4
Characterization of Synthesized Solid Materials
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The recovered solids were identified by powder X-ray diffraction (PXRD) collected in a Bruker D8 Advance diffractometer using Cu Kα radiation (λ = 1.5418 Å) in the 2θ region between 5° and 45°. Field emission scanning electron micrographs (FE-SEM) were collected using an XL30 S-FEG microscope. Multinuclear magic angle spinning (MAS) NMR spectra ( 19 F, 13 C and 29 Si MAS NMR) of as-synthesized samples were obtained at room temperature on a Bruker AV-400-WB equipment and the details have been given elsewhere. 10 CHN elemental analyses were carried out using a LECO CHNS-932 analyzer. Thermal gravimetric analyses were performed in a SDT Q600 TA instrument under air flow (100 ml/min) heating from 25 ℃ to 1000 ℃ (with a heating rate of 10 ℃/min). Nitrogen adsorption/desorption were carried out in a Micromeritics ASAP 2010 equipment at the N 2 liquefaction temperature of 77 K. The samples were outgassed under vacuum at 120 ℃.
5
Comprehensive Characterization of Porous Zeolites
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Powder X-ray diffraction (PXRD) was used to identify the recovered solids. The diffraction patterns were obtained in a Bruker D8 Advance diffractometer using Cu Kα radiation (λ = 1.5418 Å). For indexing asmade pMWW, long scan data were also obtained. The amount of organic matter occluded in the as-made zeolites was determined by CHN elemental analysis using a LECO CHNS-932 analyzer. Thermal gravimetric analysis was carried out in a SDT Q600 TA instrument under air flow (100 ml/min) heating from 25 °C to 1000 °C (with a heating rate of 10 °C/min). The morphologies of the obtained samples were investigated by field emission scanning electron microscopy (FE-SEM), using a Philips XL30 S-FEG. Multinuclear magic angle spinning (MAS) NMR spectroscopy of as-synthesized samples was obtained at room temperature on a Bruker AV-400-WB equipment and the details can be found in our previously reported work. [31] Fourier Transform infrared spectra were obtained with a Bruker IFS 66/S spectrophotometer. Nitrogen adsorption/desorption were carried out in a Micromeritics ASAP 2010 equipment at the N2 liquefaction temperature of 77 K. The calcined samples were outgassed under vacuum at 120 °C.
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