We acquired the NMR spectra of whole cells at 25 °C on a 400-MHz Bruker AVANCE DPX spectrometer using a 5-mm inverse broadband probe and running TopSpin 1.3. 31P shifts are reported relative to external 85% phosphoric acid at 0 ppm. For the proton-decoupled 31P-NMR spectra, we used “zgdc30” with WALTZ16 decoupling and sweep width of 80 ppm, a 3-s relaxation delay, 100K scans, and 20-Hz line-broadening. We packed the Prochlorococcus SB and MIT9301 whole cells into a 5-mm tube (Shigemi Inc.) with magnetic susceptibility of the glass inserts matching D2O. We acquired the 31P-NMR spectra of Prochlorococcus SB protein fraction at 25 °C on a 400-MHz Bruker Ascend 400 equipped with a Sample CASE and using the program “zgpg30” with a sweep width of 80 ppm, a relaxation delay of 2 s, a 15-Hz line-broadening, and for 13K scans. 31P chemical shifts are reported relative to external phosphoric acid at 0 ppm.
Avance dpx spectrometer
Manufactured by Bruker
Sourced in Germany
The Avance DPX spectrometer is a nuclear magnetic resonance (NMR) spectrometer designed and manufactured by Bruker. It is used for the analysis and identification of chemical compounds through the detection and measurement of nuclear magnetic resonances. The Avance DPX spectrometer provides high-performance NMR capabilities for a range of applications in various fields, including chemistry, biochemistry, and materials science.
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Lab products found in correlation
Precoated silica gel plate, by Merck Group (2 mentions)
Uv 1800 spectrophotometer, by Shimadzu (2 mentions)
Ascend 400, by Bruker (1 mentions)
Agilent 5100 icp oes, by Agilent Technologies (1 mentions)
5 bromo 2 hydroxybenzaldehyde, by Merck Group (1 mentions)
1 10 phenanthrolin 5 amine, by Merck Group (1 mentions)
Thiophene 3 carbaldehyde, by Merck Group (1 mentions)
Exactive mass spectrometer, by Thermo Fisher Scientific (1 mentions)
3 amino 5 hydroxypyrazole, by Merck Group (1 mentions)
Sonifier 450, by Emerson (1 mentions)
Dpx 500, by Bruker (1 mentions)
Avance dpx 400 mhz spectrometer, by Bruker (1 mentions)
8 protocols using avance dpx spectrometer
1
NMR Spectroscopy of Prochlorococcus Cells
2
Preparation and Characterization of Ionic Liquids
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Prior to all physical and electrochemical measurements, all ILs were dried under vacuum (ca. 10−3 mbar) at 353–373 K with stirring for at least 2 days. This treatment was found to reduce the water content to below 100 ppm, as measured by Karl Fischer coulometric titration. The resolution of the water content measurements was 0.001 wt/wt % (or 10 ppm) and measurements were completed in duplicate. Once dried, the IL samples were stored in the Ar‐filled glovebox with moisture levels less than 3 ppm water. Lithium content of the ILs was analysed by inductively coupled plasma optical emission spectroscopy (ICP‐OES) on an Agilent 5100 ICP‐OES, and along with Microanalysis, was performed by Analytical Services at Queen's University, Belfast. 1H and 13C NMR spectra were recorded at 293 K on a Bruker Avance DPX spectrometer at 300 MHz and 75 MHz, respectively. 1H and 13C NMR spectra for all [TFSI]− ILs are shown in Figures S7 to S36 in the ESI.
3
Synthesis and Characterization of Heteroaromatic Compounds
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1,10-phenanthrolin-5-amine, 5-bromo-2-hydroxybenzaldehyde, and thiophene-3-carbaldehyde were procured from Sigma (Sigma, Mumbai, India), and S.D. Chemicals (RD Chem, Mumbai, India) and used without further purification. All the solvents were obtained from Merck (Goa, India), which were dried before using them in the experiments. Thin Layer Chromatography (TLC) was used to check the completion of reaction by spotting the reaction mixture on pre-coated silica-gel plates (Merck, Mumbai, India) and the spots were visualized by UV irradiation. Infrared spectral studies were performed on Perkin-Elmer spectrometer (PerkinElmer, Waltam, MA, USA) version 10.03.09 (KBr pellet technique). 1H and 13C NMR were recorded on a 500 MHz Bruker Avance DPX spectrometer (Bruker, Ettlingen, Germany) with TMS as internal standard. Mass spectra (ESI-MS) of the compounds were measured on Agilent mass spectrometer (Agilent, Santa Clara, CA, USA). The UV-Visible absorption spectra were recorded using UV-1800 spectrophotometer (Shimadzu, Koyto, Japan).
4
Characterizing Photochemical Reaction Intermediates
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CIDNP NMR experiments were carried out with a 200 MHz Bruker AVANCE DPX spectrometer equipped with a custom‐made CIDNP probe head. A Quantel Nd‐YAG Brilliant B laser (355 nm, ca. 50 mJ per pulse, pulse length 8–10 ns) operating at 20 Hz was employed as light source. The pulse sequence of the experiment consisted of a series of 180° radio‐frequency (RF) pulses to suppress the NMR signals of the parent compounds, the laser flash, the 90° RF detection pulse, and the acquisition of the free induction decay. “Dummy” CIDNP spectra, acquired by employing the same pulse sequence but without the laser pulse, were always measured. Samples were prepared in [D8]toluene and deoxygenated by bubbling with nitrogen before the experiment. Chemical shifts δ are reported in ppm relative to TMS by using the residual methyl signal of deuterated toluene as an internal reference (δH=2.09 ppm). If necessary, line broadening (1 Hz, exponential) was applied to the spectra.
5
Synthesis and Characterization of Pyrazole Derivative
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3-Amino-5-hydroxypyrazole and m-anisaldehyde were purchased from Sigma Aldrich and were used as received. The solvents were purchased from Merck and used without further purification. The completion of reaction was monitored by thin layer chromatography (TLC) performed on pre-coated silica-gel plates (Merck, India) and spots were visualized by UV irradiation. FT-IR spectral measurements were recorded on Perkin-Elmer spectrometer version 10.03.09 (KBr pellet technique). 1H and 13C NMR were obtained using a 500 MHz Bruker Avance DPX spectrometer with TMS as internal standard. HR-ESI-MS analysis was performed on a Thermo Scientific Exactive mass spectrometer by electrospray ionization technique. The electronic absorption spectra were recorded using UV1800 spectrophotometer (Shimadzu). Steady-state fluorescence experiments were performed with a SPEX Fluorolog F112X spectrofluorometer by using optically dilute solutions.
6
Synthesis and Characterization of Novel Compounds
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Unless otherwise specified, chemicals were purchased from Sigma-Aldrich and used without further purification. CH2Cl2 was distilled from calcium hydride before use. 1H and 13C NMR spectra were recorded on a Bruker Avance DPX spectrometer operating at 400 and 100 MHz, respectively. Chemical shifts (δ) are given in ppm relative to the NMR solvent residual peak and coupling constants (J) in hertz. Mass spectra were recorded using a Mariner™ ESI-TOF spectrometer. Wavenumbers are given in cm−1 at their maximum intensity. Dynamic light scattering (DLS) measurements were carried out using a Vasco Flex instrument by Cordouan Technologies equipped with a laser diode (λ = 450 nm). Zeta potential measurements were performed on a Wallis instrument from Cordouan Technologies equipped with a laser diode (λ = 635 nm). For ultrasonic mixing, an ultrasonic probe (Branson Sonifier 450, Output 4, Duty cycle 30%) was used. Photo-polymerization experiments were carried out using a low pressure 40 W mercury UV lamp (Heraeus) at 254 nm.
7
NMR Characterization of Monomer and Polymer
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The 1H-NMR (500 MHz) and 13C-NMR (125 MHz) of the monomer and polymer were recorded on a Bruker Avance DPX spectrometer, Bruker DPX-500, (Ettlingen, Germany) using tetramethylsilane (TMS) as the internal standard. All chemical shifts were given in parts per million (ppm) relative to the internal standard tetramethylsilane (TMS = 0.00 ppm). The splitting patterns were illustrated as follows: “s” for singlet, “d” for doublet, “t” for triplet, “q” for quartet, “m” for multiplet, and “br” for broad signal.
8
NMR Characterization of TOPO Liquid Blends
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Neat liquid TOPO:malonic acid (w TOPO = 0.50-0.67) and TOPO: levulinic acid (w TOPO = 0.10-0.20) were examined by NMR spectroscopy. The samples were prepared in a glove box under a dry argon atmosphere and transferred directly to NMR. 31 P NMR spectra were recorded on a Bruker Avance DPX 400 MHz spectrometer at 162 MHz with a sealed D 3 PO 4 capillary added to supply an external lock, referencing the spectra to D 3 PO 4 (d 31 P = 0 ppm). For 1 H (400 MHz) and 13 C (101 MHz) NMR measurements, a sealed d 6 -DMSO capillary was used to supply the external lock and reference.
To determine the species formed in the liquid phase as a result of decomposition, 13 C NMR measurements were performed on a 400 MHz Bruker Avance DPX spectrometer at 101 MHz. TOPO:malonic acid samples were dissolved in d 6 -acetone as they were not homogeneous liquids at w TOPO = 0.33 at ambient temperature. TOPO:levulinic acid samples were run neat with a d 6 -DMSO capillary as a reference.
To determine the species formed in the liquid phase as a result of decomposition, 13 C NMR measurements were performed on a 400 MHz Bruker Avance DPX spectrometer at 101 MHz. TOPO:malonic acid samples were dissolved in d 6 -acetone as they were not homogeneous liquids at w TOPO = 0.33 at ambient temperature. TOPO:levulinic acid samples were run neat with a d 6 -DMSO capillary as a reference.
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